THE JOURNAL OF THE octetv of Cfyemtcct A MONTHLY RECORD FOE ALL INTERESTED IN CHEMICAL MANUFACTURES. No. 1.—VOL. XIX.] JANUARY 31, 1900. "Non-Members 30/- per annum; Members 21/- per Set of extra or back numbers ; Single Copies (Members only) 2/6. Cf)t of Chemical Past Presidents: Sir Henry E. Roscoe, B.A., D.C.L., LL.D., Ph.D., F.R.S Sir Frederick A. Abel, Bart., K.C.B., D.O.L., D.Sc., F.R.S Walter Weldon, F.R.S W. H. Perkin, LL.D., Ph.D., F.R.S B. K. Muspratt David Howard James Dewar, M .A., LL.D., F.R.S Ludwig Mond, Ph.D., F.R.S Sir Lowthian Bell, Bart., F.R.S E. Rider Cook J. Emerson Reynold*, M.D., F.R.S Sir John Evans, K.C.B., D.C.L., LL.D., Sc.D., OX) C . , . . » E. c. c/stanford.V.V/.!I!!!!!!!!!!!!!!!.'!.!... T. E. Thorpe, LL.D., Sc.D., Ph.D., F.R.S Thomas Tyrer Dr. Edward Schunck, F.R.S E. Clowes, D.Sc George Beilbv 1881—1882. 1882—1883. 1883—1884. 1S84—1885. 1885—1886. 1886—1887. 1887—1888. 1888—1889. 1889—1890. 1890—1891. 1891—1892. 1892- 1893- 1S91- 1S95- 1896- 1S97- 1S98- -1893. -1894. -1895. -1890. -1897. -1898. -1S99. COUNCIL FOR YEAR ENDING- JULY 1900. President: Prof. O. F. Chandler, M.D., Ph.D. Vice-Presidents : George Beilby. - Dr. Charles A. Kohn. 11. Forbes Carpenter. Ivan Levinstein. Prof. F. Clowes, D.Sc. j B. E. R. Xewlands. George E. Davis. Dr. Edward Schunck, F.R.S. John Heron. Wm. Thorp, B.Sc. David Howard. R. C. Woodcock. Ordinary Members of Council: Sir John Evans, K.C.B., F.R.S. \ John Pattinson, Sir David Gamble, Bart., C.B. 1 Dr. F. B. Power. W. Win wood Gossa^e. Sir Robert Pullar. E. Grant Hooper. Walter F. Reid. Dr. Rudolph Messel. | Dr. W. S. Squire. J, M. C. Paton. Thos. Tvrer. Sectional Chairmen and Secretaries. LIVERPOOL. I Dr. T. Lewis Baiil<\v. LONDON. I A. R. Ling. MANCHESTER. I J. Carter Bell. NEWCASTLE. I Saville Shaw. NEW YOBK. I Dr. H. Schweitzer. NOTTINGHAM. Prof. F. Stanley Kipping, F.R.S. | J. T. Wood. SCOTTISH Prof. G. G. Henderson, D.Sc. | Thomas Gray. YORKSHIRE. Christopher Rawson. | Prof. H. R. Procter. Honorary Treasurer: Samuel Hall, East London Soap works, Bow, E. Honorary foreign Secretary: Dr. Ludwig Mond, F.R.S. General Secretary : Charles G. Cresswell. Offices: Palace Chambers, 9, Bridge Street, Westminster, S.W. Telegraphic Address: 59, Palatable, London. A. Smotham. Boverton Rodwood. Vacant. N. H. Mnrtin. T. J. Parker. THE JOURNAL. Publication Committee: A. H. Allen. G.H. Bailey, D.Sc, Ph.D. G. Beilby. Joseph Bernays, M.I.C.B. H. Brunner. The President. Wm. Kellner, Ph.D. J. Lewkowitsch, Ph.D. A. R. Ling. Stevenson Macuclam, Ph.D, N. H. Martin. Sir John Evans, K.O.B., F.R.S. ' B. E. R. Newlands. A. G. Green. Samuel Hall. Prof. G. G. Henderson, D.Sc. John Heron. D. B. Hewitt, M.D. David Howard. Prof. J. J. Hummel. Prof. \. K. Huntington. John Pattinson. Prof. H. R. Procter. Boverton Redwood. Walter F. Reid. John Spiller. William Thorp. Thomas Tyrer. Editor: Watson Smith, 31, Upper Park Road, Haverstock Hill, N.W. Assisted by the following Staff of Abstractors; Robt. Adams I., XV. L. Archbutt.L, XII..XVIII.B. J. L. Baker XVI., XVII. H. Ballantyne II., XII. G. H. Beckett VII. XXII. D.Bendix III. E.Bentz IV., V..VI. J. O. Braithwaite XX. J. P. Briggs XVI., XVII. R. B. Brown V., VI. J. A. Butterfield, M.A. II., III. J. U. Collins X. C. V. Cross V., XII., XIX. J. T. Dunn, D.Sc. .- J. K. Halstead V., VI. II. Ingle, Ph D. .. .IV., V., VI. J. B. C. Kershaw .... VII., XI. S. Klcemann.f IV., VI., Ph.D I XIIL.XX. T. A. Lawson.Ph.D.. .IV., XX. F.H.Leeds.. III., XIII., XXI. J. McCrae, Ph.D IV. (i .W. MacDonal(l,M.Se.. XXI I. W.G.McMillan , ' H. S. Pattinson, Ph.D. ... VII. H. T. Pentor- maun T. H. Pope XX., XXI. J. C. Richardson XI. F. W. Renaut Patent List. G. H. Robertson XI. Chas. Salter [ x ""xvi" R. Sandon u t H. 11. B. Shepherd IX. J. Shields, D.Sc, 7 Ph.D .j XI. A. Shonk Gen. Chem. W. Macnab XXII. N. H. J. Miller, Ph.D XV. Chas. Mills IV., VI. C. A. Mitchell, •) VTT ^- VTT B.A \ XII., AXII. J. G. Parker, Ph.D XIV. E. Sonstadt HI., viL. X. A. L. Stern, D.Sc XVII. E -Howard Tripp,} III., VII., ^ h -^ ) XVI. V. II. Veley, M.A.,") n _, F.R.S. .'j Gen. Chem. C. Otto Weber, •) T , T _ TTT Ph.D j I^.. XIII. L. J. de Whalley, B.Sc . .XVI A. Wingham Joseph T. Wood - Wright, >IV.,XVHl B.Sc,M.A... J XX.
Transcript
THE JOURNALOF THE
octetv of CfyemtcctA MONTHLY RECORD
FOE ALL INTERESTED IN CHEMICAL MANUFACTURES.
No. 1.—VOL. XIX.] JANUARY 31, 1900."Non-Members 30/- per annum; Members
21/- per Set of extra or back numbers ;Single Copies (Members only) 2/6.
Cf)t of ChemicalPast Presidents:
Sir Henry E. Roscoe, B.A., D.C.L., LL.D.,Ph.D., F.R.S
Sir Frederick A. Abel, Bart., K.C.B., D.O.L.,D.Sc., F.R.S
Walter Weldon, F.R.SW. H. Perkin, LL.D., Ph.D., F.R.SB. K. MusprattDavid HowardJames Dewar, M .A., LL.D., F.R.SLudwig Mond, Ph.D., F.R.SSir Lowthian Bell, Bart., F.R.SE. Rider CookJ. Emerson Reynold*, M.D., F.R.SSir John Evans, K.C.B., D.C.L., LL.D., Sc.D.,
O X ) C . , . . »
E. c. c/stanford.V.V/.!I!!!!!!!!!!!!!!!.'!.!...T. E. Thorpe, LL.D., Sc.D., Ph.D., F.R.SThomas TyrerDr. Edward Schunck, F.R.SE. Clowes, D.ScGeorge Beilbv
President: Prof. O. F. Chandler, M.D., Ph.D.Vice-Presidents :
George Beilby. - Dr. Charles A. Kohn.11. Forbes Carpenter. Ivan Levinstein.Prof. F. Clowes, D.Sc. j B. E. R. Xewlands.George E. Davis. Dr. Edward Schunck, F.R.S.John Heron. Wm. Thorp, B.Sc.David Howard. R. C. Woodcock.
Ordinary Members of Council:Sir John Evans, K.C.B., F.R.S. \ John Pattinson,Sir David Gamble, Bart., C.B. 1 Dr. F. B. Power.W. Win wood Gossa^e. Sir Robert Pullar.E. Grant Hooper. Walter F. Reid.Dr. Rudolph Messel. | Dr. W. S. Squire.J, M. C. Paton. Thos. Tvrer.
SectionalChairmen and Secretaries.
LIVERPOOL.I Dr. T. Lewis Baiil<\v.
LONDON.I A. R. Ling.
MANCHESTER.I J. Carter Bell.
NEWCASTLE.I Saville Shaw.
NEW YOBK.I Dr. H. Schweitzer.
NOTTINGHAM.Prof. F. Stanley Kipping, F.R.S. | J. T. Wood.
SCOTTISHProf. G. G. Henderson, D.Sc. | Thomas Gray.
YORKSHIRE.Christopher Rawson. | Prof. H. R. Procter.
Honorary Treasurer:Samuel Hall, East London Soap works, Bow, E.
Honorary foreign Secretary:Dr. Ludwig Mond, F.R.S.
General Secretary : Charles G. Cresswell.Offices: Palace Chambers, 9, Bridge Street, Westminster, S.W.
Telegraphic Address: 59, Palatable, London.
A. Smotham.
Boverton Rodwood.
Vacant.
N. H. Mnrtin.
T. J. Parker.
THE JOURNAL.
Publication Committee:
A. H. Allen.G.H. Bailey, D.Sc, Ph.D.G. Beilby.Joseph Bernays, M.I.C.B.H. Brunner.
The President.Wm. Kellner, Ph.D.J. Lewkowitsch, Ph.D.A. R. Ling.Stevenson Macuclam, Ph.D,N. H. Martin.
Sir John Evans, K.O.B., F.R.S. ' B. E. R. Newlands.A. G. Green.Samuel Hall.Prof. G. G. Henderson, D.Sc.John Heron.D. B. Hewitt, M.D.David Howard.Prof. J. J. Hummel.Prof. \. K. Huntington.
John Pattinson.Prof. H. R. Procter.Boverton Redwood.Walter F. Reid.John Spiller.William Thorp.Thomas Tyrer.
Editor:
Watson Smith, 31, Upper Park Road, Haverstock Hill, N.W.
Assisted by the following Staff of Abstractors;
Robt. Adams I., XV.L. Archbutt.L, XII..XVIII.B.J. L. Baker XVI., XVII.H. Ballantyne II., XII.G. H. Beckett VII. XXII.D.Bendix III.E.Bentz IV., V..VI.J. O. Braithwaite XX.J. P. Briggs XVI., XVII.R. B. Brown V., VI.J. A. Butterfield, M.A. II., III.J. U. Collins X.C. V. Cross V., XII., XIX.
J. T. Dunn, D.Sc. .-
J. K. Halstead V., VI.II. Ingle, Ph D. . . .IV., V., VI.J. B. C. Kershaw.... VII., XI.S. Klcemann.f IV., VI.,
Ph.D I XIIL.XX.T. A. Lawson.Ph.D.. .IV., XX.F.H.Leeds.. III., XIII., XXI.J. McCrae, Ph.D IV.
(i .W. MacDonal(l,M.Se.. XXI I.
W.G.McMillan
,'
H. S. Pattinson, Ph.D. ...VII.H. T. Pentor-
maunT. H. Pope XX., XXI.J. C. Richardson XI.F. W. Renaut Patent List.G. H. Robertson XI.
Chas. Salter [ x ""xvi"R. Sandon u t
H. 11. B. Shepherd IX.J. Shields, D.Sc, 7
Ph.D . j XI.
A. Shonk Gen. Chem.
W. Macnab XXII.N. H. J. Miller, Ph.D XV.Chas. Mills IV., VI.C. A. Mitchell, •) V T T ^-V T T
B.A \ XII., A X I I .
J. G. Parker, Ph.D XIV.
E. Sonstadt HI., viL. X.A. L. Stern, D.Sc XVII.E-Howard Tripp,} III., VII.,
^ h - ^ ) XVI.V. II. Veley, M.A.,") n _,
F.R.S. .'j Gen. Chem.
C. Otto Weber, •) T,T _ T T TPh.D j I^.. XIII.
L. J. de Whalley, B.Sc . .XVI
A. WinghamJoseph T. Wood
- Wright, >IV.,XVHlB.Sc,M.A... J XX.
THE JOURNAL OF THE SOCIETY OF CHEMICAL INDUSTRY. [Jan. 31,1900.
itberpoolChairman: A. Smetham.
Vice-chairman: Charles A. Kohn.Committee:
Harry Baker. - Max Muspratt.A. Carey. E. Rhodes.Herbert E. Davies. , T. W. Stuart.D. Herman. Prank Tate.C. L. Higgins. W. Collingwood Williams,E. K. Muspratt.
Hon. Treasurer: W. P. Thompson.Hon. Local Secretary :
T. Lewis Bailey, University College, Liverpool,
SESSION 1899—1900.
Wednesday, Jan. 31st: —Mr. W. P. Reid. Exhibit of " Yelvril" Material.Mr. Alf. Smetham and Mr. P. Robertson Dodd. " Composition of
Rosin, with spncial reference to the Analysis of the PattyMatters of Soap.,,
Zottium &tttton«Chairman: Boverton Redwood.Vice-Chairman: Otto Hehner.
Committee:W. G. Blagden.J. J. Bowley.H. Hemingway.John Heron.E Grant Hooper.D. Lloyd Howard.J. B. Knight.
W. J. Leonard.R. Messel.H. de Mosenthal.Walter P. Reid.A. Gordon Salamon.T. Tyrer.Prank Wilson.
Hon. Local Secretary:A. R. Ling, Laboratory, 2, St. Dunstan's Hill, E.C.
SESSION 1899-1900.
Monday, Peb. 5th:—Dr. W. S. Squire. " Some Recent Objections urged against the
Adoption of the Metric System.,,
Dr. H. R. Le Sueur. ''Oil of Carthamus Tinctorius (Safllower)-"Monday, 31 arch 5th.—Mr. R. W. Allen. " The presence of Naph-
thalene Vapour in Coal Gas.,,
Monday, April 2nd.—Mr. A. Gordon Salamon. " The Manufactureof Caramel.,,
£>erttoiuChairman: Vacant.
Vice-Chairman: J. Grossmann.Committee:
I. Levinstein.A. Liebmann.A. K. Miller.F. Scudder.Edw. Schunck.C. Truby.
Hon. Local Secretary:J. Carter Bell, The Cliff, Higher Broughton, Manchester.
G. H.Bailey.F. H. Bowman.W. Brown.H. Grimshaw.J. M. Irving.31. J. Langdon.
SESSION 1899-1900.
A. Allhusen.P. P. Bedson.G. T. France.T. W. Hogg.H. Louis.H. S. Pattinson.
CJiairman: N. H. Martin.Vice-Chairman: F. S. Newall.
Committee:John Pattinson.W. W. Proctor.W. L. Rennoldson.G. Sisson.J. E. Stead.J. K. Stock.
Hon. Local Secretary and Treasurer:Seville Shaw, Durham College of Science, Newcastle-on-Tyne.
Ctoirman: T. J. Parker.Vice-Chair man: Clifford Richardson.
Committee:H. Binney. j B. G. Love.C. F. Chandler. I R. "W. Moore.H. Clememtson. ; C. E. Pellew.V. Coblentz. G. A. Prochazka.B. B. Goldsmith. , Max. Toch.J. Hartford. | S. A. Tucker.J. Hasslacher. |
Hon. Treasurer: R. C. Woodcock.Hon. Local Secretary:
H. Schweitzer, 40, Stone Street, New York, U.S.A.
Chairman: P. Stanley Kipping.
Vice-chairman: J. O'Sullivan.
L. Archbutt.S. P. Burford.P. J. R. Carulla.R. M. Caven.H. Forth.
Committee:J. F. Kempson,J. M. C. Paton.A. L. Stern.J. J. Sudborough.S. Trotman.G. J. Ward.W. Scott Herriot.
Hon. Treasurer : S. J. Pentesost.Hon. Local Secretary :
3. T. Wood, 29, Musters Road, West Bridgiord Nottingham.
SESSIOX 1899-1900.
AVednesday, Jan. 31st (Rurton-on-Trent) :—Mr. Wilton P. Rix. " Lead Frets and Leadless Glazes/ ,
Dr. A. L. Stern. " Relation between the Volumes of Sugar Solu-tions before and after Fermentation. , ,
Dr. H. G. Column and J. P. Smith. " The Estimation of Naph-thalene in Coal Gas."
Chairman: G. G. Henderson.Vice-Chairman : A. P# Aitken.
Committee:W. Carrick Anderson.E. M. Bailey.G. T. Beilby.A. C. J . Charlier.J. Christie.John Clark.C. J . Ellis.
W. Foulis.W. Frew.R. A. Inglis.Robt. Irvine.A. D. Ker.J. B. Readman.R. T. Thomson.
C. A. Fawsitt.
Hon. Secretary and Treasurer:Thomas Gray, Technical College, 2i)4, George Street, Glasgow.
Chairman: Christopher Rawson.
Vice-Chairman: George Ward.
Committee:
Edw. Halliwell.J. J. Hummel.W. McD. Mackey.H. R. Procter.G. W. Slatter.Thorp Whitaker.
Bon. Local Secretary and Treasurer:H. R. Procter, ^ Yorkshire College,
J. E. Bedford.V. W. Branson.H. K. Burnett.A. W. Cooke.T. Fairley.W, M, Gardner.
si, i8oo.] THE JOUENAL OF THE SOCIETY OF OHEMIOAL INDUSTRY. 3
NOTICES.
PRIZES EOR THE SOLUTION OF INDUSTRIAL PROBLEMS.
It has been felt for some time that it would tend to theadvancement of applied chemistry if the Society were toencourage manufacturers to bring their problems and diffi-culties under the notice of men of skill and experience, suchas may be found in works and technical laboratories as wellas in universities and colleges.
The Council is now prepared to consider applicationsfrom manufacturers and industrial associations who desireto avail themselves of such assistance.
The order of procedure will be as follows :—The manufacturer or his representative will read a paper
at one of the Sectional Meetings setting forth clearly andfully the nature of the problem awaiting solution, and theconditions, chemical, physical, and economic by which it issurrounded. Sufficient statistical information will be sup-plied to give a fair general idea of the scope and magnitudeof the problem. This paper would appear in the Society'sJournal, and would serve as a guide to the competitorsand a standard of reference to the prize committee whichthe Council would appoint to regulate the competition.
When the manufacturer or Industrial Association offers asum of money for a prize or prizes, the Council will acceptthat sum in trust on behalf of the prize committee.
Problems may be dealt with in several ways, of which thefollowing will serve as illustrations :—
(1.) Special investigations bearing on the subject, apartfrom the suggestion of practical applications ofthe facts discovered.
(2.) Practical solutions of problems. The competitorsmight patent these.
(I?.) Essays on the work of others which might bear onthe solution of problems.
These last would be a valuable training for students,while the essays themselves would serve as a starting pointfor new investigations, and would enhance the value of theSociety's Journal.
The first prize competition under this scheme is now setforth on p. 1098 of the December number 1899. TheScottish Papermakers' Association offers prizes to the valueof 100/. for solutions of certain problems connected withtheir industry. Mr. K. C. MeDzies has described the natureof the problems, and the Prize Committee appointed by the( ouncil has laid down the conditions of the competition,particulars of which may be obtained from Mr. G. MonroThomson, W.S., 123, George Street, Edinburgh. Subsequentproblems will be advertised from time to time under theSocietv's official list of notices in the Journal.
COLLECTIVE INDEX.
The Collective Index (1881 —1895) is now ready. Theprices are as follows :—
To Members and Past Members; Libraries,Societies, and Exchanges on the Society'sList Each copy 10s.
To Subscribers „ 12s. 6d.To others ,,
Notice is hereby given, for the information of members andadvertisers, that the advertisement columns of this Journalhave been contracted for by Messrs. EYRE and SPOTTISWOODE,the Society's printers and publishers, to whom all commu-nications respecting them should be addressed. The circu-lation of the Journal is now more than 3,500 per month.
LIST OP MEMBERS ELECTED 23rd JANUARY 1900.
Alexander, Jerome, c/o National Gum and Mica Co.,502-510, West 45th Street, New York, U.S.A.,Chemist.
Thomson, A. L., l/o Baltimore; 69, West 85th Street, NewYork City, U.S.A.
Thornton, W., l/o Veraguas ; (Journals) c/o Isaac Brandonand Bros., Panama, Central America ; and (subsn.) c/oThos. Thornton, Hermand, West Calder, N.B.
Trewbv, H.: all communications to 62, St. John Street,E.C.
Van Slooten, W., l/o Xew York ; 52, Sidney Place, Brooklyn,N.Y., U.S.A.
Yoorhees, 3. S., l/o Alexandria; c/o Xew York Central andHudson River Railroad, West Albany, N.Y., U.S.A.
Wade, A. L., l/o Hawick; 28, West Kensington Gardens,W.
Want, W. Philip, l/o 42 ; 44, Bishopsgate Without, London,E.C.
Wilson, Frank, l/o Castle Street ; 7, Bedford Square, W.C.Woolf, Julian, l/o Marlboro, Place ; 51, JBuckland Crescent,
Soath Hampstead, X.W.
JBeatfcs*Inndlay, J. T. J., c/o Spencer, Chapraar, and Messel, Ltd.,
Silvcrtown, E.
Hauff, Julius, Eeuerbach, bei Stuttgart.Longshaw, Jas., Hollinside, Huyton, Liverpool.Moncrieff, Jno., Elmside, Balhousie, Perth.Stockdale, Albert, Birstall, near Leeds.
Meeting held on Monday, January 8/A, 1900,
MR. BOVKHTON KKDWOOD IN THE C1IAIK.
COLOUR PHOTOGRAPHY:THK " JOLT " PKOCESS.
BV J. AV. HINCIILEY, A.R.S.M., WILSC, F.C.S.
VERY early in the present century the influence of colouredlight on the salts of silver suggested the possibility ofdirect colour photography.
In 1810, Seebeck noted that a film of chloride of silver,when exposed for some time to the solar spectrum, becametinged with colours approximately those of the incidentlight; a brown shade was produced where the violet lightfell, a shade of blue where the blue fell, a red tint wrherethe red fell, the film exposed to the yellow remainingunaltered.
Almost all the pioneers of ordinary photography wereencouraged by such results to further experiment, Sir
John Herschel, Fox Talbot, Poitevin, de Saint Flonent,Becquerel, and Niepce de Saint Victor being amongst thenumber. Most of their pictures were obtained by exposing,in the camera, paper, first sensitised with silver chloride,and then floated on baths of various solutions ; none ofthe results were either good or permanent: Becquerelused a polished silver plate, on which a film of rose-coloured sub-chloride of silver had been formed electrically;his photographs of the spectrum were remarkable, butincapable of fixation. Lippmann's method, although duevery probably to the same phenomenon as that of Becquerel,can hardly be considered a development of i t ; instead ofattempting to find a material, which, after certain treat-ment, assumes permanently the colour of the light allowedto fall on it, lie endeavoured to register in the film thewaves of light themselves. His success, announced in1881, claimed the admiration of the whole world; bybacking a sensitive film with a mirror of mercury, heproduced stationary waves from the incident light, whichbecame registered in silver deposit on development; it isclear that instability in the film, and consequently silverdeposit, would be produced in those regions subject to thegreatest disturbance, viz., the ventral segments of thestationary waves. Unfortunately, the process fails forcomplex colours, and proves to be very difficult; probablynot more than half-a-dozen workers have been able toclaim any degree of success, and these testify to itsimpracticable character.
In practical work to-day, direct methods of colour photo-graphy have no place; indirect processes, however, inwhich only records of colour are photographed, pigmentsbeing used to supply the colours themselves, have animportant place in the world's industry. That branch ofprocess work, three colour printing, depends mainly on theprinciples laid down by Clerk Maxwell in 1855 and 1861,who, reviving Young's theory of colour vision enunciatedin 1802, showed how it indicated a method of photograph}'in natural colours, and even went so far as to project,by means of the triple lantern, results of his own.
Stated briefly, according to the Young-Helmholtz theoryof colour vision, the sensitive portion of the retina isprovided with three sets of nerve fibrils, each correspondingto a particular colour sensation; one set is most stronglyacted on by red light, the second by green light, and thethird by violet light; if all three are about equally stimu-lated simultaneously, the sensation of white, light results,other compound colour sensations being produced by tlu*more or less response of each. It does not follow fromthis, that green light, does not act on the nerve fibrilsconcerned Avith the red; in fact, an examination of ab-normal colour vision SIIOAVS that persons with normalvision can never appreciate the fundamental green sensation.
The modern idea of three primary colours is based onthis theory, and though not absolutely true, gives resultsso good as to defy ordinary vision.
Assuming three fundamental colours, Maxwell plottedcurves indicating the amounts of each necessary to re-produce the tint of any particular Avavc length of thespectrum. Such curves which are usually referred to hythe colour photographer, are of course not4 colour sensationcurves ; that the synthesis of the spectrum can be per-formed in this way, is readily shown by moving the curvesat right-angles to their base line, in their true relativepositions, and coloured with their respective fundamentalcolours, rapidly before the eye.
The method of colour photography suggested by Maxwoll,is essentially that brought to great perfection by'lves since1886 ; by means of coloured screens, photographic nega-tives, each recording the relative amount of a particularcolour sensation in silver deposit, are obtained, and positiveson glass printed from them. These positives, each backedwith a glass of the fundamental colour, of Avhich there is arecord, are combined optically either by means of the triplelantern, or by Ives' chromoscope. The result, if the photo-graphic work has been correctly performed, is a representa-tion of the object in natural colours.
This process is not so simple as it may appear; thechoice of colour screens is difficult in the extreme Aglance at Maxwell's curves reveals the fact that the
6 THE JOUSNAL OP THE SOCIETY OF CHEMICAL INDUSTRY. [•».» a.
maximum height and average position of the curve, indi-cating the amount of fundamental red required in thesynthesis of the spectrum, does not lie in the red, hut inthe orange ; so that a screen transmitting light accordingto this curve is quite different in colour from the funda-mental red adopted: for similar reasons the green andviolet screens, used when taking the photograph, also differfrom the fundamental green and violet screens used inviewing the photographic records. This difference in colourbetween the taking and viewing screens was first insisted onby Ives in 1888. "Some further modifications of the coloursof the taking screens may be necessarv to eliminate defectsin sensitiveness of the photographic plates used in makingthe records.
The plate to Maxwell was the primary difficulty ; in histime, the practical photography of reds and yellows was animpossibility. In 187*.*, Vogel discovered that certain fugitiveaniline dyes had the property of altering the range of sensi-tiveness of the film, and since then the development of thecolour sensitive plate has advanced and culminated in theremarkable plates due to James Cadett, which have an almostuniform sensitiveness throughout the visual spectrum withthe exception of a small gap in the extreme red, practicallyuseless in colour-forming power, but which provides thephotographer and manufacturer with the possibility of a safelight to work by. All plates, however, have a considerabledeirree of sensitiveness to the ultra-violet, rendering an addi-tional screen necessary to prevent its action on the plate ;such a screen or interceptor may consist of a film ofcelluloid, collodion, or gelatine, stained with picric acid orother suitable dve, to such a tint as not to cut off morethan the extreme violet when intercepting the ultra-violet.
With the complete apparatus beautiful and truthfulresults can be obtained by the expert, but owing toaltering conditions of light, the necessary for differentexposures and the difficulty of developing those parts ofthe negative representing the whites of the object to thesame deiiree of density of silver deposit, absolute accuracyis impossible, and, in any case, optical representation incolours not a true colour photograph is produced.
This optical combination of three positive images may bereplaced by the superposition on glass or on paper of threenegative images complementary in colour to the funda-mentals adopted. These films may be produced by photo-graphic or mechanical means; by the first method we havethe early work of Ives and the later work of Lumiere andSelle, and although their results are exceedingly beautiful,their truth and practical merit do not appeal to the everyday worker.
When mechanical means are adopted,, we have the wellknown three colour printing processes, which introduce usto a subject too vast for this paper.
It is to Joly, however, in 1894, that we owe the stepfrom composite colour photography to the true colourphotograph. His idea, he says, referring to the Voung-llelmholtz theory, " is to carry the appreciation ofphysiological principles still further, and divide up theplate like a hypothetical sub-division of the retina, so thatall over the plate there should be minute regions uniformlydistributed, wherein the sensitive silver salt is excited tobecome reduced to the 'photogenic , material in the samedegree in which the sensations of redness, grernne<s, violet-ness, would have been actually excited in the several nervesof the retina, had the image been formed upon if,. Theessential point, of the process is a method of colour mixturewhich does away with optical superposition, and is at thesnne time extremely simple. If strips of colour sufficientlynarrow be placed side by side and viewed from a suitabledistance, the eye will perceive the colour due to theirmixture. Acting on this, Joly combines the two sets ofthree screens into two, one a. taking screen, and the other aviewing screen. Each consists of a glass plate carryinlines of the three colours side by side, these lines beino-'lcssthan ^z
ff wide and in contact with each other withoutoverlap. By means of these screens the* production of acolour photograph is comparatively a simple operation • theinterceptor being placed in the lens of the camera,' theplate and taking screen are arranged in the dark slide filmto film in such a way, that on exposure the lined screen
g
filters the light before it reaches the pJate. On (levelop-ment a negative is obtained recording in density of silverdeposit under the three lines the degrees in which flu:several colours of the object have power to excite in theeye the three fundamental colour sensations. A positheprinted from this negative, and adjusted in contact with aviewing screen, so that the red record line of the positivecoincides with the red line of the screen, and the other linessimilarly coincide, will reveal the object in its true coloursThe ease and accuracy of the method are remarkable, forall the difficulties which the worker in composite colourphotography has to face arc overcome in the manufactureof the screen. If the taking screen in photographing awhite object gives an equal density of silver deposit undereach of the lines, then the colours of any object will becorrect; should one of the lines be too dense, an alterationof the interceptor, by tinting it slightly to cut oft' theparticular colour, will bring about the equality easily.
It will be readily understood from this description thatthe manufacture of the screens is not a simple* process*The glass plates on which the lines are to be placed arethoroughly cleaned after the manner adopted in drv platemanufacture, except that the necessity for perfectly cleanglass is, if possible, greater; they are then coated with afilm of gelatine, somewhat, thicker than that of a drv plate:the gelatine used must; be very hard and at the same timeas absorbent as possible, and since thecertainl\ of chemicalaction on the dyes prevents, the use of antiseptics, thegelatine solution must he freshly made at as low atemperature as possible.
The operation of lining the plates is a most difficult one,and is carried out in exceptionally accurate* ruling machines,ordinary drawing pens carrying reservoirs of red, green,and violet ink, being the means of producing the lines.The pens are trailed across the plate, and the pressureallowable being very small, the lightest pen consistent withrigiditv that can be made is used*
In the early machines the spindles of the pens rested inV grooves, the lateral movement being prevented by littlemagnets attracting a disk on the spindle against the adjust-ing screw. Killing took place in both directions of movement,each side of the pen being used alternately. It was found,however, that a great many difficulties, mechanical andphotographic, could be avoided by ruling with one side ofthe pen, and in one direction only; in the latest machinesthe pens swing in jewelled bearings, rule in one direction,and are lifted on the idle or quick return stroke. Time forthe absorption of each line is provided by each pen rulinga few lines in advance of that following. About one and ahalf minutes is required for efficient absorption. The inksare water inks, aniline dyes being used to produce theintense colours necessary, and gums to give them viscosity.
After much experiment and failure it was found thatregard must be had to the following points :
(1.) The hygrometric state and temperature of the air.(2.) The shape of the pens and the pressure thev exert
on the film while ruling.(3.) The viscosity of the ink at the temperature of
ruling.(I . ) The rate of ruling.(5.) The correct adjustment of the pens.(f>.) Absolute uniformity of conditions during ruling
Of these the hygrometrie state of the air is perhaps themost important factor, for should the air he too drv the inkin the pens becomes too thick and refuses to rule* and toomuch moisture causes difficulties from the non-drviuf ofthe ruled lines ; the evaporation of the water from the"mkline is negligible in comparison to its absorption bv thegelatine, and since gelatine is very sensitive to changes oftemperature and hygrometric state of the air, there arelimits to the teraparature of ruling, and a t ' a n v criventemperature, there are definite limits of hygrometric sHteat low temperature (10° or 12° C ) , the dew point nuiv be7 or 8-' below the temperature of ruling without seriousconsequences, but every degree above this temperaturenarrows the hygrometric limits considerably until -it 19° Cthe limit is between 1° and 2° C , and above this temperatureruling becomes practically impossible.
Jan. si, i m ] THE JOUENAL OF THE SOCIETY OF OHEMIOAL INDUSTKY.
The shape of the pens is also an important factor ; thenibs should slope evenly together, their inclination to eachother being about 3°; the points must be semi-circular inform, corresponding to the natural shape of a drop, andthe diameter of the semi-circle must not be more than 2 mm.,or it becomes difficult to maintain the exact width of line;the ends of the nibs must be carefully shaped and broughtto knife edges which are finally rounded, to prevent thecutting of the film, by rubbing on wash leather; one penwill rule about 100 plates before requiring to be re-set, thus,its point will rub on gelatine for two miles before the wearis such as to cause bad or faulty lines. The pens aretrailed across the plate their own weight giving the pressurerequired to maintain a continuous line; under ordinaryconditions they are inclined about 5 or 8 degrees, for thepressure on the plate must not be more than one and a halfgrammes ; if one nib is a little longer than the other, or ifit touches the ridge formed on the gelatine by the previousline, a wavy line is the result and the screen becomesuseless.
It was speedily found that the quality of the screensdepended on the viscosity of the ink, and the necessity arosefor the measurement of this property; the inks beingopaque, ordinary methods were unsuitable, and finally themeasurement of the rate of flow through a capillary tubeinto a constant partial vacuum was found to provide thesimplest and easiest test.
The rate of ruling will depend on the viscosity of theink ; with ink giving the best results, the speed is about £"per second.
The adjustment of the pens was a mechanical questionwhich gave a great deal of trouble but was solved by means,which need not concern us here ; the distance apart of thenibs was usually found to be about ~ of the width of theline ruled; with too viscous ink, however, the nibs arefound to be wider apart than the width of the line ruled,and in this case the ruling becomes very erratic.
Perhaps no more important factor in any manufacture isuniformity, and no product could suffer more from lack ofthis than the " Joly " screen. A rise in temperature of onlylrt C. means at some temperatures a lowering of theviscosity of the inks to less than half their former value,with the result that the lines, on account of an increasedflow of ink, widen ; a correcting tendency, however, appearsin the increased rate of absorption of the gelatine, so thatthe after spread of the line will be less ; again, should thehygrometric state of the air alter, the absorption of thegelatine increasing or diminishing will bring about similarchanges ; also, while ruling, the slight drying of the ink inthe pen produces a secular narrowing, so that it is necessaryto commence with a wider line than would produce a perfectscreen.
All these changes have their corresponding colourchanges which make it imperative to ensure absoluteuniformity of conditions, for true colours are just asessential to perfect results as perfect ruling.
After the ruling of the screen is an accomplished fact,it is dried by wTarm air for some hours and protected byvarnish. A satisfactorv varnish which would not attackthe colours nor dissolve them could not be found, andfinally a compromise was made and though the medium ofthe varnish slightly dissolved the green dye, the loss ofcolour, with a very concentrated varnish was so small as tobe quite inappreciable.
The manufacture of celluloid films and interceptors is asubject great enough for a single paper and calls for nospecial mention at the end of this.
All methods of testing the inks for truth of colour werefound to be unsatisfactory unless applied to the ruled line,and the greatest difficulty was found in preserving uni-formity in this respect, perhaps the greatest need of all wasthat of a green dye, whose absorption would enable theadopted curves to be imitated more closely.
All the attempts to photograph landscapes by the Jolymethod were, for a reason which remained mysterious forsome time, failures; natural greens, illuminated out ofdoors, were hopelessly wrong, while the same greens photo-graphed in a studio were reproduced correctly ; the failurewas proved to be due to a defect in the old spectrum plate,
which was very sensitive to a band of no colour valueon the border of the visual spectrum at the red end. Allattempts at cutting out this band (it was transmitted by allthree lines) were unsuccessful until by accident it was foundthat a trace of mercuric chloride added to an ethyl greensolution would do so; a method based on this was toocomplicated for practical work, and when the new"spectrum" plate appeared, was rendered unnecessary.By means of this plate correct renderings of all colourscould be obtained.
The discovery of permanent dyes, of film material, &c,must proceed further before any great advance in this workcan be expected, and' we can only hope that the results ofthe diligent workers of the past may encourage those of thepresent to make colour photography still more of a practicalsuccess, rather than a laboratory experiment.
DISCUSSION.
The CHAIRMAN said that even if, strictly speaking,exception might be taken to the title of the paper, noexception could be taken to the manner in which theauthor had treated his subject. He had made it quiteclear that no claim could be advanced for what wasgenerally understood, at any rate by those who knew butlittle about the subject, by the term* colour photography ;and he (the Chairman) might add, that speaking in thelight of present knowledge, there was unfortunately verylittle ground for hope that any sensitive substance might bediscovered which would register and reproduce the variouscolours of nature. At the same time it was clear that onehad in this process a practically available method ofproducing colour effects. The process, moreover, was notmerely one of beauty, but it appeared likely also to be oneof considerable practical value ; and they all felt grateful toMr. Hinchley for bringing it before them.
Mr. J . CADETT said he was very gratified to hear such apaper read before the Society. He would not say that it wasnecessary that every chemist should be a photographer,but it was unquestionable that every photographer ought tobe a chemist; and it would not be amiss if the Society tookmore account of photography than it did at present. Thechemical reactions that were involved in photography wereeven more puzzling than those in the average range ofchemical research, for in photography they had not onlychemical reactions, but also physical conditions to consider,and these were often baffling. For this reason photographicmanufacturers needed the aid of the chemist. For instance,very little was known of the nature and properties ofgelatin, the principal basis of the modern dry plate. Thatbody had been the bane of his existence. What they wantedwas a chemist who would devote his life to gelatin, anduntil some such help was forthcoming photographic manu-facturers would be condemned to flounder on in helpless"ignorance. The paper to which he had listened that nighthad given him an insight into the Joly process which hehad uever possessed, and had enabled him to appreciate itsdifficulties, especially as to the production of the beautifulscreens they had seen. With regard to the platesthemselves it was easier to make a plate sensitive throughoutthe whole range of the spectrum than to make one with agap in the extreme red such as his own sensitive plates had.It had taken him two years to do this. Plates sensitivethroughout the whole of the spectrum could only be madeby working in total darkness; such a procedure was abso-lutely impossible in a factory where tons of plates had tobe produced. The author, in speaking of Maxwell's curves,had omitted, no doubt unintentionally, to mention the curvesgiven by Sir William Abney in his lecture before the RoyalSociety. Sir William had drawn the curves in such amanner that the various colour sensations were representedas the various fundamental colours, plus white light exceptingthe red ; and since the reading of that paper they had hadsomething tangible to go upon. The only fundamentalsensation they could have in perfect purity was the red •in the green, one must have white light or mixtures with theblue and red; and if those curves were drawn so that theycrossed each other plus white light the purest effects of colourwere obtained. Sir William Abney had given us these par-ticular curves for the first time ; and to manufacturers and all
8 THE JOURNAL OP THE SOOIETT OF CHEMICAL INDUSTRY. [Jan. si, 1&00.
interested in the future of colour photography they would be ofthe utmost value. What was really required in the sensitivecolour plate ? I t must be affected by the various portionsof the spectrum so as to give densities proportionate to thelogarithms of the intensities of .light in the spectrum itself.I t was impossible to single out the colour sensation curves.They must have admixtures ; but if the plate followed thosecurves they had all that was necessary. With regard to thefuture, he thought they need not sigh for a material whichwould give all the colours of nature; for in getting thosethey would lose all that reproductive power which tricolourprinting gave them. If they could make screens whichwould give results on the plates comparable with the curves,and printed in inks transparent in themselves, which werethe complementaries of the colour sensation curves, theywould have all that would be necessary to reproduce colour.From three negatives and half-tone blocks, 20 millionprints had recently been made, and the prints from themwere chosen in preference to some of the best lithographicartists' work. The author had given so able a description ofhis process, that it was unnecessary for him to say more.He believed that before long trichromatic printing wouldbecome the general process in use. The regular illustratedjournals would probably be printed by this means, and theeve would be satisfied bv its rendering, of colour.
The CHAIRMAN remarked that it might be taken asevidence of the rapidly growing importance of the NewYork Section that three of its members were present therethat evening. Judging from the variety of papers whichthe Publication Committee received from the New YorkSection, it might be said that the Section was possessed of a
s omewhat encyclopaedic knowledge ; if, therefore, any of themembers present were qualified to contribute to the discus-sion, they would be gladly heard ; but in any case, he feltsure he was only fulfilling the wishes of every member ofthe London Section in extending to them a very heartywelcome.
Mr. H. DE MosENTiiAL said that he could not see howprints or process blocks could be obtained from a singlenegative ruled alternately in the three colours as described,and asked whether there was any means of doing so.
Mr. IIiNCiiLEY said that the question was perhaps some-what apart from the paper; but he might explain that thereAN as an American process for using the Joly method forproducing colour blocks, and that by this process threeblocks would be used all produced from one negative bytaking each line separately. He was, however, not in aposition to enter more fully into it. lie did not think theJoly process offered more facilities for colour printing thanthe ordinary process of Maxwell and Ives.
Dr. S. RIDEAL said the point that interested him mostwas the difficulty which the inventors had had in ruling thelines of their screens with viscous gums. He had doneconsiderable work on the viscosity of gum solutions, andhad encountered most of the difficulties referred to bv theauthor, due chiefly to variations of temperature. If heremembered rightly, he had managed to get what IK* calleda gum solution of standard viscosity by using ordinarygum arabic mixed with an insoluble gum. The viscosity ofa gum depended on the presence of insoluble metarabin,and the amount of metarabin varied with gums grown atdifferent temperatures and under different conditions ; butby taking a soluble gum and adding insoluble metarabin,such as occurred in the cherry, it was possible to make abody of constant viscosity; and he ventured to think thatthis course^ might be found useful by the author.
Mr. J. A. HICKS asked whether it was necessary to havea separate screen for every lantern slide exhibited.
Mr. HIXCIILEY replied that it was not. Several lectureshad been given with only two viewing screens, an assistantadjusting one positive while another was being exhibited.
Mr. W. F. REID asked if it was absolutely necessary tomake the screens of gelatin. From the details which theauthor had given them it seemed to him that a substancehad been chosen for those screens which offered the utmostdifficulties. Would it not be possible to use, say, celluloidor another substance which he had exhibited not long ago ?If some such material were employed, it seemed to himthat it would be possible to produce the lines by merelypressing the sheet of celluloid or similar material against
a metal plate upon which depressed lines had beenengraved. The colour could be applied to the raised linesthus produced by means of a roller in one operation, and,if necessary, the raised lines could be flattened by pressingon a level plate. Then, again, the author had chosen forhis inks aniline dyes soluble in water. But water itself,from the hygroscopic nature of our climate, produceddifficulties of its own. Why not choose a liquid in whichaniline dyes are soluble, and which might produce verygood lines upon such a substance as celluloid ? There wasa great deal of truth in Mr. Cadett's remark as to thenecessity of investigating the properties of gelatin; forthe irregularity of those properties brought about difficultiesin the various processes in which gelatin was used. ^ Itwould be quite possible to use gelatin as a thickeningmaterial for the ink, which could be done by denuding itof its gelatinous properties, and thus the ink would not beso susceptible to atmospheric variations as gum arabic was.
Mr. J. W. HINCHLEY, in reply, said that in writing thepaper his great difficulty was, not to find matter to put in,but to decide what to cut out. He had cut out what he hadwished to say with regard to Sir Win. Abney's curves inorder to give more prominence to the practical part of thesubject, which he deemed would be more interesting for theSociety. Referring to Mr. lieid's remarks on the manufac-ture of the screens in some other way, he had made a greatmany attempts to use celluloid and other substances, but allhis attempts had ended in failure, and he was hopeless offinding any substance which would compare with gelatinin its wonderful absorbing properties. The suggestion ofadding insoluble gums to the gum solutions used in makingthe inks, was a valuable one ; but in a short time precipi-tation of the dyes might occur. He had attempted toovercome the difficulties of the hygrometric state of theatmosphere by providing an artificial atmosphere in theinstrument itself ; but this attempt failed because variationscould not be avoided, and the slightest change altered thelines. With regard to Mr. Reid's suggestion as to producingthe lines by pressing a roller on the material employed, itmust be borne in mind that they must be of a certain widththroughout and transparent. It was easy to merely drawlines, but the difficulty was to draw them of such an exactwidth as to join without overlapping, for even the over-lapping of one-twentieth the width of a line would make aperceptible difference on the screen. Owing to the absorbentcharacter of gelatin it was possible to draw the lines sothat they tilled up the space completely without overlapping,whereas with another material they would have to wait forthe lines to dry. The great difficulty, however, was tomake the atmospheric conditions constant.
THE MICROSCOPIC APPEARANCE OF VICUNACAMEL-HAIR, AND ALPACA FIBRES.
BY R. M. PRIDE AUX.
ALL three of the above present certain strongly markedfeatures in common which serve to distinguish them veryreadily from ordinary sheep's wool.
The fibres, especially the coarser ones, are compara-tively free from curl. The imbricating scales are vervclosely adprcssed to the shaft of the fibre, which fea t™serves principally to mark the somewhat artificial distinctionbetween hair and "wool/; the latter term being usuallyapplied to fine curly fibres, with strongly marked scales, andno medullary area. '
The three fibres under consideration are in aDDeirmasses of soft brownish hair, consisting for ?b e m S t
t£££Z^Twhlch much
1. Vicuua.-The fibres are the finest of the three thetouch being exquisitely soft of the mass -a lmoY a 4 a * yfeel There are very few coarser fibres present. & *
Lhe first glance at these fibres under the microscopefails to discover the presence of any scales whatever^ a
Jan. si, woo.] THE JOURNAL OF THE SOCIETY OF CHEMICAL INDUSTRY.
- ; ; • •
9
CM ly**.- - :*^/*"Kf^».
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lystv** <*-**£•«3
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Fig. 1 .—VICUNA F I B R E S .
A. Largest form, opaque black medulla; scales faintly indicated; pigment absent. B. Stout fibre, showing pigment disposed only, on leftside; medulla broad, granular, ill-defined, brown; no scales seen. C. Smaller fibre; intermittent medulla; scales faintly indicated.D. Small fibre (commonest size) ; scales unusually well indicated. E. Small fibre, showing pigment disposed, only. ¥. Fibre between theB and C types; scales well indicated. All x 290 (C x
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c
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Fig. 2 .—CAMEL-HAIR F I B R E S .
A, B, C, I). Non-medullated fibres, showing pigment-disposal. E, P, G, H, J, K, L. DiiTmmt forms of non-medullated Hbros M TVPDifferent forms of medulla fibres. Q. Medullated fibre, showing pigment-nucloi. R. Fibre showing irregular disposal of medullary Kranul iS. Large pale form of fibre; pigment finely present \ no nuclei; medulla black and opuque. All x 2U0 (C x 4|) &1
'HE OF THE SOCIETY OF GHEMIOAL INDUSTRY. [Jan, si, 1900.
region, and there are a few intermediate examples seen, ofmoderate size, and partially interrupted medulla.
Accompanying these, and but rdrely seen, is a very stoutpale fibre nearly or entirely free from pigment, with ablack opaque medulla, which can only be seen to be of agranular nature by the use of strongly transmitted light.
The disposal of the pigment is an important point. In thesmall fibres of vicuna*, the pigment is regularly and finelydistributed in uniform and faintly defined " dashes,,, through-out the fibre. These can only be observed by usingstrongly transmitted light from an Abbe's condenser, witha completely open diaphragm, when the pigment disposalwill become clearly visible, all scale and medullary structuredisappearing. Tins adjustment will invariably be found tobe necessary when the colour-particles are to be clearlyseen.
It is only on the large medullated fibres that the pigmenttakes a different form, and here are occasionally observedsmall circular patches of colouring-matter, which muchresemble the n knots " in a deal board; these are foundamongst the streaks, dashes, and lines noticed elsewhere.
2. Camel-hair.—These fibres are, on the average, muchcoarser than those of vicuna, there being a largerproportion of large medullated fibres to the finer woollierones. The scales in the latter are decidedly more con-spicuous than in those of vicuna, which would account forthe softer touch of the latter.
A very large variety of medullated fibres are present,showing various degrees of stoutness, and breadth andcontinuity of medulla.
There is also a very stout pale type of hair, occasionallyseen, as in vicuna, with a black opaque medulla. Thedisposal of the pigment is very irregular.
Some of the finest fibres appear to be without any. Thefine fibres are clear and transparent, except where irregulardashes and blurrs of pigment are seen. There is nouniform distribution, as a rule, the edges of the fibre beingconspicuously free from it. Even in the finest fibres (butquite erratically), the pigment is seen in the form ofcircular nuclei, these being large and conspicuous in thelarge medullated fibres, as a rule, but in others this featureis looked for in vain.
Fig. 3.
• • • • • - • -
ALPACA FIBEES.
A. Fibre of the fine> w h i t e c l agg . gcaleg u n u s u a l l y w e l l i n d i c a t e dB. Small pale fibre, with early trace of medulla; well scaled.G* Same, with medulla more advanced
P. Very dark fibre, showing pigment disposed only.< a )
« * • * - « .
Jan. si. woo.] THE JOUENAL OF THE SOCIETY OF OHEMIOAL INDUSTRY. 11
The medullary area is better defined than in vicuna,frequently very narrow, in proportion, and the granularmasses of which it is composed coarse and irregularlyplaced. *
3. Alpaca.—These fibres are the coarsest of the three,stout medullated fibres preponderating over the small€i woollier" ones. There is less discrepancy of diameter,on the other hand, between the largest and smallest fibres.
The amount of pigment present varies very considerably,from entire absence to dark, almost opaque brown.
In disposal it is characterised by a complete absence ofany of the " knot "-like nuclei noticed so often in the twopreceding fibres, the arrangement being, indeed, singularlyuniform, whatever the degree of intensity of colour reached.In the palest fibres the pigment is present as a very faintpowdering, the " dashes " being almost imperceptible.
On the whole, in the small non-medullated fibres thepigment disposal would be difficult to distinguish fromthose of vicuna.
The scales are less pronounced than those of camel-hair.The breadth and coarseness of granulation of the medullavaries very much; in some smaller examples it isexceedingly ill-defined throughout its course.
Table of Distinguishing Points.
Vicuna. Camel-hair. Alpaca.
The finest fibres ofthe three ; few stoutmedullated examples;scales least con*spicuous.
Largest differencein size betweenno n* and medullatedfibres.
Pigment alwayspresent, except in afew of the largeopaque - medullatedfibres.
Amount of pigmentvery uniform; dis-posal pretty regular;circular nuclei rare,and only in medul-lated fibres.
Intermediate infineness; medullatedfibres common;scales most con-spicuous.
The coarsest fibres;few non*Hiedullatcd.
Many of thesmaller fibres colour-less.
Amount of pigmentvariable ; disposalhighly irregular;circular nuclei fre-quently seen, infibres of all sizes.Distinctive streaksand blurrs wellmarked.
Least differencebetween non- andmedullated fibres.
Many fibres, es-pecially larger ones,colourless.
Amount of pigment-very variable; dis-posal very regularlydiffused, in palespecimens almost asif dyed ; circularnuclei never seen.
CINCHONA.
BY J . M. VARGAS-VERGAKA, F.C.S., ETC.
THE recent rise in the price of cinchona bark having givensome hope of our being able to enter into competition withthe Indian and Javanese planters, the object of the presentcommunication is to describe the results of some analysesI have made of wild and cultivated barks, as it seemedlikely that these might be interesting to manufacturers.
It is well known that in former years, when Colombiaexported cinchona, very few barks gave more than 3 percent, of sulphate of quinine. The barks that came up tothis percentage were indeed very few, and barks containing1*5 and 2 per cent, of quinine sulphate were consideredfairly good samples.
Some years ago I had occasion to analyse some samplesof Cuprea bark from Los Llanos, which had been stored inwell-ventilated rooms, so that there wras no fear of the barkaltering or decomposing by keeping. The analyses which1 made gave a mean of 0#5 per cent, of sulphate ofquinine, and, although some native chemists reported asmuch as 3 per cent., I failed to obtain a higher per-centage by repetition of the analyses, which gave con-cordant results. These analyses made it clear that noreliance could be placed on the work of the native chemists.
The cinchona fever, as was to be expected, almost com-pletely exhausted the Colombian forests, and those plantsthat are now to be found in the woods cannot be more than20 years old.
As the extraction of the bark in bygone days was a veryprofitable business, it was not unfrequent to find samples
mixed with all sorts of rubbish. The Quineros were notvery particular as to the quality of bark, their chief aimbeing to obtain as many bales as possible, without anyconsideration as to its content of alkaloids. Thus I amunable to determine whether there has been a favourablechange in the constitution of the bark, or whether theincrease in the yield of quinine is due to the extra carewith which the extraction is now made.
r\ - ;, • Quinine Cinchoni-Qiumne. gS l p h a t C i d i n c .
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According to J. Holmes (Chein. and Druggist, 40 ,580 —581), who analysed some varieties of Colombian barks,the Ledgeriana did not give any cinchonidine, the Tunaonly gave 0*40 per cent., and the Succirubra 2*77 percent. The Tuna examined bv Mr. Holmes was cultivated,and came from a rich variety found wild in the forests near
v'
Chaporral: the variety I examined is found wild in the estateof l)oa, and used to assay 1*5 to 2 per cent., and never hasyielded any cinchonidine. Undoubtedly the new plants aremuch richer than the old ones, confirming De Vrij's theories ;but while the barks from cold and high regions of the Andesyield a richer bark, the trees of the warm and moist valleyshave remained unchanged. Although Mr. Holmes foundcinchonidine in the cultivated Succirubra, I failed to detectany, having carefully examined the quinine with themicroscope, as the wet reactions showed me the absenceof this alkaloid. Can this be attributed to the soil andclimate ? It is also interesting to note that, though in theSuccirubra there is not a large variation in the yields ofquinine from the trunk and branches, this variation is verygreat in the Ledgeriana.
As far as I have been able to ascertain the Colombianbarks from the cold Andes are much richer in quinine thanin the olden times, and the cinchonidine has almost dis-appeared from these barks. Whether this is an advantageto manufacturers or not I cannot decide, as commercialinterests must be taken into consideration.
A curious fact in connection with the Legeriana, old andnew, is that whilst the old is the same bark as the new, buthas been kept under most unfavourable conditions for someyears, being exposed to the rain, wind, and sun, so that theowners thought this bark had become completely useless,on analysis it proved equal to the freshly gathered bark.
DISCUSSION.
Mr. DAVID HOWARD wrote as follows :—The questionof the supply of cinchona bark is one of very great interestFormerly the native bark in the forests of South Americawas the only source, now uncultivated bark is almostunknown in commerce. At present almost the wholesupplies come from Java. Owing to the rich soil and greatamount of land suitable for cinchona cultivation and to thegreat skill shown in selecting the best varieties of bark andm cultivating k, the practical question of successfullybringing bark into the market depends on bein<t able toproduce it as advantageously as the Java planters. Thebark grown there is of very fine quality, averaging formanufacturing bark over 5 per cent, of sulphate of quinineIt is difficult to learn exactly what it costs to grow it, butthe best information to be had seems to show that 35 to40 cents per kilo, leaves a margin for profit
For commercial success, therefore, bark must be producedat certainly not more than 3d. to 3±d. per pound for a5 per cent. bark.
The difference in tests of bark made by the author ardby other chemists is not surprising. A study of the comparative results obtained by the leading Amsterdamchemists from the same parcels of bark as occasional^published in the catalogues of the Amsterdam cinchona
12HE JOURNAL OF THE SOCIETY OF OHMICAL INDUSTRY.
[Jan. 31,1900.
sales, show what wide divergencies are possible betweenchemists of high standing, and show what great errors maycreep in, either in sampling or in testing, or in both.
One of the most interesting results obtained is theanalyses of suecirubra bark showing no einchonidine. Nospecies jields bark with more varied alkaloidal contentsand relative proportion of the alkaloids than succirubra,hut we have never found it free from einchonidine.
The final separation of quinine and einchonidine is verydifficult, and if ether is used, specially in a hot climate, aconsiderable percentage of the latter alkaloid may escapedetection.
The best method of separating small proportions ofeinchonidine seems to be to separate the greater proportionof quinine by crystallisation of one of its salts, preferablythe hi-sulphate, before attempting the separation of thealkaloids bv ether.
Meeting held on Friday, January othy 1900
DR. J. GttOSSMANX IX THE CHAIR,
equal amount of gas out of cannel coals, as that producedin technical practice is the most extreme white heat ob-tainable by ordinary fuel. I tried different temperatures ona sample of cannel coal, and I found-that only 60 to 70 percent, of the gas could be obtained by heating the coalin an ordinary muffle furnace for gold and silver assays,the temperature being about 1,000° C.
The furnace used by myself was a Fletcher furnace fordraught. I then determined to use unglazed porcelainretorts with the Fletcher injector furnace, and I constructedan apparatus for the purpose, the details of Avhich arcgiven below : —
Fig. 1.
A LABORATORY METHOD FOR THE ANALYSESOF COALS FOR GAS MANUFACTURE.
BY J. G. A. UIIODIX, F.I.C., ETC.
FKOM the point of view of the analyst this subject presentsmany difficulties, as the technical users require to know notonlv the chemical constituents of the coal, but also certainphysical properties, the determination of which falls ratheroutside the sphere of the ordinary analytical practice.
In consulting most of the written works on gas manu-facture and the assay of the materials for the purpose, thechemist finds not what he wants, but a description of acertain amount, or rather large amount, of special appara-tus designed for use in the gas works. However plausiblethe apparatus may be, and however ingenious, it isgenerally too cumbersome, expensive, and arbitrary for useby the scientific chemist. Nothing is left to the skill andjudgment of the analyst, and everything depends upon theapparatus in the first instance, and the instructions aceom-panvinff the same in the second instance. To take anexample : —
When you are requested to determine the amount of gasdeveloped from a ton of coal, and its illuminating power,vou are supposed to use iron retorts 3 feet long, and gasholders weighing something like half a ton, and all kinds ofgauges and apparatus for regulating the flow of gas, &c.You are told to use a thousandth part of a ton, roughly1 kilo., for the experiment, and also to use pieces of the sizeof a walnut. The question whether an average sample canhe obtained in this way is not discussed, and you are told torepeat \our determination several times and take a mean ofthe results.
In considering the question I could not exactly sec thereason why work on this large laboratory scale should givea better result than work on a smaller scale, selecting yoursample more carefully, crushing the coal to smallerparticles and quartering the sample, and selecting a iinaiexample of, say, 100 gr.ns. In fact, I made up my mindthat a sample obtained in this way ought to be morerepresentative than the sample obtained in the other way,even if the latter be larger, considering the size of piecesrecommended. All practice of mineral, metal, and oreanalyses has proved that if a proper average sample bechosen it can be made fairly representative, even if small inquantity. When it is a question of gas coals, however,where the gas evolved has to be examined as to its illumi-nating power, the sample must not be too small. Werequire at least 20 to 30 litres of the gas for the determi-nation of the illuminating power. A specimen of lOOgrms.is quite sufficient for this purpose. This is so much more tobe recommended as the temperature required for driving an
SCHEME OF ARRANGEMENT FOR DEVELOPING- GAS.
The apparatus consists of the following parts:—B is aFletcher injector furnace, and through its side a porcelainretort marked A is fitted by drilling a hole through thematerial. The neck of this retort communicates with anair condenser, the tube having a branch C closed by acock. I constructed the air condenser out of small Woulffbottles with a bottom tubulure,which can serve for letting thetar out when the apparatus is cleaned. The main part of thecondenser is made out of long U-shaped tubes aboutr> ft. in length and 10 mms. internal diameter connectedwith these bottles with rubber ligatures, as shown in theillustration. Five or six of these tubes are sufficient for allpractical purposes. For purifying the gas I use a large sizeFresenius tower, which I charge with soda lime. Two ofthese towers might be used, one charged with lime and theother with ordinary ferric hydrate, such as used in the gasworks; but the soda lime, on account of its physicalproperties, is better for laboratory experiments, as it ensuresthe apparatus against accidental stoppages. From thispurification tower F the gas is led into the gas holder G.This gas holder is constructed both for measuring the gasand the regulation of its subsequent flow, and I have chosena very small diameter in order to get large readings on thescale. The divisions being about 3 cms. for 1 litre, thebell is roughly 20 cms. diameter and 1 m. long, and fittedwith tube for holding thermometer, &c. The counterpoiseis also arranged on well-made rollers, and the gas holdermade so as to be perfect and as smooth in its run as anyregulator which it is possible to obtain. When making anexperiment I charge retort A with 100 grms. of the coal tobe analysed, and through the tube C I displace all the airin the condenser and purifying apparatus either by gasfrom the mains, or else by working a small charge of10 grms. of coal in a small retort through the same. Theunoccupied ™iume of the condenser and the purificationapparatus in the retort being only a few per cent, of thevolume of the gas holder and the gas to be measured, thefilling of the apparatus from the main would not cause anyappreciable error apart from the great saving in time andlabour. As it is always desirable to control results byrepeated experiments, 1 prefer to work on three charges of50 grms., one after the other, and to let out the gas fromthe first charge, making an approximate estimation of the
Jan.3i, 1900.] THE JOURNAL OF THE SOCIETY OF OHEMIOAL INDUSTRY. 13
illuminating power and utilising gas from the two lastcharges for the accurate determination of the illuminatingpower.
For some classes of coals 150 gnus, might be found tohe too much for the capacity of the gas holder which Ihave constructed, and which holds 30 litres. In this casethe first working off of 50 grms. will show what quantitywill he carried. One mode of procedure is as follows : —
I work the charge off by heating the retort slowly duringthe first five minutes, and afterwards increasing the heat assoon as possible to an intense white heat. It is generallynext to impossible to prevent all tar from entering thegas holder, but in the construction which I have made thisholder can be easily cleaned from the inside. In about20 minutes the charge is worked off, and the apparatus isdisconnected from the gas holder, which is allowed to standfor a short time to allow the gases to assume a uniformtemperature, which is then observed together with thebarometric pressure. Afterwards, the volume is reducedto gas of a temperature of 60° F., and 30" barometricpressure (the gas saturated with water vapour). The cokeformed out of cannel coal can easily be removed out of theretort by shaking the same, a thing which is not the caseAvith caking coals, which require a rather larger retort madeof iron to screw apart. When the gas has been measuredthe gas holder is connected with the burner on the photo-meter, and you can then easily proceed to take theilluminating power of the same. According to the usualcustom you regulate your flow of gas so as to have,roughly, five cubic feet passing in the hour from the burner,and it is customary for gas from cannel coals to utilise anordinary bat's wing burner. For coal-gas an Argandburner is required, the normal burner being described veryparticularly in the instruction for gas referees. For thosewho prefer to do so, a burner fulfilling exactly the require-ments can be obtained from any firm supplying chemicalapparatus.
The regulating of the flow of gas is done by means of alarge tap with a rather long lever. The approximate flowof gas is observed on a suitable indicator such as, forinstance, Thorpe's instrument. The actual flow of gas istaken by time observations and measurement on thegas holder, and the pressure in excess of barometricpressure by means of a small water gauge on the holder.
1 do not propose to give the exact operations with thephotometer, which are all well known. I onlv wish toremark that for the measurement you ought always tocompare with at least two spermaceti candles, as the readingsbecome larger than what is the case when only one isemployed. It is self-evident that even with the bestarrangement for regulating the flow of gas it is an utterimpossibility to make this flow to correspond absolutelywith five cubic feet an hour, and hence corrections have tobe made to reduce the actual result to the result obtainablewhen the exact amount of gas is passing. The ordinaryprocedure for doing so is to reduce the gas volume perhour as observed by the gas holder to 60° F. and 30"barometric pressure, then afterwards to divide by li\e, findto divide the result in candle-powers obtained before by thisfigure. Correction is also made for the amount of sper-maceti burned per hour, and the c.p. reduced to c p.corresponding to candles burning 120 grains per hour.
I may say there are very grave objections to this methodof calculation, and the results are not absolutely correct andaccurate. For instance, when the gas burns in air of lessdensity, a smaller bulk of normal temperature and pressureis burned than if the air had this normal temperature andpressure. As the illuminating power depends upon thefierceness of the combustion, it is evident that a somewhatlarger correction ought to be made for the low pressure, asthis gas, when issuing, does not come in contact withas much and as dense oxygen per surface unit as itshould do when burned under normal conditions. Theoreti-cally, a gas issuing from an orifice has work exertedupon it by the weight of the gas holder, this work beingconverted to heat when the gas issues from the narrow slot,the heat being retained by the issuing gas. This gas alsoexerts a certain amount of work upon the surrounding air,the equilibrium of temperature being slowly brought about
by the cooling effect of the air into which the. gas issues.Under the same conditions of temperature and barometricpressure we can therefore supply a different amount ofenergv to the issuing gas, inversely proportional to the sizeof the slot in the burner and directly proportional to thepressure above the atmospheric pressure exerted by thegas holder. If the same volume of gas issues per unit oftime, your pressure depends upon alteration of the orificein the burner. If the formula usually used for reducingthe illuminating power to the normal conditions be correct,such an alteration in the potential energy of the gas wouldnot affect the illuminating power.
The referee " tabular number "a re calculated from theformula—
V =r V 11 ~
1 7 ' 6 4
460 + t1
This formula is identical with the formula
(1)
V •= (2)
\r
n
a =
a, =
1 (30 - cti) (1 + n (<! - 0 )
observed volume,„ barometric pressure in inches.„ temperature in degrees Fahrenheit.„ coefficient of expansion of coal gas per
degree Fahrenheit.- pressure of saturated water vapour at the observed
temperature,pressure of saturated water vapour at 60° F.
The experimental evidence required for arriving at anaccurate formula for the purpose of reducing illuminatingpower can be obtained by burning the same kind of gas inburners with different orifices under the same conditions ofpressure and temperature. Another factor that will alsohave to be taken into consideration is no doubt the moisturein the air, as this will strongly influence the cooling effectupon the flame from obvious reasons.
With reference to the photometer to be used thisinstrument may be of any construction which allows anaccurate estimation of candle power. The main part of theinstrument, namely, the photometer head, ought to be of aconstruction which is less liable to personal errors than theold-fashioned grease spot, and we have in the LummerBrodhun photometer head an excellent development in theright direction. This photometer head has an arrangementof prisms which enables you to observe and compare thelight reflected from the two sides of a white porcelain discin one visual observation, and I find that this instrumentwill indicate very minute variations in candle powerdistinctly, long before any effect can be observed on agrease spot. Messrs. Hartman and Braun, of Frankfort,make a large photometer provided with this class ofphotometer head, which has been adopted as a standard atthe German national laboratory at Charlottenburg. i dopot, however, quite approve of'the way of mountTng thisinstrument, and I made slight modifications in the same,suspending th.3 bars from brackets on the wall &c, theinstrument being made for me by the Central En°-ineerincrWorks, King Street West, .Manchester. Amongst otherthings I provided the tube on the photometer which servesfor holding the gas burner with a Thorpe's indicator, whichshows approximately the flow of gas.
From the above you will see that the only apparatusrequired outside what is generally found in any laboratoryare the photometer and gasholder. The photometer is ofcourse useful for other purposes although its use may notbe very extensive in the analytical practice. The actualcost ol this apparatus is, when constructed on my planabout 2:J/., which is not very much out of the way. Withreference to the other determinations to be made I can onlyrecommend certain methods. For determinations of volatilematter, take a small crucible and enclose the same in alarger one, surrounding the little crucible with finelvpowdered charcoal, then heat the whole to a bright redheat, and take the loss as volatile matter. The result*agree far better than what is obtained when heating directover a burner in a platinum crucible. For instance in twodeterminations of the same cannel coal I got 34-6 and 35.3
14 THE JOURNAL OF THE SOCIETY OF OHEMIOAL INDUSTRY. [Jan. si. l&oo.
per cent, volatile matter, A slightly higher result would ofcourse be obtained by increasing the temperature, butexpressed as a percentage of weight the gas evolvedbeyond a bright red heat is very inconsiderable.
I must remark, however, that the heating must becontinued for a considerable time. Constant weight isobtained only after a couple of hours , heating. Thedetermination of ash is of course well known to all of you,and the fact that hygroscopic water has to be determinedby direct weighing of the water. The determination of thespecific gravity of a coal is of great importance, and noother method except the pycnometer method is sufficientlyaccurate. It is also to be recommended to put the pycno-meter under the receiver of an air pump in order to take awaygas bubbles adhering to the particles of coal. I mentionthis as some classes of coal when heated in water give off acertain amount of soluble substance. Sulphur can bedetermined by heating with mixed carbonates of potashand soda in a roomy platium crucible using a large excessof the reagents, and heating over a small luminous flamefor at least an hour and a half before increasing the heatto anv considerable extent. The ordiiuirv method ofusing lime in the combustion tube can also be used, and theresults of the two methods agree well, but in both eases carelias to be taken against quick heating. The analysis of thecoal gas produced can of course be carried out accordingto tbe choice of the analyst himself. I find that bvadhering to these instructions as given above, results areobtained agreeing with practical working exceedinglyclosely, and closer by far than the results obtained in theMiiall furnaces with iron retorts used ordinarily in gasworks. With this latter apparatus it has always been afact that the analyst lias found a smaller quantity of gas ofa higher illuminating power than that which is obtained inpractice. This no doubt depends upon the fact that theheat used is not intense enough for driving out the lasttraces of gas. Working on the lines that I have put down,I arrive at a slightly larger quantity of gas of approximatelythe same illuminating power as that obtained in practice,tbis depending upon the faet that the temperature of thesmall injector furnace can be raised to anything thatis practicable.
DISCUSSION.
In the discussion which followed several speakers whohad had considerable experience in analysing and testinggas coals for illuminating purposes, both in the laboratoryand also in the works, expressed an opinion that laboratorymethods were practically valueless from a gas manager'spoint of view. The only practical method of testing coalintended to be contracted for in large quantities was bypassing, from r>0 to 100 tons through the works. It wasthought that Mr. Khodin's apparatus would give too lowresults, both as regards the quality and quantity of gas,on account of the large condensing area. Having to startwith a cold retort which had to be heated gradually, wouldresult in condensation of the rich benzol products, thetoluene and naphthalene, which ought to go into the gas.
The CHAIKMAN explained that Mr. lihodin haddescribed a laboratory method for the analysis of a numberof samples of coals. They all knew that analyses given intext books did not always give the same results, but theywere considered to be near enough for comparative purposes.He expressed his disappointment that Mr. Rhodin had notshown in his paper in what respect his method agreedwith or differed from the old methods, and how muchcloser would be the result obtained by the same coal on alarge scale. If Mr. lihodin could give the figures theywould be exceedingly useful.
Mr. RHODIN, in reply, said that he only wished to showone method whereby research could be made which wasless cumbersome than so-called laboratory methods, andhe maintained that by his method better results could beobtained than by a retort which contained one kilo. Allhe attempted to do was to reduce the present u laboratory "methods to a smaller scale. Everybody knew that it wouldnot represent large quantities of coal, but it would give someidea of the quality of the coal under examination. Hecontended that, the sm;|]] apparatus being, made of o-lnss
the heat carried to the gas would graduate down to thelower temperature very gradually. He could not answerthe points raised on the technology of the gas manager, norput an analysis before them which he had been makingfor others, but he would furnish the figures required by theChairman at some future meeting.
&tttion.
Meeting held on Friday, December 22nd, 1899.
MR. T. J. PARKER IN THE CHAIR.
A CONVENIENT LABORATORY APPARATUSFOR THE GENERATION OF GASES.
BY N. J . LANE.
Tins is a modification of the apparatus described inPresenilis' Qualitative Analysis. Its advantages are thatit requires no regular stand and is simpler in construc-tion, consisting of a globe ground into the neck of anaspirator which is connected by thick rubber tubing withanother aspirator of larger capacity placed above it ona shelf. The globe is charged through its neck, a diskof lead being placed in the contraction to prevent thematerial used (CaCO3, FeS, &c.) dropping into theaspirator below. The flow of gas is regulated by astopcock, and when shut off there is no waste, the gasforcing the acid back into the large aspirator above. Inlaboratories where the apparatus is being constantly used, itis convenient to have a three way-cock in the cork of theglobe, or to use a doubly perforated cork closing one holewith a glass rod, so that on removal the neutralised acidmay be drawn off without disturbing the rest of theapparatus. Of course any necessary purifying tubes maybe attached to the exit tube.
DISCUSSION.
Dr. D. WOODMAN asked why the lower bottle was solarge.
Mr. N. J. LANE replied that the calcium chloride solutionwent to the bottom, and with less space, action would sooncease.
THE ESTIMATION OF COPPER I N CYANIDESOLUTIONS.
BY J . E. CLENNELL.
AMONG the elements which interfere with the successfuloperation of the cyanide process there are few, if any,which are more dreaded than copper. Rightly or wronglythis metal is made to bear the responsibility of a la r α-epercentage of the failures which occur in the treatment *ofcomplex ores. That this opinion is in a measure wellfounded, may be demonstrated by the simple experiment ofshaking up a small quantity of crushed ore containingcarbonate of copper in a small flask or test tube withcyanide solution. Even with extremely weak solutions afew seconds contact is sufficient to enable one to detect thepresence of copper with certainty, if a little of the mixtuiebe filtered and the filtrate tested, after acidulatinff bvadding a drop of very dilute potassium ferrocyanide Theintensity and completeness of the reaction vary considerablyhowever in different ores, and we must beware of anyhasty generalisation. The writer has met with cases inwhich an ore containing 5 per cent, of copper could betreated with a moderate consumption of cyanide and asatrfaotory extract™ of the gold at>d Silver valuesobtained In such cases the copper existed as sulphide incomparatively large crystals, which from their physicalcondition probably resisted the action of the solvent Inother ores the presence of 0-4 per cent, of copper (ascarbonate) .made treatment impossible from an economicpoint oi view. It is obvious, therefore, that a sin p edetermination of the percentage of copper in the ore $
Jan. si, 1900.] THE JOUBNAL OF THE SOCIETY OF OHEMIOAL INDUSTRY. 15
not enable one to decide as to its adaptability or otherwiseto cyanide treatment.
The first and most obvious suggestion in such a casewould be to determine by a test on a small scale whatextractions could be obtained, and what consumption ofcyanide may be expected with the ore under consideration.So far as extraction is concerned, this question may besettled with tolerable accuracy by this means, especially ifthe results be confirmed by a test on as large a sc-ile ascircumstances will permit. But with regard to the con-sumption of cyanide an ambiguity occurs to which, so faras I am aware, attention has not heretofore been drawn.If a cyanide solution containing copper be tested in theordinary way by silver nitrate, a fairly definite end-point isobserved. If, however, another portion of the same solutionbe tested, with previous addition of potassium iodide, adifferent and considerably lower reading will be obtained,likewise quite definite. The mean of a large number ofexperiments made with copper-potassium cyanide solutionsof various strengths containing known quantities of copper,showed, when potassium iodide was added before titrationwith silver nitrate, an apparent consumption of 3*5 partsby weight of potassium cyanide for every part of copperdissolved. When no iodide was added, the apparentconsumption averaged 2 * 5 parts of potassium cyanide forone part of copper. The tests were made by dissolving aknown quantity of copper in dilute nitric acid, boiling toexpel red fumes, adding alkali (caustic soda or carbonate ofsoda), until the copper was completely precipitated and theliquid showed a slight excess of alkali, then immediatelyredissolving the precipitated copper in an excess of solutioncontaining an exactly known quantity of pure potassiumcyanide. By this means the copper was obtained in theform of double cyanide without any loss of cyanogen takingplace. It was found—
(1) That when the solution was very strongly alkalineno definite reading could be obtained in the absence ofpotassium iodide; in such cases the addition of silvernitrate produced a blackish precipitate, and finally thewhole liquid acquired a blackish-violet tinge.
(2) That variation in the quantity of potassium iodidewithin wide limits (in one set of experiments between• 05 and 1 grm.), did not perceptibly affect the result.
I am at present unable to give any satisfactory explana-tion of these curious facts. Until some light is thrownupon this point we cannot decide whether the indicationgiven by silver nitrate with or without iodide correctlyrepresents the free cyanide in the solution. Probablyneither indication is a correct measure of the efficiency ofthe solution for the purpose of gold and silver extraction.
It will be generally admitted, however, that under thesame conditions the more copper is dissolved the less Avillbe the efficiency of the cyanide solution in performing otherwork. As in the case of the corresponding zinc compound,the double cyanide of copper and potassium may perhapsbe capable of dissolving a small quantity of gold and silver,but its solvent power would be far less than that ofa pure cyanide solution containing the same weight ofcyanogen.
A determination of the amount of copper present in thesolution obtained after treatment of the ore under definitelyknown conditions will accordingly give us very valuableinformation, and will go far towards deciding whether theore is or is not suitable for cyanide treatment. For thisreason a description of the following method for makinga rapid approximate estimation of the amount of copperpresent in a cyanide solution may be of some interest.
Attempts to separate the copper from complex cyanidesolutions, without going through the tedious process of
from slightly acidulated cyanide solutions bysulphuretted hydrogen was found to be very imperfect. Asomewhat better precipitation was obtained by boiling withsodium hyposulphite and acidulating with sulphuric acid,but the results were not always reliable. Various othermethods suggested themselves, but were rejected, as theygenerally involved concentration of a large quantity of
liquid to a small bulk. This was inadmissible, as the objectof the present investigation was to obtain a rapid methodwhich would be accurate enough for technical purposes.
The method described below seems to answer therequirements, and is so simple that with a little practicefive or six determinations can be easily made in an hour.
This method depends upon the facts—(1.) That cyanide of copper is precipitated from solutions
of the double cyanides of copper by the addition of dilutemineral acids.
(2.) That hydrocyanic and carbonic acids have little orno action on methyl orange.
(3.) That when an acid is added gradually to a mixtureof a double cyanide of copper with free alkali-metalcyanides and caustic or carbonated alkalis, no precipitationof the copper occurs until the whole of tbe alkalis and freecyanides have been neutralised, the first appearance of apermanent white precipitate of copper cyanide correspondingprecisely with the point at which the solution becomesalkaline to methyl orange.
The determination is carried out as follows :—A measuredvolume (say from 10 to 50 c.c.) of the liquid to be tested,which must be perfectly clear and transparent, is placed ina 100 c.c. measuring flask, and dilute sulphuric acid isadded drop by drop from a burette with continual shakinguntil the turbidity formed ceases to disappear, but leavesthe liquid slightly milky. The reading of the burette mustnow be carefully noted. This point is in general perfectlysharp and definite. A further quantity of sulphuric acid isnow added, more than sufficient to precipitate the whole ofthe copper. (This may be ascertained if necessary by apreliminary experiment. A little of the liquid is filtered off.If the filtrate gives no further precipitation on additionof more sulphuric acid, and if it is distinctly acid to methvlorange, the reaction may be considered complete.)
The copper being thrown down as a white curdvprecipitate of copper cyanide, and a slight excess ofsulphuric acid being present, the reading of the burette isagain taken. Let us call the difference of the tworeadings A.
The 100 c.c. flask is now filled up to the mark withdistilled water and the contents thoroughly agitated. Theprecipitate generally settles rapidly in a flocculent condition.Now filter off 50 c.c. of the supernatant liquid, taking careto use a filter paper free from iron or other substancessoluble in acids.^ The filtered liquid is now titrated with the addition of a
single drop of methyl orange of 0-25 per cent, strength,using a standard solution of sodium carbonate, until thepink colour changes to a scarcely perceptible yellowishtinge. The strength of the sodium carbonate solution mustbe accurately determined with reference to the sulphuricacid solution used in the first stage of the test. A decinormalsolution is convenient ; it is not necessary that the twosolutions should be of exactly equivalent strength, but theexact value of a given volume of one solution should beknown in terms oi the other.
The number of c.c. of sodium carbonate used, multipliedby 2, gives us very approximately the equivalent of theexcess of sulphuric acid beyond that required to precipitatethe copper. L l
r ^ *Z i ? ° f C*°- o f s o d i u m carbonate used foro0 c.c. of the filtrate, and C = number of c.c. of sulphuricacid equivalent to 2B, then A - C = number of c c ofsulphuric acid equivalent to copper present. * "
The operations are very simple, the essential pointsbeing to note carefully the exact point at which permanentprecipitation of copper cyanide takes place, the amount ofacid added beyond this point, and the precise amount ofsodium carbonate added. The end-point with methvlorange leaves something to be desired in point of sharpnessbut by carrying out the test exactly as described andarranging matters so that the final bulk of solution is about60 to 70 c.c, results may be obtained which are more thansufficiently accurate for any technical purpose. A triflWerror (which makes the calculated percentage of eless than the truth) is introduced owing to the
16 THE JOURNAL OF THE SOOIETY OF OHEMIOAL INDUSTBY. [Jan. 31,1900.
occupied by the precipitated copper cyanide beingdisregarded.
Variation within tolerably wide limits in the amount ofcopper, the quantity of free cyanide and alkali, and theamount of sulphuric acid given in excess of that necessaryfor precipitation of the copper did not appear to have anyappreciable effect ou the result.
The results were unsatisfactory when less than • 02 grm.copper was present: when the proportion of copper wasreduced below this point, the apparent percentage increasedprogressively as the quantity of copper was diminished.
When very much alkali is present it might be advisableto use a stronger acid for the preliminary neutralisation toavoid undue dilution, adding the decinormal acid only Avhennear the point of permanent precipitation of coppercvanide.
The following illustration will perhaps serve to elucidatethe modus operandi more clearly: —
20 c.c. of copper cyanide solution containing anexcess of free cyanide and caustic soda were taken forthe test, and introduced into a 100 c.c. measuring flask.(In this instance the total cyanide present was equivalentto *O9 grm. KCy, and the caustic alkali was equivalent to•11 crnii. XaOH.)
Sulphuric acid (rather stronger than decinormal) wasdelivered from a burette with continual shaking. After11'15 c.c. had been added a permanent cloudiness wasobserved. The reading of the burette was now noted. Afurther quantity of sulphuric acid was then added,amounting to 6 c.c, so that the burette now stood at17' 15 c.c. The neck of the flask was washed down withdistilled water, the contents were agitated, the flask filledup to the 100 c.c. mark with distilled water, again wellshaken until the contents were thoroughly mixed, andallowed to subside for a few moments. The supernatantliquid was then decanted through a funnel with a drytilter-paper into a measuring column until 50 c.c. ofperfectly clear liquid was obtained. This was transferredto a small Erlenmever flask, the column rinsed out withdistilled water, and a single drop of • 25 per cent, methylorange added by means of a dropping tube. The contentsof tlie flask now assumed a pale but distinct pink tinge ;sodium carbonate (approximately decinormal) was addeduntil the pink tinge was scarcely perceptible, then, verycautiously, a few drops more until a very faint golden-yellow appeared. In this test 1*9 c.c. of sodium carbonatewere needed. Hence for 100 c.c. we should require 3*8 c.c.Previous comparison of the two standard solutions showedthat 1 c.c. of the acid wa< equivalent to I ,185 c.c. of thecarbonate. Hence 3 '8 c.c. of carbonate are equivalent to,V21 e.c. of acid, and f> — :? - 21 or 2*79 c.c. have beenconsumed in precipitating copper.
The sulphuric acid solution may be standardised bydissolving known weights of copper in nitric acid, boilingto expel nitrons fumes neutralising with caustic soda,adding cyanide until a perfectly clear and colorless liquidis obtained, and titrating with the standard acid as abovedescribed.
The following results were obtamrd with a coppersolution containing 0*2 per cent. Cu., and will illustrate thedegree of accuracy of which the method is susceptible : —
the indication obtained with 0*02 grm. copper correctlyrepresents the actual percentage of copper, the followingtable shows the amount of divergence observed when theamount of copper was reduced. A 0*2 per cent, coppersolution was used in each case.
As before stated, the results obtained with smallerquantities cf copper Avere iips»tisfactory. Assuming that
This method of determining copper in cyanide solutionsis, of course, not applicable to liquids containing, otheringredients precipitable by sulphuric acid from theirsolutions in cyanide, as for example, zinc and silver.When iron is present (as ferrocyanide), the copper isimmediately converted into the well-known and character-istic reddish-brown ferrocyanide of copper as soon as thealkali has been neutralised. This precipitate is verydifficult to filter, and in any case the test is not valid inpresence of ferrocyanides, Sulphocyanides and ammoniumsalts do not appear to interfere materially.
Where interfering metals are present it becomes necessaryto eliminate them before making the test, and this wouldseem at first sight a serious limitation to the usefulness ofthe method. Experience with a large number of ores andtailings has shown however that, owing to the extraordinarilyrapid action of cyanide on copper compounds when a puredilute solution of potassium cyanide has been allowed toleach through, or has been left in contact for a short timewith a sample of cupriferous ore or tailings, the liquordrawn off contains practically no other impurity than thedouble cyanide of copper and potassium. In all suchcases the method herein detailed may be successfullyapplied.
It is also obvious that it might be applied with certainmodifications to the estimation of copper in ores andby-products. It would be essential (as in all knownmethods for the accurate estimation of copper), to obtainthe metal in a solution free from iron, but it would not benecessary (as in the iodine process) to eliminate all freemineral acid. Having obtained the copper in an acidsolution free from zinc, iron, or other interfering metals, aslight excess of caustic alkali is added, then cyanide untila perfectly clear and colourless liquid is obtained. Thissolution is then transferred to a suitable measuring flaskand titrated in the manner described with standard solutionsof sulphuric acid and sodium carbonate. I t wouldprobably be advisable to make a check determination witha quantity of pure copper approximately equal to theamount obtained in the extract from the sample of oretested. The end-point is decidedly more definite than inthe case of the well-known and much employed " cyanide "process of copper estimation,
A NEW PROCESS FOR SENSITISING PAPER AND
OTHER SURFACES.
BY ROBERT C. SCUUPPHAJJS, PII.B.
THIS new process of sensitising paper and other surfacesis the invention of DΓ Johannes Meyer, a practising pin"sician of Brooklyn. It is based upon the application ofone of fte phosphates of silver to the s u r f a c e d be sensi-tised in conjunction with an organic acid. The^BritishJournal of Photography hpeaks in its issue of the 17th ofNovember 1899 of this invention as the rediscovery of oneof the oldest printing processes, namely Dr. Fvfe's andincidentally charges the inventor with a lack of familiar^
Jan. 3i, mo.] THE JOURNAL OF THE SOCIETY OF CHEMICAL INDUSTRY. 17
with the older literature of the art. In this particularinstance I think it is well that Dr. Meyer knew nothing of•the earlier work and comparative failures of Dr. Fyfe andMr. Maxwell-Lyte, for such knowledge might have pre-sented him from making an invention which in its sim-plicity and beauty is a boon to every photographer. Thefriendly critic is in error, however, when he speaks ofDr. Yyie's process as " not materially different from thatAvhich has just been patented/* meaning Dr. Meyer's,He quotes quite freely from Hunt's Kesearches on Light,published in 1854 in support of his position. I quote fromthe same author's " A Popular Treatise on Photography/ ,
Glasgow, 1841, page 21 :—
" Dr. Eyfe appears to have been the first to suggest theuse of the phosphate of silver as a photographic material,but I am obliged to confess it has not, in my hands, provedanything like so successful, as, from Dr. Fyfe's description,U was in his own.,,
And this same passage appears in Hunt's " Manual ofPhotography/' London and Glasgow, 1854, p. 120. WhatDr. Fyfe actually did, was this :—
(1.) He produced a precipitate of silver phosphate in thefibres of the paper by double decomposition between sodium
phosphate and silver nitrate.(2.) He coated paper with a solution of silver phosphate
in ammonia or ammonium carbonate.(3.) He spread a paste made of precipitated silver phos-
phate, dried in the dark, with spirits of turpentine andCanada Balsam on canvas.
Dr. Meyer was searching for a paper more sensitive thanthe ordinary commercial article, and certain theoreticalconsiderations led him to experiment with the silver phos-phates. After establishing their solubility in certainorganic acids such as tartaric, citric, and succinic acids, heapplied silver phosphate dissolved in an organic acid topaper, and in further pursuit of this kind of work, dis-covered the emulsion of silver phosphate and tartaric acid.It took many months of patient research before the con-ditions were determined under which this remarkableemulsion is formed. Before going into the details ofpreparation, I will say that the metaphosphate and pyro-phosphate do not differ materially in their behaviour fromthe orthophosphate, but that by phosphate simply, theorthophosphate of silver is meant. To make the emulsionof silver phosphate and tartaric acid, which has given suchgood results in making photographic prints, 4 grms. ofsilver nitrate in aqueous solution are precipitated by4-7 grms. of sodium phosphate dissolved in half a litre ofwater. The precipitate is washed carefully by decantation,and by tapping and cautious removal of water brought tothe volume of 32 c.c. From 18 to 20 grms. of tartaric acidare dissolved in an equal number of c.c. of cold water, andwhile this solution is added as rapidly as possible to thephosphate precipitate, a quick rotary motion is imparted tothe containing vessel, preferably a wide-necked bottle madeof yellow glass. The experienced observer will notice achange of colour, the yellow phosphate held in suspensionturns into a whitish cream. We have now about doublethe volume of the original mixture as a stiff jelly. Bykeeping it at a temperature of about 38° C , it is renderedmore fluid. In this fluid condition it is suitable for coatingpaper, plain, albumenised, or otherwise prepared, by meansof a flat brush or of suitable machinery. The proportionsabove given are the best for practical work, they also yieldgood results when much larger quantities are employed.It is possible, however, to obtain the emulsion with a gooddeal less of tartaric acid, say 8 grms. in 8 c.c. of water tothe 32 c.c. of mixture previously referred to. With theseproportions the emulsion will set more readily, and it maybe better for a beginner to first try these. When theemulsion is left in the cold, crystallisation sets in after sometime, and only a portion of the silver remains in solution.The chemical reactions coming into play are so far entirelyobscure. It would appear probable that acid phosphatesmight be formed, yet the ordinary silver phosphate isdeposited unchanged from its solution in acetic acid.
Of acid solutions the citric - phosphate solution hasbeen most tried. With 32 c.c. of the phosphate mixture
48 grms. of citric acid yield a clear solution of greatsensitiveness. Both emulsion and solution have beenapplied to materials other than paper, such as wood,celluloid, lithographic stone, marble, silk, cotton, and linen,and prints of great beauty and durability been producedthereon. They may be applied to the surfaces as such orthese surfaces may first be coated with albumen, gelatine orthe like. In the latter case a print can be obtained eitherin direct or diffused sunlight in less time than with theordinary photographic papers, and there is no difficulty inprinting out by arc light just as quickly as in shaded day-light, the emulsion permitting more rapid work than thesolution. While the ordinary albumeuised papers will notkeep, papers sensitised after this new method will keepindefinitely in any climate, if only protected from dust andlight. The prints can be toned and fixed in the ordinaryway with only this difference, that a dilute hypo-bath mustbe employed. Toning and fixing may be done at any time,even months after printing. The predominant colour ofthe prints being a very pleasant brown or auburn, toningmay, in a guod many cases, be dispensed with. Veryagreeable reddish effects can be obtained by giving theprints a citric acid bath before fixing. If this method isfollowed the prints are washed with wrater before trans-ferring them to the hypo-bath. The latter should becomposed of 35 grms. of sodium hyposulphite, 2 to 3 grms.of carbonate, or bi-carbonate of soda, and 1 litre of water.After leaving the prints from one to two minutes in thissolution, they are washed for five to ten minutes in cold orwarm water. In this alkaline bath the tone is not changed,though the colour appears considerably lighter in the wetstate than it does after drying. Only the slightest over-printing is required, if the prints are removed directly fromthe printing frame to the fixing bath. They need no over-printing at all, if they are toned, as they gather strength inthe toning bath. If left too long m the hyposulphitesolution, sulphuration of the prints wrill set in. Yet if nottoo long continued, the sulphur-toned prints obtained arepermanent.
The sensitiveness of the emulsion may be still furtherincreased by the addition of a small quantity of citric acid.When the ordinary silver bromide emulsion "is added to itdirect prints can be obtained by the light of a petroleumlamp. The silver phosphate papers can be used fordeveloping out just as well as for printing out.
DISCUSSION.
Mr. S. V. HAUS asked what were the proportions ofphosphate and tartaric acid ?
Mr. M. TOCH, asked what was the effect if the printswere subjected to sulphuretted hydrogen gas ? It was veryessential that that should be tried because the permanencyof the print depended on it. Five or six years ago, whengelatine printing out paper was invented* photographerswelcomed it as it did away with the old method of silveringalbumenised paper; but after a year the prints turnedgreenish and then faded out in spots. Dr. Leo Baekelandand himself had attempted independently to find out thecause of this fading, and they both came to the con-clusion that sulphuretted hydrogen was the cause.
Mr. Hvus asked if the'emulsion had ever been micro-scopically examined to see whether it was true emulsionand if they had ever tried to tone it down to a blue colour ?
Mr. HERMAN POOLE asked if the author had ever usedlactic acid ?
Dr. K. C. ScnuprHAus, in reply, said that the proportionswere 4 grms. of nitrate= to 4-7 grms. of sodium phosphate,borne ot the prints exhibited that night were over two yearsold and had been kept under the most varied conditionswithout any apparent change. It was a true emulsion.They had tried to tone it down to a bluish colour and itstood the precipitation from the toning in the case o'f sroldLactic acid had not been tried so far.
18 THE JOURNAL OF THE SOCIETY OF CHEMICAL INDUSTRY. [Jan. 31,
Meeting held at Derby on Wednesday, November 29th, 1890.
PROF. F. STANLEY KIPPIXG IN THE CHAIR.
THE REACTIONS OB, MAGNESIUM, ZINC, ANDIKON WITH SOLUTIONS OF CUPRIC SULPHATE.
BY R. M. CAVEX, B.SC., *M.C.
Historical.—The first observations upon this subject weremade by Bergmann in the latter part of the 18th century.The following is the explanation of the phenomena ofmetallic precipitation given by this observer (Physical andChemical Essays [1788-91]", vol. ii., p. 392) :—a Sincemetallic solutions are of such a nature that they cannotrestore what they hold dissolved to its metallic splendourwithout the accession of a new portion of phlogiston, it isevident, as well as conformable to experiment, that thiscannot be effected by the addition of calces. If, therefore,ochre be put into a solution of copper no copper will beprecipitated, but iron added to the solution is soon observedto be covered with a cupreous pellicle, for it yields part ofits phlogiston, which is necessary for the reduction of thecopper, and by this means becomes itself soluble, withoutthe emission of any inflammable air.,.
The first anomaly in the phenomena of simple displace-ment appears to have been observed by Odling in 1857. Ina paper "On the Reciprocal Precipitation of the Metals , ,
(J . C. S. 9, 289) he observed that "An equivalent ofcadmium will completely abstract the copper from a solutionof the neutral chloride containing verv much more than anequivalent of copper. In one experiment only 72 to 75 percent, of an equivalent of cadmium precipitated an equivalentof copper. Of course a portion only of the copper was inthe metallic state/ . This result, recorded without furthercomment, is of much significance in the light of facts whichwill be discussed in the present paper.
In 1866, Commaille (Comptes Rendus, 63 , 556) describeda number of experiments made with magnesium andsolutions of various salts. In many cases the evolution ofhydrogen was observed, and when solutions of cupricchloride and sulphate were employed, cuprous chloride andcuprous oxide were formed respectively, together with basiccupric salts. The evolution of hydrogen was attributed tothe decomposition of water by the metallic couple, andespecially to the electro-positive nature of magnesium.
Lothar Meyer (Ber. 9, 512) observed the evolutionof hydrogen from a solution of cupric sulphate by zinc. Hefound that a basic zinc sulphate was formed, and attributedits formation, together with the evolution of hydrogen, tothe action of the couple upon water. No cuprous oxidewas observed.
Observations by Kern (Chem. News, vol. xxxii., p. 309,and vol. xxxiii., pp. 112 and 236) and by Vitali (L'Orosi.1895, 18, 289-303) do not add materially to our knowledgeof the subjects with which they deal.
J . B. Senderens (Bull. Soc. Chim. [iii.] J 7 271; thisJournal, 1897, 443) has examined the reactions, between alarge number of metals ^ and salt solutions ; and in only10 cases, out of 90 which were investigated, was thereapproximate equivalent precipitation of metal by metal. Inone case only, the reaction between zinc and lead acetatesolution, did the author find the assumption of exactequivalent displacement true.
lieactums of Metals with Cvpric Sulphate Solution.The experiments now to be recorded embrace the reactionsof magnesium, zinc, and iron with solutions of cupric sulphateof various strengths, both at atmospheric temperature andat the temperature of the water-bath.
A number of reactions are shown to take place side byside; and, for reference, those which are consideredestablished are given at this stage:—
Reduction—(i.) CuSO4 + M "
(ii.) CuSO4 + Cu(iii.) 2 CuSO4 + M "(iv.) Cu2SO4 + M
Hydrolysis—(v.) CuSO4 + HoO(vi.) Cu2SO4 + H2O
M"3O4 + Cu.Cu,SO4.C11OSO4 + M"S0 4 .
M"S0//
Evolution of Hydrogen—(vii.) H0SO4 + M "
(viii.) HoSQi + Cu(ix.) Cu-M" + HoO
CuO + H2SO4
Cu2O + HoSC
M"S04 + Ho.C11SO4 + H2 .M"O + Cu H
A short note, giving an account of some of the earlierexperiments with magnesium, conducted in conjunctionrwith F . Clowes, was published in Chem. Soc. Proc. 1897221, and to this Divers replied in a criticism (Proc.Soc. 1898, 57), which furnished several valuable suggestionsin view of further investigations* These will be acknow-ledged in due course.
Properties of Cupric Sulphate Solution.—When a solu-tion of cupric sulphate is made with cold air-free distilledwater, such a solution is found to give a faint acid reactionwith litmus paper, but the colour of methyl orange solution-remains unchanged. If this solution is boiled for a shorttime a precipitate of a basic cupric sulphate is formed.* andthe liquid develops acidity which can be indicated bymethyl orange. A strong solution of cupric sulphate, bow-ever, does not give a precipitate on boiling, and neither doessuch a solution, after boiling, affect methyl orange. The*production of insoluble basic salt, and development ofacidity sufficient to be indicated by methyl orange, aretherefore connected, since one effect is not produced with-out the other. These phenomena, which are produced indilute solution only, are the result of the hydrolysis ofcupric sulphate by the mass action of the hot water, as waspointed out by Divers (ibid.). The reddening of litmus-paper by cold solutions of all strengths, however, requires-accounting for. The amount of free sulphuric acid presentwhich produces this effect must be exceedingly smalLComparison was made between the degree of hydrolysis ofdilute equivalent solutions of cupric sulphate and potassmm<alum, according to the observations of Long (JournalAraer. Chem. Soc, 1896, 18, 120). Equal volumes of adilute solution of saccharose were mixed with the equivalentsolutions of the two substances, and the liquids maintainedat a temperature of 50°—60° C. for six hours ; at whichtemperature precipitation of insoluble basic cupric sulphatedoes not take place. At the end of this time an appreciablereduction of Fehling's solution was obtained where alum,solution had acted upon saccharose, but in the case wherecupric sulphate solution and saccharose had been placedtogether, the amount of cuprous oxide formed fromFehling's solution was "barety perceptible. These experi-ments show that only an infinitesimal amount of free sul-phuric acid exists in a solution of cupric sulphate from*which no basic salt has been precipitated ; the amount ofhydrolysis of such a solution being very much less than inthe case of an equivalent solution of alum, which indeedgives an acid reaction with methyl orange. These resultsare of importance in considering the source of the hydrogenevolved in the following experiments.
Reaction of Magnesium with Cupric Sulphate Solution.Cuprous oxide and hydrogen invariably accompany theseparation of copper from cupric sulphate solution bvmagnesium, and when the solution is dilute, containing50 grms. or less of the crystallised salt per litre, the residuecontains, in addition to the cuprous oxide and coppermagnesium oxide and basic cupric sulphate. *
The presence of these various substances is accountedfor as fellows : —
It is believed thai the hydrogen owes its origin to thefollowing causes : —
(a) Action of magnesium on sulphuric acid produced bvhydrolysis of cupric sulphate (Divers).
(6) Action of magnesium on sulphuric acid produced bvhydrolysis of cuprous sulphate.
(c) Action of the magnesium-copper couple upon water.
Jan. si, woo.] THE JOURNAL OF THE SOCIETY OF CHEMICAL INDUSTRY. 19
Basic cupric sulphate, cuprous oxide, and magnesiumoxide, respectively, result from the above reactions.
The theory of the hydrolysis of cuprous sulphate, as theorigin of cuprous oxide and sulphuric acid, is not putforward by Divers, who accounts for the formation ofcuprous oxide by the action of the basic cupric sulphateupon cuprous sulphate.
Up to a certain point either theory will serve equallywell to account for the facts. The theory of Divers will,however, fail to account for the formation of cuprous oxidein those cases which will subsequently be described, inwhich the separation of insoluble basic salt cannot beobserved at any stage of the reaction, and in which a con-siderable quantity of free sulphuric acid remains at the end,in spite of the evolution of hydrogen gas, under circum-stances in which cupric sulphate solution cannot produceany quantity of sulphuric acid by spontaneous hydrolysis.
The theory of the hydrolysis of cuprous sulphate as theorigin of cuprous oxide and sulphuric acid will, however,meet all the requirements, since it is independent of theseparation of basic cupric compound. In support of thistheory the observations of F . Foerster (Zeit. Elektrochern.1897,* 3, 479, 493 ; this Journal, 1897, 742) maybe quoted.This author attributes the separation of cuprous oxide duringthe electrolysis of a strong solution of cupric sulphate tothe formation and hydrolysis of cuprous sulphate.
The results obtained by the action of magnesium uponcupric sulphate solution under different circumstances aregiven below, the quantities of the three products beingexpressed in copper equivalents :—
CαCu equivalent of Uu2O.
?** )> }y -*•*- • • • •
Sum of equivalents.Cu equivalent of Mg.
Strength of Solution.
of) grrns.
4
per Litre atAtin. Temp.
0*01900'1120O"1O77
0-23030•2592
SaturatedSolution at
Atm. Temp.
0-092*0*0877
0*27070*2853
400grms.per Litre at
lUU°l/\
0,0*2370*14750-0353
0' 2f>C)50*2710
The results are necessarily somewhat, inaccurate in thefirst case, owing to experimental difficulties.
The cuprous oxide occurred embedded in, and mixed with,the mass of MgO and basic cupric sulphate, It was esti-mated volumetrically by titration with permanganatesolution. ^
It will be seen that in all cases quite a small proportionof the residue consists of metallic copper. The excess ofcopper produced with cold saturated solution over theamount produced with a similar solution at 100° C, is dueto the prolongation of the reaction in the former case inthe presence of IJ2SO4 produced by the hydrolysis ofCu2SO4.
CiioS04 + H o O ^ C i i o O + IJ2SO4, andCu,SO4 = Cα + CuSO4.
It is well known that when H2SO4 acts upon ,metallic copper and CuSO4 are produced.
In the case of the dilute cold solution, it is evident thatno quantity of free acid can be present at any time, sincethe permanent separation of MgO and basic cupric sulphateoccurs from the first.
With strong solutions, either hot or cold, the basiccompounds at first separated are entirely redissolved bythe H2SO4 produced before the reaction is completed.
In those cases in which copper and cuprous oxide aloneremain in the residue, the quantity of hydrogen evolvedmay be calculated from the difference between*the amountof H2SO4 chemically equivalent to the cuprous oxide foundand the amount actually present at the end of the reaction.This has been done in the two following cases.
The hydrogen was collected and measured .over water freefrom air. The quantity found is a little low, partly owino- to
H2SO4 in solution.
0*0221.
Cu 0*0455Cu equivalent of Cu2O ' O'lStiO
„ „ „ H calculated . . \ 0*091)4„ „ „ H measured
Sum of equivalents 0*2809Cu equivalent of Mg 0 * 2828
0#0455 0*0S990-12130-1069
0*0948• •
0-2763 \ 0*28810*2828 I 0-2S80
0-05990'1213
0*0989
0-28010'2880
the solubility of the gas in water, no correction for solubilitybeing applied.
It should be pointed out that the above quantitativeresults, as regards the agreement of the sum of the equiva-lents with the equivalent of .the magnesium, do not furnishany direct evidence of the hydrolysis theory apart fromthe H0SO4 remaining. They - nn'gnt still be obtained ifcuprous sulphate reacted with basic cupric sulphate as longas any of the latter salt remained, and then the remainingcuprous sulphate was decomposed entirely into cupricsulphate and metallic copper.
The presence, however, of a quantity of H 2 SO 4 in astrong solution of cupric sulphate such as does, not undergospontaneous hydrolysis, is quite inexplicable apart fromthe theory of the hydrolysis of cuprous sulphate.
The above results will justify the calculation of thehydrogen evolved in other cases, in which' the actualmeasurement of the volume of the gas is very difficult.
The method adopted for the titration of the acid presentin these and subsequent experiments was as follows:—Ablank solution -was prepared containing the same amountof cupric sulphate, and magnesium, zinc, or ferrous sul-phate, as the solution to be' titrated. Equal quantities of"solution of methyl orange were then added to the twoliquids, and the purple solution containing the free acidtitrated with N/10 alkali, until its colour matched the puregreen of the blank solution.
Reaction of Zinc with Cupric Sulphate Solution.-—Further reference must first be made to the experimentsof Lothar Meyer (ibid.).
Meyer mixed together 100 grin?, of zinc, 100 grins, ofcrystallised cupric sulphate, and 200 grms. of water, theamount of zinc present being always in excess ; and after-eight months, during the whole of which time hydrogen-continued to be evolved, the residue was found to consistof metalhc copper covered with a coating of basic sulphateor zinc. r
1 have repeated Meyer's experiments in a modified formusing small weighed quantities of zinc in conjunction withexcess ot solutions of cupric sulphate of various strengths -and by this means the experiments were brought to"adefinite conclusion, and quantitative results arrived at
1 he reaction was studied at atmospheric temperature andat the temperature of the water-bath
Reaction at Atmospheric Temperature.—The amount ofhydrogen displaced by zinc from a cold solution*™ cupricsulphate vanes much with the strength of th7g of t
but the amount diminishes with, ^ , r o m » ™ " *
,rom
a'lays but was completed in C l i m etrated solutions were employed. The resMuT^L-always fo«nd to contain a small quantity of f™"'".'J00
was estimated according to the' me hoVde c r i W ' IIhc hydrogen was estimated from ,he cuprous oxide
c %
20 THE JOUENAL OF THE SOCIETY OF CHEMICAL INDUSTRY. [Jan. si, woo.
acidity, and also, in the case of the most dilute solution,measured directly, a correction being applied for thesolubility of the gas in water on the assumption that thedilute solution, with which it stood in contact for a week,absorbed the same volume as air-free water at the sametemperature. This method of estimation is manifestlyrough, and the results are not as reliable as those obtainedby calculation.
The following are the results :—
CiiSO4.5H3O per Litre.
120 grms* , 50 grms.
CuCu equivalent of Cu2O
„ ,» H (calculated) , . .
Sum of equivalentsCu equivalent of Zn
„ H (measured).
0*45070•0*0428
0*5020(K02200*0166
300 grms.
0-4S90O-O05-10*0027
„o-0'0"
539153720419
00•5106•5407• •
00•4971•41)52• •
The equivalent precipitation of metal by metal is evidentlylittle departed from in strong solutions, and the formationof cuprous oxide and lydrogen might very well be over-looked by superficial observation. Even in the more dilutesolutions, if the Cu2O were weighed as copper, and thehydrogen ignored, the total weight of the residue wouldapproximate to the weight of copper equivalent to the zincemployed. Thus, owing to a compensating error, theformation of 0u2O and hydrogen is likely to be ignored.
Reaction at the Temperature of the Water-bath.—-Zinccauses evolution of hydrogen from hot solutions of cupricsulphate of various strengths ; and this hydrogen is alwaysaccompanied by a quantity of cuprous oxide, appearingtogether with metallic copper in the residue.
The evolution of gas, though slow at first, becomes briskeras the reaction proceeds, and continues until all the zinchas passed into solution. The solution never becomesturbid throughout, whatever its strength, but lapidlvdevelops acidity, which is the cause of the evolution ofhydrogen; and at the end of the reaction much sulphuricacid remains in the liquid.
The following results were obtained when zinc in theform of fine turnings reacted with hot solutions of cupricsulphate of various strengths : —
CuSO4.5H2Oper Litre.
(1.)
Cu, 0*3208Cu equivalent of Cu2O.. ! 0M217Cu equivalent of H (cal- 0"052:2
eulated). !Sum of equivalents . 0*4947Cu equivalent of Zn. 0*11)74H2SO4 in solution . . 0'1071
20 grms.
(2.)
0-3G030*09670*0510
0*5170(rSliK)0*0705
(3.)
0-4:3490-07140-0(518
0-A7110*57120*0108
50 300grms. j grms.
0*31520-13310*0538
0
0\W>S
0-0270
0 T>1930*5040 0*5171
In the second of the above experiments with the 20 grms.per litre solution, the beaker and its contents stood in awarm place for an hour and a half previous to filtering.The effect of the action of the dilute sulphuric acid presentupon the cuprous oxide during this time is seen in theincrease in the quantity of copper at the expense of thecuprous oxide. The final outcome of this action should beto leave a quantity of cuprous oxide, in a non-acid solution,chemically equivalent to the hydrogen evolved. An ap-proximation to this is seen in the results given in the thirdcolumn above. In this case the solution and residue stoodin contact with each other for 10 days previous to filtration.We may suppose that equilibrium was attained, and thata small amount of sulphuric acid in dilute solution canexist side by side with some cuprous oxide.
As regards the influence of the concentration of thesolution upon the quantity of hydrogen and cuprous oxide
formed, it will be seen that only in the case of the verystrong solution are the quantities of these two productsdiminished. The proportions present in this latter case showa marked contrast to those produced when zinc reacts withthe same solution at atmospheric temperature, in whichcase the departure from simple displacement is very slight.
Reaction of Iron with Cupric Sulphate Solution.—Theaction between iron and cold cupric sulphate solution isgenerally recognised as one of simple displacement, butSenderens (ibid.) has recorded the evolution of hydrogenunder these circumstances. My experiments were per-formed with fine iron wire, which contained an almostimperceptible amount of carbon, and under no circumstanceswas the evolution of hydrogen observable.
Since iron is far less active with dilute sulphuric acidthan zinc, there is no proof that cuprous sulphate is notproduced and hydrolysed in small quantities.
In experiments with dilute solutions the rusting of ironhas to be taken into account. I have not been able toprevent the slight rusting of iron in ordinary distilled waterwhen precautions were taken to exclude air by lengthened,boiling, cooling out of contact with air, and rapid sealing,the sealed vessel being then placed under water. Whenfine iron wire is placed in dilute cupric sulphate solutionprepared with similar precautions, a turbidity graduallyappears in the liquid which we may suppose is simply dueto the rusting of iron ; but after a few days, as the reactionbetween the iron and the cupric sulphate is completed, theliquid becomes quite clear again, except for the precipitatedcopper. Even when orange flakes of rust have separated,in cases where the solution was previously aerated, theyeventually disappear, while similar flakes, separated fromiron immersed in water only, remain.
The residue of copper always contains traces of cuprousoxide, and the solution is found to be distinctly acid tomethyl orange. Moreover, all the iron is found to bepresent in solution, and in the ferrous state. Cuproussulphate is evidently produced in minute quantities andhydrolysed, the acid which thus comes into existenceserving to dissolve the rust; the ferric sulphate formed bythis means being reduced to the ferrous state in solution.
The quantity of cuprous oxide formed was too small to beestimated with any accuracy, and no attempt was made toestablish equivalence between the iron and the reactionproducts, because, since rusting by agency of atmosphericoxygen appeared to play some part, no such equivalencecould be expected.
Reaction at the Temperature of the Water-bath.—Iron inthe form of fine wire causes evolution of hydrogen from hotsolutions of cupric sulphate of all strengths, and the residueconsists of cuprous oxide mixed with metallic copper.
With dilute solutions (50 grms. per litre or less)contained in a beaker immersed in the water-bath aturbidity appears immediately after the introduction of themetal, starting from the surface of the wire, and graduallyincreasing until fine orange particles are seen floatingthroughout the liquid. During the formation of thisprecipitate the evolution of hydrogen is slow, because theiron ^ is protected, but after a maximum separation ofprecipitate has been reached the orange particles oraduallvdissolve, and the liquid becomes clear again. At "the sametime the rate of evolution of hydrogen increases/amicontinues brisk until all the iron has passed into solutionIt the original solution of cupric sulphate is very dilute andexcess of iron is used, the evolution of hydroeen' willcontinue after the solution has become colourless byprecipitation of all the copper. •*
If the ^ reaction is arrested when the orange precipitate ispresent m considerable quantity, a n examination of thisprecipitate, after filtration and thorough washing, proves itto consistently of hydrated ferric oxide. At tfcnlnJA S
g pAt the closeof
r , e iron is found to be presentin the solution in the ferrous state, 'and the liquid containsfree sulphuric acid. " H LUUW1I1S
y y er ic oxide. At thethe. experiment, however, all the iron is found to be presentin the solution in th f i
The formation of a ferric compound is not due to
Jan. 3i, woo.] THE JOURNAL OF THE SOCIETY OF CHEMICAL INDUSTRY. 21
separation is exceedingly slow compared with the rate offormation of the ferric oxide. Indeed, when zinc reactswith a solution of the same strength, no hasic sulphate,either of zinc or copper, separates.
The following explanation of the separation of hydratedferric oxide under the above conditions is submitted.
Cuprous oxide is known to react with ferrous chlorideto produce cuprous chloride, ferric oxide, and metalliccopper, in the following manner : —
' 3Cu2O + 2EeCl2 = 2Cu + 2CiuCL + Fe2O3,
and although cuprous oxide does not react with ferroussulphate solution under ordinary circumstances, we mayreasonably suppose that unstable cuprous sulphate, formedby the reduction of cupric sulphate, can oxidise ferroussulphate thus—
2EeSO4 = Fe,(SO4)3 + 2Cu.
Ferric sulphate readily undergoes complete hydrolysis inhot dilute aqueous solution, for when some basic ferricsulphate is digested with water, and a clear solutionobtained by filtration, such a solution gives a precipitatewhen poured into excess of boiling water, and thisprecipitate consists entirely of hydrated ferric oxide.
If ferric sulphate is produced and hydrolysed in theabove manner when iron reacts with hot dilute cupricsulphate solution, the separation of hydrated ferric oxidecan be accounted for.
Cuprous sulphate and ferrous sulphate will not, however,be produced side by side in the proportions required for theabove reaction, but in equal numbers of molecules thus—Ee + 2CuSO4 = Cu2SO4 + EeSO4, and it is improbablethat all the ferrous sulphate that is produced in the firststages will have an opportunity of reacting with cuproussulphate. Owing to the extreme instability of cuproussulphate- probably much of it will be hydrolysed, and willnot react with FeSO4. Thus the accumulation of acid bythe independent hydrolysis of cuprous sulphate willeventually cause the hydrated ferric oxide which hasseparated in the first stages of the reaction to be re-dissolved, and will also prevent the further hydrolysis offerric sulphate. Ferric sulphate in solution will speedilybe reduced to the ferrous state by the influence of themetallic iron, and evolution of hydrogen will proceed bythe action of the acid produced in the continued hydrolysisof cuprous sulphate.
If the solution of cupric sulphate with which iron reactsis sufficiently strong, this separation of ferric oxide doesnot take place, but the evolution of hydrogen, and forma-tion of cuprous oxide and copper, continue until all theiron is dissolved. In this case, therefore, if ferric sulphateis formed in the liquid, the mass action of the water is notpowerful enough to effect its hydrolysis, and it is thereforedirectly reduced to the ferrous state.
The results obtained by the action of iron on solutions ofcupric sulphate of different strengths, at the temperature ofthe water-bath, are shown in the following table :—
CuSO4. 5H2O per Litre.
20 50 grms.
CuCu equivalent of Cu2O„ „ „ H calculated
0*44150*13270*0398
Sum of equivalents .Cu equivalent of Fe
0*01400*6157
0-66780-08020*0333
300 grms.
0*62720*07950*0112
0*78130*7833
0-71790*7181
Although the amounts of cuprous oxide and hydrogenproduced diminish with increasing strength of solution, itwill be seen that, as in the case of zinc, these quantities areconsiderable, even with the strongest solution.
The agreement, in the case of the dilute solution, of thesum of the equivalents with that of the iron taken, is proofthat the formation of the hydrated ferric oxide, whichmakes a temporary appearance, is not due to atmosphericoxidation.
Origin of Cuprous Sulphate.—No attempt has been madein the foregoing to give any general theory of the origin ofcuprous sulphate, although the existence of this body hasbeen repeatedly assumed in accounting for the observedphenomena.
There are three possible theories of the origin of cuproussulphate :—
(1.) By reduction of cupric sulphate by "nascenthydrogen. , ,
(2.) By reduction of cupric sulphate by direct action ofthe displacing metal.
(30 Synthetic production, by the action of precipitatedcopper on cupric sulphate.
With regard to the nascent hydrogen theory, Divers (ibid.)has given reasons for discarding it. If we do not acceptthis theory, it remains to consider whether one or other ofthe remaining theories suffices to account for the facts. I tmay be pointed out that, provided the theory of syntheticproduction of cuprous sulphate were found adequate, thenthe separation of cuprous oxide could not be considered asan essential part of the reactions in which the displacingmetal is concerned, but rather as the result of an unavoid-able supplementary reaction. So that the correctness of ourviews of the phenomena considered as a whole depends to avery large extent on an answer to the question of the originof the cuprous sulphate.
Action of Cold Cupric Sulpliate Solution on PrecipitatedCopper,—In order to discover if cold cupric sulphate solutionhas any action on finely divided copper, small, approxi-mately equal portions of pure precipitated copper wereexposed to the action of solutions of different strengths, andalso to the action of pure water. Air was carefullyexcluded, and the action went on for some weeks*
The solutions were then decanted, the copper washedwith air-free water, digested, in absence of air, with dilutehvdrochloric acid, and the acid solution in each easetitrated with standard KMnO4 solution, after the additionof magnesium sulphate.
The following results were obtained : —
Strength ci Solution of Cupric Sulphate,
Water20 grms. per litreoO ,»
e
300 „
C.c 's of KM11O4,Solution.
o-i0'5
0*60-6
Hence the conclusion that by the action of solutions ofcupric sulphate of various strengths upon precipitatedcopper at atmospheric temperature, small quantities ofcuprous oxide are produced, but that the strength of thesolution employed has little effect upon the reaction.
If this cuprous oxide is formed by the hydrolysis ofcuprous sulphate, the cupric solutions should become acidduring the reaction. This was found to be the case, andan attempt was made to establish an equivalence betweenthe cuprous oxide and sulphuric acid. The quantities,however, were very small, and the estimation of cuprousoxide by Titration is not accurate. The following are theresults of four experiments with a dilute solution :
H2SO4. H2SO4 equivalent of
0*01270*01230-01470-0127
Mean.... 0*0131
0*01310*00620-02390-0131
0-0141
These results are sufficient to show that formation andhydrolysis of cuprous sulphate occur to a slight extentunder the above conditions.
In the above experiments a condition of equilibriumbetween the cuprous oxide and sulphuric acid is set upbut by eliminating the acid as it is formed a much larger
THE JO OF THE SOCIETY OF OHEMIOAL INDUSTRY. [Jan. 31,1000.
amount of cuprous oxide may be obtained. This is shownto be the case by the following experiment:—A smallquantity of pure precipitated chalk was placed togetherwith copper and dilute cupric sulphate solution in a cylinder,which was carefully stoppered and immersed in water.At the end of a week much of the chalk had disappeared,and in place of it there appeared a small quantity of basiccupric sulphate, and also needle-shaped crystals of hydratedcalcium sulphate. The most noticeable phenomenon, how-ever, was, that when the stopper was withdrawn a briskeffervescence of carbon dioxide took place throughout theliquid. Thus carbonic acid was formed in solution underpressure by the action upon the chalk of the sulphuric acidgenerated by the hydrolysis of cuprous sulphate. Underthese circumstances, therefore, a considerable amount ofcuprous oxide was to be expected in the residue.
Examination proved this to be the case. In two experi-ments performed side by side the hydrochloric acidsolution of the residue required G3*0 and 74*0 c.c. of anapproximately X/10 solution of KMnO4; and in two otherexperiments 45*5 and 41*0 c.c. were used respectively.
It is therefore shown that a considerable amount ofcuprous oxide is formed by the interaction of cupric sul-phate solution and metallic copper at atmospheric tem-perature, provided the acid liberated by the hydrolysis ofcuprous sulphate is not allowed to accumulate.
miction at the Temperature of the Water-bath.—Whenprecipitated copper is heated with cupric sulphate solutionat the temperature of the water-bath, under the conditions ofthe previous experiments with magnesium, zinc, and iron,the solution rapidly becomes acid, and a considerableamount of cuprous oxide is formed. During the course ofthe heating the copper becomes slightly darker in colour,and is found on closer examination to be covered with-email dark-purple patches. A microscopic examination ofthese patches shows them to consist of aggregates of ruby-red crystals in the shape of regular tetrahedra. A drop ofdilute hydrochloric acid disintegrates them, a white granularprecipitate appearing in their place.
This is very satisfactory evidence of the formation ofcuprous oxide by the action of hot cupric sulphate solutionon metallic copper.
In attempts to show that the cuprous oxide and sulphuricacid were chemically equivalent, the amount of acid wasinvariably found somewhat deficient; and it was ultimatelydiscovered that the reason for this deficiency was the actionof hot dilute sulphuric acid on precipitated copper.
25 c.c.'s of X/10 HoSOi were diluted with 200 c.c.'s of boiledwater and heated with precipitated copper for half an houron the wnter-bath, out of contact with air. It was foundafter this time that the acidity had diminished and somecopper had passed into solution.
In two experiments the loss of acidity was 1*7 and1*9 c.c. X/10 H«SO4 respectively. The amount of copperfound in the solution exceeded by about 0*003 grm. thecopper equivalent of the IT2SO4 used up. During the timeof heating small bubbles of gas continuously made theirappearance on the surface of the copper, and passed upthrough the liquid. I t can hardly be doubted that copperdisplaces a very small amount of hydrogen from dilutesulphuric acid under the above conditions.
If a correction for loss of acidity in accordance with theabove results is made, the cuprous oxide and sulphuric acidproduced by the interaction of precipitated copper and hotcupric sulphate solution may be shown to be chemicallyequivalent to each other.
The following are the results of four experiments :
In order to test this question, experiments were performedto ascertain the quantities of cuprous oxide produced from0*5 grin, of precipitated copper, when hot solutions orcupric sulphate of the three different strengths employed,acted upon the metal as nearly as possible under the samennnrlitinns as in the Tjrecedinff experiments with a
H2SO4 by titrationCorrection
Total 2 4H3SO4 equivalent of Cu2O
0*07790*0039
0-08380*0869
0-11610*0088
O'l2490*1252
0*08130*0084
0*09110*0074
0-09850*1028
It is evident from the above results that much at leastof the cuprous sulphate owes its origin to the action of thesolution on precipitated copper, and the question ariseswhether or not this is the only method of formation.
conditions as in the precedingdisplacing metal.
Strength of Solution. Time.
20 grms, per litre50 „
300 „
1 hour30 mins.30 „ .
Cu EquivalentofCuoO.
0'05390*05400*0725
It will be seen, on comparing these amounts of cuprousoxide with those obtained when a displacing metal is used,that there is much less Cu.,0 in the case of dilute solutions
id
and but about the same amount in the case of the strongestsolution.
What is more striking, however, is, that when adisplacing metal is employed the amount of cuprous oxidediminishes with increasing strength of the solution ; whereas,when copper alone is immersed the opposite is the case,the most cuprous oxide being produced with the strongestsolution.
From these considerations I have concluded that, withhot solutions, cuprous sulphate owes its origin both to thereducing action of the displacing metal—whether magnesium,zinc, or iron—and to synthetic production from precipitatedcopper and cupric sulphate.
With regard to cold solutions, since a large amount ofcuprous oxide may be produced as a result of the action ofthe solution upon the copper when the sulphuric acid formedat the same time is neutralised as soon as liberated, it wouldappear that the synthetic production of cuprous sulphatemay be sufficient to account for all the cuprous oxide. I twould be impossible, however, under the circumstances, todeny the other method of formation.
What is most probable is that magnesium, when actingon the cold solution, produces a considerable quantity ofcuprous sulphate by reduction ; that zinc produces a muchsmaller quantity ; whereas it may be safely concluded thatin the case of iron the very small amount of cuprous oxidefound owes its origin alone to the synthetic production ofcuprous sulphate.
DISCUSSION.
Mr. J N O . GOLDING asked whether the metals used wereabsolutely pure.
Mr. J . T. WOOD said he was much interested in thepaper. I t might seem a purely scientific one, but hethought it had some practical use. In making chrome-tanned leather, if the chrome alum were dissolved in hotwater the leather could not be tanned with it. Dissolvedin the cold the solution was purple, dissolved hot it had agreen colour. He would like to ask Mr. Caven if this wascomparable to the CuSO4 solution mentioned by himwhich yielded a basic salt on boiling. '
Dr. J . J . SUDBOROUGH referred to experiments in whichalthough theoretically accurate results were obtained theprecipitate had been found to contain an appreciablequantity of the precipitating metal, the apparent accuracybeing due to a balance of errors (J . Amer. Chem Soc1899, 932). He thought that the numbers obtained w)zinc and copper sulphate solutions were of great interestthey showed that the simple replacement of copper bv ziu,deviated more from the theoretical as the solution becan*diluter or as the temperature increased. Did not this «to indicate that the origin of any secondary iprobably due to the hydrolysis of the sulphate
CuSO4 + HoO =
aszinc
e
CuO H2SO4,
^ & ^ r ? U n d 0 u b t e% "crease, both withand with the temperature ? What the nature of
these secondary reactions might be it was difficult to say; «they were due to free sulphuric acid, surely one of the m0 t
Jan. 81,1900.] THE JOURNAL OF THE SOCIETY OF OHEMIOAL INDUSTRY. 23
important of them would be a reduction by and of nascenthydrogen from the zinc and free acid.
Mr, L. ARCHBUTT thought that Mr. Caven would by hisinvestigations save many students from struggling in theirwork with erroneous theories.
T H E CHAIRMAN remarked on the great difficulty of thework on which Mr. Caven had been engaged, some of the'estimations having to be made with very small quantities.TKe explanations which Mr. Caven had given were certainlyiQOt dogmatic, but from a certain standpoint the views ex-pounded were unfortunate. In the past they had beencontent to represent by one equation the precipitation ofone metal by another. If, however, they gave the studentan explanation involving eight equations, they would havegood cause to regret the loss of simplicity.
Mr. R. M. CAVEN, in the course of his reply, said thatthe substances he had used were the purest that could bepurchased. In reference to chrome alum, it was knownthat when a cold solution was heated the violet colourchanged to green, the following equation representing theaction that occurred—
2Cr2(SO4x;3 + H2O - [Cr4O(SO4) 4] SO4 + H2SO4
the formation of the acid due to hydrolysis probably havingdie baneful effect remarked upon by Mr* Wood.
In reply to Dr. Sudborough, Mr. Caven admitted that allthe reactions might be traced back to the influence of nascenthydrogen, if the theory of its action were admissible. Thiswould even be possible in the case of the supposed syntheticproduction of cuprous sulphate, since a small amount ofhydrogen is liberated by the action of the acid upon theprecipitated copper. He thought it easier, however, toftelieve, with Divers, that nascent hydrogen does not play apart in these reactions.
Meeting held on Wednesday, December 20th, 1899.
PROF. F. STANLK5T KIPPING, F.R.S., IN THK CHAIR,
ON LEATHER DYEING.
BY PROF. H. R. PROCTER, 1M.C.
'{Contribution from the Leather Industries Laboratory ofthe Yorkshire College?)
T H E chemistry of leather dyeing is somewhat complex, aswe are not dealing with a fibre of uniform constitution, buthave already combined and modified it in various ways inthe processes by which it has been converted into leather.Dyeing, no doubt, depends on the combined action of forceswhich we rudely distinguish as chemical and physical,without, however, being able to draw any definite linebetween them; but it will be convenient to consider thesubject first from the chemical side. The constitution ofthe gelatinous fibre of skin is unknown, but one is justi-fied in stating that, like the amido-acids which are impor-tant proximate products of its decomposition, it containsboth acid and basic groups, and is therefore capable ofattracting both bases and acids. It is well known, forinstance, that the neutral fibre is capable of withdrawing•sulphuric acid from a deci-normal solution with such vigourthat the residual liquid is neutral to litmus paper; and itwill also absorb caustic alkalis with perhaps equal avidity.It is thus readily dyed by colouring matters of either basic oracid character, and in many cases will even dissociate theirsalts, dyeing the characteristic colour of the free dyestuff,but possibly at the same time fixing the liberated base oracid with which the colouring matter has been combined.Many tanning processes consist in a somewhat analogousfixation of weak bases and acids, and it is therefore to beanticipated that they will profoundly modify the colour-fixing properties of the original fibre, as indeed proves tobe the case. Exactly what the result of a particular tan-ning process in this respect will be is less easy to foresee.
In the ordinary vegetable-tanning process the tannins,which are of acid nature, are freely fixed by the fibre. Itis therefore not surprising that vegetable-tanned leather
most freely fixes the basic colours, especially as thesemostly form insoluble compounds with the tannic acids, sothat it is quite probable that the dyeing is mainly effectedby the formation of tannin-colour lakes on the fibre, ratherthan by actual fixation of the colour base in combinationwith the original matter of the skin. I t is noteworthy, how-ever, that even fully tanned skin has by no means lost itsattractions for acid-colouring matters, many of Avhich willdye it even without the presence of free acid, though itis possible that the tannic acid performs the function o£saturating the alkaline base with which the colour-acid hasbeen combined.
In Germany, basic colouring matters of the coal-tarseries are largely employed in the dyeing of vegetable-tanned leathers, on account of their rapid absorption andgreat colouring power, while in England, where largernumbers of skins are usually dyed in one bath, but for alonger time, acid colours are generally preferred, on accountof the greater evenness with which they dye, and theirlesser tendency to " bronze.'. It should be pointed outthat while the substance of animal skin consists practicallyof gelatinous fibres, it is covered on the outer surfacewith a thin membrane of extreme tenuity, called thehyaline or glassy layer, which, in the living animal,separates the true skin and the epidermis. This layer,the chemistry of which is quite unknown, reactsto colouring matters differently from the gelatinousfibres, and probably is less absorbent for basic colours, andmore so for the coloured anhydrides of the tannins, andperhaps for acid colours generally, than is the true skin.As a result, it colours more darkly in tanninp, and less soin dyeing Avith basic colours, and as it is extremely liable todamage in the preliminary operations of removing hair andlime by the tanner, this irregularity of colouring is a seriousdisadvantage which is most marked with the basic colours," Bronzing,5' the dichroic effect produced by light reflectedfrom the surface of many colouring matters, complementaryto that transmitted by them and reflected by the surface ofthe dyed material, is not peculiar to basic colours, but isgenerally more marked than in acid ones. Basic colours,from their great affinity for tannins, and consequent rapiddyeing, are apt to dye irregularly, and without sufficientlypenetrating the leather, and if the soluble tannin is notwholly washed out of the skins previously to dyeing, itbleeds in the dyebath, and precipitates insoluble tanninlakes, which waste colour and adhere to the surface of theleather. The inconvenience of basic colours due to their toorapid fixation may sometimes be lessened by slight acidifi-cation of the dyebath with a weak acid, such as acetic orlactic. The precipitation of tannin lakes in the bath maybe prevented by previous fixation of the tannin with tartaremetic, or some other suitable metallic salt.
Irregular and surface dyeing sometimes occurs also withacid colours ; while in other cases the affinity of the dye istoo small to allow of reasonable exhaustion of the bath.Addition of salts of weak acids, such as tartar, or of thoselike sodium sulphate, which form hydric salts, lessenrapidity of dyeing; while acids generally increase it, and itis also often increased by addition of common salt, whichlessens the solubility of the dye. Weak acids, such asacetic or lactic, or acid salts, such as sodium bisulphateare generally to be preferred to sulphuric acid as anaddition to the dyebath; and if the latter is used, greatcare is desirable in its complete removal. There is nodoubt that the rapid decay of leather bookbindings andupholstery is largely due to the careless use of sulphuric acidin " clearing " and dyeing the leather ; and even if it is fullvremoved, it has saturated all bases such as lime, which arenaturally present in leathers in combination with weakacids, and which would otherwise act as some protectionfrom the sulphuric acid evolved in burning coal o-as.
The use of the natural polygenetie colours^ in dyeingleather of vegetable tannage, which was once universal isgradually disappearing, except for the production of blacksLeather cannot be very satisfactorily mordanted for thesecolouring matters; but they have some natural attractiontor the leather itself, and are generally dyed first, and theircolours afterwards developed by metallic mordants, such asiron, chrome, tin salts, and alum, which act not only on
THE JOURNAL OF THE SOCIETY OF CHEMICAL INDUSTRY. [J«i.3i,i9uO:
the absorbed dyestuff, but frequently on the tannin andcolouring matters derived from the tannin materials. Forblack-dyeing the use of coal-tar colours* either alone or todeepen the colours produced by iron, is gradually extending.Claus and Ree's " Black C. W the " Corvolines " of theBadische Co., and Casella's " Naphthylamine Black/ ,
"Aniline Grey/ , and " Naphthol Blue-black , , may bementioned as useful colours. As coal-tar blacks are mostlydark violets rather than dead blacks, their colour may bedeepened by the admixture of suitable yellows or browns,and this has already been done in one or two of the coloursnamed. Apart from the coal-tar colours, black dyeing isgenerally produced by the action of iron (and chrome),either on the tannin of the leather itself or on logwood.As the leather is frequently greasy, and the satisfactoryformation of a tannin or logwood lake can only take placein presence of a base to absorb the liberated acid of theiron salt, the skins are either brushed with, or plunged in, alogwood infusion, rendered alkaline with soda or ammonia,or the tanned leather receives a preliminary treatment withAveak soda or ammonia solution alone. As such solutionsact powerfully on tanned leathers, rendering them harshand tender, great care must be taken to avoid unnecessarystrength. The effect of this alkaline treatment is not onlyto assist the Avetting of the greasy surface, but to preventtoo deep penetration of the dye, by causing rapid precipita-tion of the colour lake. In recent times, however, leathersare sometimes demanded in which the colour goes rightthrough, and in this case it might be well to reverse thetreatment, beginning with a Aveak solution of a ferroussalt, perhaps with addition of sodium acetate or potassiumtartrate, and finishing Avith alkaline logwood, as withoutalkali the full colour is not developed. The use ofiron salts is not very satisfactory in regard to thepermanence of the leather; and in this respect it is ofgreat importance that they should not be used in excess,and that any strong acids they contain should be saturatedAvith permanent bases, and if possible Avashed out. Leathersurfaces blacked Avith iron almost imariably ultimately losetheir colour, becoming brown if tannins, and red if logAvoodhas been employed, and at the same time the leathersurface usually becomes brittle or friable. This is to alarge extent due to the effect of iron oxides as oxygencarriers. Exposed to light, they become reduced to theferrous state, oxidising the organic matters Avith Avhichthey are combined, and in the dark the}' re-oxidise, andthe process is repeated. It is therefore of the firstimportance that excess of the organic colouring mattershould be provided, and that the quantity of the ironshould be as small as possible, and in stable combination.These points are greatly neglected in practice, especiallywhere blacking is done by the application of iron saltswithout logwood, Avheu the evils mentioned are intensifiedby the actual removal of part of the tannin of the leather,and perhaps by the combination of ferric oxide Avith theskin fibre itself, forming a brittle iron-leather. Treatmentwith alkaline sumach or gambier or logAvood solutions, bothbefore and after the application of the iron, Avould lessenthe evil. In practice, iron blacks are generally oiled infinishing, and this renders them more permanent, both byprotecting the lake from air and by forming iron soapsAvhich are stable. The use of actual soaps in blacking andfinishing is not unknoAvn, and probably deserves moreattention. Hard soaps of soda and stearic acid form anexcellent finish where a moderate glaze is required, thesoap jelly being applied Avith a brush very thinly, allowedto dry, and polished Avith a flannel or brush, or glassed.Many acid colours are soluble in such soap jellies, whichmay thus be employed for staining. Similar but harderfinishes, and capable of being glazed to a high polish, aremade by dissolving shellac Avith dilute borax or ammoniasolutions. Both of these finishes are useful in lesseningthe tendency of iron blacks to smut or rub off, a failingwhich is due to the precipitation^ of loose iron lakes onthe surface, instead of in combination with the fibre, and isparticularly obvious where " inks " or one-solution blacksare employed, or where the mordant afid the colouring mattersolutions are allowed to mix on the surface of the leather.Such " inks " are generally made with a ferrous salt, and
logAvood or tannin, together with some aniline black, andof° course the colour lake is only formed on oxidation.Chrome is not much employed in blacks on vegetabletannages, as it only produces blacks on logwood, thechrome compounds of tannins having no colouring value;,and bichromates used at all freely being very injurious tothe leather.
In dyeing blacks on other than vegetable tannages,,however, chrome becomes of importance, as logwood isprincipally employed, though sometimes in conjunctionwith tannin, and often with addition of quercitron or fustic,to correct the bluish shade of the logwood-chrome orlogwood-iron lake.
In alumed leathers the fixing power of the original hide-fibre is much less affected than in vegetable tannages..Whatever may be the truth with regard to the latter, thereis little doubt that physical influences are at least asimportant as chemical ones in those produced by mineralsalts. The amount absorbed is greatly influenced by theconcentration of the solutions, and in ordinary alum taAAringmuch of the alumina may again be removed by freewashing. The sulphate of potasli present takes no part inthe operation, but the alumina salt is absorbed apparentlyas a normal salt. Alum or alumina sulphate alone isincapable of producing any satisfactory tannage Avithoutthe assistance of common salt, the quantity absorbed beingsmall, and the fibre becoming swollen by the action of theacid. In presence of salt the absorption is greater, and theswelling is prevented. The explanation of this is not to befound in the formation of aluminium chloride, for thoughthis undoubtedly takes place, it lias been shown that theaction of aluminium chloride Avithout salt is not moresatisfactory than that of alum. It has long been knownthat salt prevents the swelling action of acids on skin,,although it does not lessen the absorption of acid ; and the*fact is capable of explanation on modern osmotic theories.The skin so treated is found to be converted into leather,but if the salt be washed out, the acid is retained by theskin, which returns to the state of acid-swollen pelt. I t isprobable, therefore, that although the acid and alumina areabsorbed in equivalent proportions to each other, they arereally dissociated, and attached to different groups in thegelatine molecule, and that the effect of the salt is to alloAvthe absorption of the acid without swelling, and, osinoti-cally, to increase the dissociating power of the pelt. If,in place of a normal alumina salt, a basic salt is employed,,such as maybe obtained by partial neutralisation of thesulphuric acid with soda, satisfactory tannage may beaccomplished Avithout salt, a basic compound is absorbed," andthe leather is much less affected by washing. In theanalagous case of chrome tannage, this basic compoundmay be almost if not quite deprived of its residual acid,by washing the tanned skin Avith alkaline solutions, leavinga leather which is extremely resistant eA en to hot water*-and a somewhat similar result may be obtained withalumina, though with more difficulty, as apparently a small,
excess of alkali destroys the qualities of the leather.The results on dyeing are almost what might have been*
foreseen. While ordinary alumed leather absorbs bothacid and basic dyes readily, the chrome-oxide leather haspractically lost its affinity for the latter. Both chrome andalumina leathers readily absorb vegetable tannins, thussupporting the view that the acid-fixing groups of thegelatine molecule are still unsaturated (tannins are capableof tanning pelt SAvollen Avith sulphuric acid and apparentlyof expelling the acid). In the ease of chrome leather theeffect of retanning Avith tannins is greatly to lessen itsstretch, and if carried too far, to destroy its toughness butit at once becomes capable of fixing basic dyesSiffs Thisproperty is frequently made use of in dyeing, but the effecton the leather must not be disregarded where softness a n *stretch are important, as in the case of glove leathersPolygenic dyes are, of course, fixed by alum and chromeleathers as alumina or chrome mordanted, though anparently the base does not exist in the most favourable,condition for fixing colours. Thus logwood extracted.Avithout alkali dyes tanned leather yellow, alumed leatherviolet blue, and chrome leather blackish violet, and some ofthe ahzarme group dye very well on chrome as its resistance-
Jan. a. mo.] THE JOUENAL OF THE SOCIETY OF CHEMICAL INDUSTRY.
to hot water allows much higher temperatures to be usedthan with most other leathers. The tannin contained indyewoods has the effect of lessening the stretch of chromeleathers.
Something should perhaps be said on the dyeing of oiland aldehyde leathers, but the subject has as yet beenscarcely treated scientifically, and our practical knowledgeof the subject is insufficient to justify theorising.
DISCUSSION.
Prof. H. R, PROCTER writes that he considers a suggestionmade by Mr. Pentecost in the course of discussion—that apotash-oleine soap might be used in place of an alkali oralkaline carbonate for preparing leather for blacking—as aperfectly practical one in many cases. Soaps were often usedfor the purpose in blacking alumed leathers, and formed ironcompounds which were more resistant to change than thosein which fatty acids were absent. Soaps also added to thepermanence of iron blacks when applied after blacking.
^ It was not generally known that soaps and soap emulsions(fat-liquors) could be applied Avith success to vegetable-tanned leathers for softening purposes, so long as freealkali was avoided. Considerable quantities were absorbed,giving a plump and soft leather without oily feel, and insome cases the soap might be fixed with advantage bysubsequent treatment with basic alumina (or probably basicchrome) solutions. Another useful softening agent forleather which was intended to be dyed, and which wasscarcely known to leather manufacturers, was " Turkey-redoil" (sulphonated castor oil), which was miscible with water,and could be applied as a fat liquor. It also could be fixedby basic alum solutions, and then formed a mordant foralizarin and many aniline colours.
Meeting held at Glasgow on Tuesday, December 19th, 1899.
DR. G. G. HENDKRSOX IN THE CHAIR.
THE CYANIDE PROCESS AT YALWAL, N.S.W.,AUSTRALIA.
BY ALFRED CHIDDEY.
T H E pioneer pyanide plant consists of five leaching vats,each 20 feet in diameter, with 6 foot staves ; 2 concretesumps each of 50 tons capacity, and 1 of 20 tons capacity,3 zinc boxes; and 1 dwt. special Blake pump.
The tailing treated average about 5 dwt. of gold per ton.They were formerly brought down by a stream of water inlaunders, from a large heap which had accumulated at somedistance from the plant; they were then passed throughSpitzkasten to separate the slimes, and thence into theleaching vats. This method was discontinued as the slimeswere found to carry off fully 40 per cent, of the gold. Thetailings are now trucked dry to the leaching vats, and about3 lb. of ground lime are spread over each truck load.When the vats have been charged to within 9 inches of thetop a dilute (0*10 per cent.) solution of potassium cyanideis pumped in, and leaching is commenced when the vat isfull. The solution of the gold takes place very rapidly.A few minutes after the pinch-cocks leading to the zincboxes have been opened the solution is often found tocontain half an oz. of gold per ton, whilst the amount ofcyanide has been reduced to 001 to 0'02 per cent.
Twelve hours later the contents of the vat are levelled,and a strong (0*3 per cent.) solution of cyanide is pumpedin, and the surface of the tailings is kept covered by thesolution during the remainder of the leaching processin order to prevent packing. In addition to the quantityof cyanide solution used for wetting the tailings, a columnof solution 9 feet high, and of the diameter of the vat isused in all. About one-third of this consists of the strongcyanide solution* A water wash is usually given at the endof the operation if time permits, but if not the tailings are
sucked as dry as possible by means of the vacuum pump-The duration of the leaching process in 144 hours.
The following table shows the rate of extraction of thegold :—
Time.
24 hours.48 „72 ,.96 „
320 „144 „
Amount of Gold dissolved.
31'5 per cent.r>8 „70 „7079 „82
The operation of leaching is considered complete whenthe amount of gold extracted reaches 82 per cent., as thevalue of the gold which would be dissolved bv moreprolonged treatment with cyanide solution does not coverthe additional cost of extraction.
Caustic soda was formerly used in place of lime Avhenfilling the vats from the launders, hut it was found to foulthe zinc boxes and to render the solution turbid. Whenlime is used, the solutions are perfectly clear, and theprecipitation is very satisfactory when the solution containsmore than 0 • 10 per cent of cyanide [92 to 94 per cent.].From a solution obtained by passing through two solutionscontaining respectively 0-05 and 0*13 per cent, of cyanideand mixing these, 90 per cent, of the gold was precipitated.From a solution containing 0*03 per cent, of cyanide, and2 dwts. 18 grains of gold per ton, 75 per cent, of the goldwas precipitated, and in the case of a solution containing0-01 per cent, of cyanide, and 4 dwts. 12 grains of gold perton, the amount precipitated was 6G per cent. The amountof gold precipitated was considerably increased by allowingan alkaline solution of lead, prepared by adding excess ofcaustic soda to a solution of lead acetate, to drop slowl'vinto the 6th division of the weak solution box. Under thesecircumstances, 98 per cent, of the total gold present wasprecipitated from a solution containing 0*02 per centcyanide, and 6 dwts. 18 grains of gold per ton. The use ofthe lead solution was not continued, as it was always foundpossible to keep the quantity of cyanide in the solutionabove 0-10 per cent, by regulating the stopcocks.
The zinc shavings are cut from the end of a roll of zincon a lathe. The metal contains about 1 per cent, of lead,and is practically free from arsenic and antimony.
The clean up is made once a month, but the first threedivisions of each box are cleaned out once a week. Theslimes are placed in a barrel with a locked cover. At theend of the month water, or a very dilute solution ofcyanide, is allowed to run through each of the boxesI h e zinc shavings are rubbed against a sieve containing10 meshes to the linear inch. The portion which passes'through the sieve goes to the settling pit, and the remainderis returned to the boxes. As the shavings are very touo-hbreaking up of any that are useful need not be fearedVery short pieces of zinc are not put back into the boxesas they would quickly choke up the gratings. In c h a i - Sthe zmc boxes, new shavings are placed on the g r a w fand the short pieces which have been previously used a?Tarranged above these. J
The slimes are allowed to settle in the pit for 12 hoursand the supernatant clear liquor, which often contains San ounce of gold per ton, is then pumped off into t h T
t$X£ i ^until the barrel is about half full. A thinsulphuric acid is now allowed to run
the poisonous fumes which are evolved Tn
^T^^«: : & a &acid can be carried ouf WithoutPSc«Uy buthas been used for neutralising ftee acTand "d
26 THE JOURNAL OP THE SOCIETY OF CHEMICAL INDUSTRY. [Jan. 8i, woo.
Tmsic iron salts in the leaching vats, the frothing is soexcessive as to preclude the possibility of applying thismethod of treatment, and the slimes must be dried and'burnt before adding acid.
In about six hours the solution of the zinc is complete.The barrel is then filled with water and the contents arewell stirred and allowed to stand for 24 or J36 hours. The•sulphate of zinc solution is now drawn off. The barrel is•again filled with water, the contents are stirred and allowedto stand for 12 hours, after which the liquid is drawn off.The slimes are twice washed with water, but a third washingwould be advantageous. After the last washing the slimesare allowed to stand for 24 hours, until they have settled•down compactly, and the water is then drawn off to withinquarter of an inch of the slimes. They are then removed•and dried on an iron plate with turned up edges, No filteris used. The slimes, which are disturbed as little aspossible in the process of dryinsr, are obtained in the formof lumps about an inch in diameter.
The dried slimes are now placed in a well annealed No. 4plumbago crucible, with about half their weight of a flux-which has been previously prepared and fused. The fluxconsists of two parts of soda and one part of borax. Inthe first charge the slimes are kept round the sides of thepot and the flux in the centre. The slags are kept thick•enough to prevent them from attacking the pots.
The following table gives the results of a partial analysisof the slimes after acid treatment :—
Per CentGold and silver 10*0Lead 7 0Copper 12*0Silicious matter 22*0
A certain amount of matte approximately of the followingcomposition, is always produced : —
Per Cent.Gold 2-85Lead 2S*80Copper 40'00Sulphur 15*00Silver 9* 15
A sharp blow with a chisel will generally cause thematte to separate from the bar.
The matte is fused with an equal weight of the above-mentioned flux and metallic iron, A bar of metal, con*taining about 8 per cent, of gold and 26 per cent, of silver,is thus produced.
The gold bar is refined as follows :—A large clay pot is placed inside a No. 40 plumbago
crucible and heated to dull redness. The bar to be refinedis now introduced, and when the lower end of the barbegins to melt, about a pound of nitre is shot in from ascoop. When the bar has melted the whole is vigorouslystirred with an iron rod till the action has ceased ; afterwhich about half-a-pound of dried borax is added, andwhen the metal is in a state of quiet fusion the bar ispoured.
The gold bar so obtained is about 900 fine for gold andsilver, and is worth about 3Z. to 5/. per ounce.
The slimes are not ground but fed into the pot in lumps,just as they come from the drying pan. As the flux hasbeen previously fused there is no boiling over in meltincrthe slimes. The slag exercises a very powerful corrosiveaction on the pots, which only last for three charges.
The slag is coarsely powdered and washed for frillsof metal and matte. It still retains gold to the amount ofabout 30 to 40 ounces per ton, and is sent to the smeltingworks when it has accumulated in sufficient quantity. °
DISCUSSION*
Mr. C. J . ELLIS said Mr. Chiddey's paper was an in-teresting one, giving, as it did, a statement of the workingof the cyanide process at the Pioneer Plant, more or less indetail. Taken as a whole the method employed did notappear to differ very materially from that usually adoptedin the treatment of tailings-sands of normal character • hemight, however, remark shortly on the following points
The first runnings of solution from the percolators, asMr. Chiddey found, were generally comparatively rich in goldand poor in cyanide, and this was only to be expected, as atthe beginning of the treatment the maximum of free oxygenwas usually present, and the first solution acted quickly bothon the more easily soluble portion of the gold and also onany " cyanicides" which might be present. When theemployment of alkaline treatment was called for at all, limewas usually preferred in practice to caustic soda, as IDaddition to its being cheaper, it acted both as a neutralise!' ofany acidity present and also tended to accelerate filtrationwhen slimes were present, and to give a clearer effluentcontaining less foreign salts. The time required for theleaching of the tailings referred to in this paper (viz, 6 days)was in excess of the average normal time for tailings sands ;this was, however, probably mainly due to the presence of alarger proportion than usual of slimes. It would be noticedthat only a few grains of gold per ton were extracted duringthe last couple of days, but the value of this gold no doubt;more than paid for the cost of allowing the treatment tocontinue for these two days. Mr. Chiddey apparently foundlittle or no difficulty in obtaining satisfactory precipitationof the bullion by the normal method of employing zinc-shavings ; it was, however, interesting to note that he hadfound the use of a lead solution beneficial when dealingwith solutions very weak in cyanide, as this gave furtherconfirmation to the fact which was now more or lessrecognised, and which, so far as he was aware, was firstpointed out by Mr. J. S. MacArthur some five years ago,that the formation of a lead-zinc couple in the first one ortwo compartments of the extractor aided the precipitationof gold and silver from solutions of certain character. Themethod which Mr. Chiddey described for preparing thebullion slimes for smelting differed somewhat from the usualpractice of filtering and washing these slimes rapidly, eitherby means of suction or in a filter press, followed or notfollowed, by acid treatment of the washed slimes ; it hardly,however, struck one as being an improvement on theordinary method, and must certainly be less expeditious.Details of this sort were, however, very much a matter ofpersonal choice of the chemist in charge of a cyanide plant*
SEPARATION OF BISMUTH FROM LEAD.
BY JOHN CLARK, PH.D.
THE only methods of separating bismuth from lead based onthe precipitation of the bismuth in the metallic state arethose of Ullgreen, Patera, and Classen. Both Ullgreen andPatera precipitate the bismuth with metallic lead, theformer in an acetic acid solution and the latter in a dilutenitric acid solution, but it is very difficult, if not im-possible, to get the whole of the bismuth in this way, andaccording to Olav Steen(Zeit. angew, Chem. 1895, p. 531)the deficiency generally amounts to from 20 to 30 per cent.
Classen separates the lead and bismuth electrolyticallyfrom a nitric acid solution, the lead being precipitated asbinoxide and the bismuth in the metallic state, but thebinoxide of lead always contains a considerable quantity oibismuth.
The method which I have to bring before you depends onthe precipitation of the bismuth by means of metallic iron.The metals in the form of chlorides are boiled with steelturnings, which rapidly bring down the whole of the bismuthcarebeing taken not to dissolve all the iron, as otherwise aportion of the bismuth will redissolve.
Example.
Bi2O3 taken.
0*8970-445o-oio
PbO taken.
0-50-5
B12O3 found
0-8960-4450*009
potash, and iwith sulphuretted
Jan. 8ia9oo.] THE JOUENAL OF THE SOCIETY OF OHEMIOAL INDUSTRY, 27
being washed free from iron, the sulphide of bismuth isdissolved in nitric acid precipitated with carbonate ofammonia, and weighed as oxide.
The chloride of lead in the filtrate is converted intoacetate by the addition of an excess of acetate of soda, thenprecipitated with sulphuric acid and weighed as sulphate.
This method will be found to be verv convenient for theestimation of small quantities of bismuth in alloys of leadand tin.
ANALYSIS OF COPPER, &c.
BY JOHN CLAUK, PH.D.
I N the analysis of copper in which the total amount ofimpurity is small in comparison with the copper, it isnecessary to operate on a considerable weight of metal ifwe wish to be able to estimate the various impurities, andit is of great advantage to remove the copper before theseare separated and estimated.
For this purpose Jean (this Journal, 1896, 677) sug-gested that the copper liquid should be poured into asolution of sodio potassium tartrate, and the copper reducedwith glucose, but this process is so cumbersome that it isof very little practical value.
As far back as 1853, Flagolot (Jr>iu\ prakt. Chera.LXL, 107) introduced a method for the precipitation ofcopper as iodide in a solution acidified with sulphuric ornitric acid, and containing excess of sulphurous acid, tartaricacid being added when antimony is present.
He states that aqua regia can also be used as a solvent,but that in this case the HCl must be driven off completelyafter solution by boiling with sulphuric acid.
Jn 1888 Paul Jungfer (Zeits. Anal. Chem. 27, 64) sub-jected Flagolot's method to examination for the purposeof ascertaining whether it could be used for the completeseparation of copper from arsenic and antimony, and hefound that the whole of the arsenic remained in solution,but that a portion of the antimony was carried down bythe iodide of copper, and could only be removed by veryprotracted washing. To overcome this difficulty he sug-gested the addition of fluoride of potassium, which, he says,keeps the antimony in solution owing to the formationof a readily soluble double fluoride of antimony andpotassium.
I have made a number of experiments for the purpose ofascertaining whether copper could be separated fromantimony by Flagolot's process, and I find that even inpresence of free HCl, as well as tartaric acid, the iodide ofcopper has a tendency to carry down a portion of theantimony which is not removed by washing with water,but that the antimony so precipitated is readily dissolvedout by moderately dilute, HCl (15 per cent.), and that thewhole of the antimony remains in solution when theliquid from which the copper is precipitated contains asufficient excess of H O .
According to Flagolot, when a mixture of nitric andhydrochloric acid is used in the solution of the copper, it isabsolutely necessary to drive off the whole of the HCl byboiling with sulphuric acid, but I find that when the copperexists as chloride, or if the copper is precipitated withcarbonate of soda and then dissolved in HCl, the nitricacid and sulphuric acid in the original solution do notin any way interfere with the precipitation of the copper,as iodide and the HCl, when present in sufficient quantity,completely prevents the antimony from being carried downby the iodide of copper, but, as a measure of precaution,it is advisable to wash the precipitate with dilute HCl beforewashing with water.
Process.—10 grms, of the metal are dissolved in nitricacid, evaporated to small bulk, rendered alkaline withcarbonate of soda and dissolved in HCL To the coldsolution 30 grms. of iodide of potasium are now added, andthen solution of sulphite of sodium till the precipitatecoutains no free iodine which is easily recognised by thecolour. The precipitate of iodide of copper thus producedis very dense and settles readily—when cold it is nearlyinsoluble in water—according to Kohlrausch and Rose
(J . Chem. Soc. 1894, A., p. 7) the solubility of iodide ofcopper in water at the ordinary temperature is 8 milli-grammes per litre, and in dilute HCl it seems to be equallyinsoluble. After settling the iodide of copper precipitate isthrown upon a filter and washed first with dilute HCl andthen with cold water. The fitrate, which must be dliuted ifit contains too much HCl, is then boiled till no more SO2 isevolved, tantaric acid added, and the solution renderedalkaline with caustic soda or ammonia, which should notproduce a precipitate, and a little sulphide of sodium orsulphide of ammonium is added to precipitate the remainingtraces of copper and all the other metals present with theexception of arsenic antimony and tin.
The solution containing the black precipitate is boiledto cause the precipitate to settle, filtered and the filtrateacidified with HCl and saturated with H2S to ensure thecomplete precipitation of the arsenic. After standing forsome time the precipitate, which contains very little freesulphur, is collected on a filter, and while still moist it iswashed into a flask, with 20 per cent. HCl, mixed withtwice its volume of strong HCl and connected with adistilling apparatus.
In a former paper (J . Chem, Soc. 1892, 425) I showedthat sulphide of arsenic could be separated from thesulphides of antimony and tin by distilling with HCl andferric chloride. I have since then proved that the presenceof ferric chloride is unnecessary, and that when thesulphide of arsenic is freshly precipitated the whole of thearsenic can be volatilised by boiling with strong IIC1, thesulphide of arsenic being decomposed into H2S and AsCl3,which combine again in the water of the receiver, so thatthe formation of a yellow precipitate in the receiver is anindication of the presence of arsenic. When sufficient strongHCl is used, the whole of the arsenic will be found in the fil-trate after three distillations, partly in the form of sulphideand partly in solution. It, there is any deposit in the deliverytube, it is washed out with dilute ammonia, the solutionsaturated with H2S, the arsenic colleected on a weighedfilter, washed with bisulphide of carbon and weighed assulphide.
The antimony and tin may then be separated by mymodification of the oxalic acid method (J . Chem. Soc. 1892,427), but I prefer to separate the antimony with steelturnings and precipitate the tin in the filtrate with H2S andweigh as SnO2. As I have had occasion to point out(J. Soc. Chem. Ind., 1896, 255), a portion of the tinis apt to be carried down by iron, but in the case ofsteel, the quantity is so minute, that in my opinion it isthe most reliable process for the separation of smallquantities of antimony and tin ; and when a portion of thesteel is left undissolved and thrown on the filter with theantimony, oxidation is prevented and there is no loss inwashing. The antimony and steel are then dissolved inHCl, with the assistance of a little chlorate of potash, andthe antimony is precipitated and weighed as sulphide.
Qualitative Separation of Arsenic, Antimony, and TinThe above method of separating arsenic, antimony, and
tin, is very suitable for qualitative analyses.For this purpose the mixed sulphides, or a portion of
them, are introduced into a small flesh mixed with from 20to 30 c.c. of strong HCl and distilled without the use of acondenser into a test tube containing water till the waterbegins to boil, which requires only a few minutes. Ifarsenic is present, a yellow precipitate makes its appearance,
in the test tube, which is sulphide of arsenic. The residualliquid is then filtered if necessary, and boiled with aconsiderable quantity of steel turnings to precipitate,the antimony ; the precipitate, which can be detached fromthe iron by shaking, is then thrown upon a filter andwashed with water, and the filtrate is tested for stannoustin with mercuric chloride. The precipitate on the filteris dissolved by washing with dilute HCl, containing a littlechlorate of potash, and the solution is divided into two partsIn one of these the antimony is brought down as an orantre"coloured precipitate with H2S, and in the other depositedon platinum with zinc. uepowiea
The metals which have been precipitated with sulphideof sodium or sulphide of ammonium in the alkaline
28 THE JOURNAL OF THE SOCIETY OF CHEMICAL INDUSTRY. [Jan. 31,1900.
tartrate solution are dissolved in HC1 with the assistanceof a little chlorate of potash, and the copper bismuth andlead thrown down with H ^ redissolved in HC1 with alittle chlorate, the bismuth and copper precipitated withsteel turnings, converted into sulphides, then dissolved innitric acid, and the bismuth precipitated with carbonate ofammonium and weighed as oxide.
To the filtrate from the bismuth and copper excess ofacetate of soda is added and the lead is precipitated withsulphuric acid and weighed as sulphate. The iron, nickel,&c. are estimated in the usual way.
The lead may also be removed before precipitating thecopper as iodide by adding sulphuric acid to the nitric acidsolution, boiling down to small bulk and allowing to standfor several hours.
Analyses of Rio Tinto and Tharsis cake copper by thisprocess gave the following results :—
In the above analyses the copper was determinedvolumetrically by E. O. Brown's modification of the iodideprocess ( J . Chem. Soc., X., 65), which gives very accurateresults, as has been pointed out by J . W. Westmoreland(J . Soc. Chem. Ind., 1886, 49), who examined hundreds ofsamples of all descriptions of copper by this method. 1am aware that doubts have been expressed by somechemists as to the accuracy of the iodide process, butwhen the copper is entirely in the form of acetate it will,in the absence of more than traces of iron., comparefavourably with any other.
THE OXIDATION OF AMMONIA BY IRON ORE.
BV W. CARUICK ANDERSON, M.A., D.SC. AND
GEO. LEAN, B.SC.
FROM experiments conducted by Lowthian Bell andrecorded in his " Principles of the Manufacture of Iron andSteel" (p. 183), it appears that the reduction of peroxideof iron by carbon monoxide gas, begins at comparativelylow temperatures. In the case of precipitated oxide, hefound that a slight action showed itself at temperatures aslow as 141°—149° C.
Cleveland stone, on the other hand, began to actappreciably on the gas only at temperatures over 200° C.
The oxidation of hydrogen gas would also appear,according to the same authority, to start at or about thesame limits of temperature.
From consideration of these results, it might fairly beconcluded that other hydrogen-containing gases wouldundergo a like decomposition by iron ores at similartemperatures. In a recent paper read before this Society,(Carrick Anderson and Roberts, this Journal, p. 1099) it wasshown that on distilling mixtures of raw coal and iron oresin a retort, a considerable proportion of the ammonialiberated in the decomposition of the coal was destroyedthrough the action of the oxides, and this destruction wasindicated as a possible source of loss in the recovery ofammonia as a by-product in blast-furnace working.' It seemed, therefore, a matter of some practical importance
to determine definitely the relative amount of this decompo-sition at different temperatures.
The ore used in our experiments was a soft brownhaematite of American origin and having the followingcomposition : —
Per Cent," l ' ;Moisture (hydroscopic)
Water (combined)Ferric oxide »Manganese oxideCalcium oxideMagnesia ••• /Insoluble } *38Carbon dioxide # %SO3, P2O5, at?d loss ^
IUO'00
A column of this ore in rough pov/dtr TVHS takeur,measuring 15 centimetres (about 15 guns. 7/eight) andcontained in a " IT " tube of diameter about one centimetre.
To introduce the ammonia a slow current of nitrogenwas made to bubble through a solution of ammonia liquorof medium strength, and after thorough (hying hy passagethrough a tower containing quick-lime, was led throughthe ore-tube, kept at the desired temperature. The rate ofbubbling was maintained uniformly at 36 per minute, andthe temperature of the ammonia liquor at 64° C.
The total weight of ammonia carried over :n eachexperiment was ascertained by substituting for the ore-tube one of similar dimensions, charged with pure whitesand, and maintained at the same temperature.
The alkali was estimated in all cases by collecting in ameasured quantity of standard acid which was afterwardstitrated. Each experiment was run for exactly 30 minutes.Duplicate trials were done with the ore at each temperature,and were in all cases preceded and followed by a blankexperiment. The current of ammonia gas v/iis allowed topass through the ore tube for, as nearly as possible, threequarters of an hour before collecting the sample.
The results showed that when the ore was freshlvcharged its destructive action upon the alkali was morevigorous than when it had been exposed to heal for sometime.
At lower temperatures it was found that a considerablequantity of alkali was absorbed by the fresh ore before itbecame completely saturated, whereas in the sand-tubeequilibrium was established in a few minutes.
The ammonia carried over in each experiment of 30minntes duration varied from 0'06 to 0*09 grm., and thepercentages destroyed by the fresh and previously heatedore were found to be as follows : —
Temperature of Ore.Percentage N H 3
destroyed byfresh Ore. *
Percentage NH ; ;destroyed by pre-
viously heated Ore.
Per Cent.100-0
00*278-1
57*229" S
19*68*5
I'er Cer.r
241 • or,23'D^21-70
Iβ-0
S-5
An experiment made at ordinary temperatures on oreand sand showed equal quantities of ammonia ivassine;through in each case. *
From these figures it may be concluded that the action ofammonia on ferric oxide begins at temperatures between140° and 150° C., a result which agrees with the statementof Lowthian Bell, quoted above, that carbon monoxidebegins to effect a reduction of the peroxide at or about thesame temperature.
Our figures, moreover, bear out the conclusion arrived aftby the same authority that difference in the Dhvsionlcondition of the peroxide as it exists in its various naturaand artificial forms, materially influences its activity in theoxidation process. J <J
DISCUSSION.
Mr. BUMBY said that the oxidising action of iron ores wouldaccount for the destruction of part of the ammonia bTheblast furnace gases but added that the action in the blastfurnace was considerably modified by the presence ofwater vapour, and gases, which would tend to protect -
Jan. 3i,i9oo-] THE JOUENAL OF THE SOCIETY OF CHEMICAL INDUSTRY. 29
ammonia from oxidation. He was interested to learn thatthe oxidation of ammonia began at so low a temperature as140°.
Dr. CLARK asked whether the authors had examined theiron ore after passage of the ammonia to ascertain theexact nature of the change which had taken place.
Mr. LEAN, in reply, stated that the ore had not beenexamined at the end of the experiment, but that theyconcluded from the formation of water that the chargewas solely one of oxidation of the alkali, the peroxide ofiron being reduced to protoxide.
Journal anlj patent* literature*Class.
I.—II.—
I I I . -IV . -V.-
VI.
VII.—
VIII.-IX.-X.
XLXII.-
XIII.-
XIV —
XV.XVI.-
XVII.-XVIII.-
XIX.-XX.-
XXI.-XXII.-
XXIII.-XXIV.
PageGeneral Plant, Apparatus, and Machinery 29Fuel, Gas, and Light 31•Destructive Distillation, Tar Products, Petroleum 3GColouring Matters and Dyestuffs 37Textiles: Cotton, Wool, Silk, &c, 42•Dyeing, Calico Printing, Paper Staining, and
Bleaching 13Acids, Alkalis, and Salts, and Ts"on - Metallic
Elements , 45Glass, Pottery, and Enamels 47•Building Materials, Clays, Mortars, and Cements. 43Metallurgy 50Electro-Chemistry and Electro-Metallurgy 53Eats, Fatty Oils, and Soap 54•Pigments and Paints ; Resins, Varnishes, &c.;
India-Rubber, &c 55Tanning, Leather, Glue, Size, Bone, and Horn ;
Ivory and Substitutes 57•Manures, &c 01Sugar, Starch, Gum, &c 61•Brewing, Wines, Spirits, &c <J2Foods : Sanitation ; Water Purification ; and Dis-
T H E author tried to discover the cause of a serious explo-sion in a steam cylinder on board a German man-of-war.The boilers were of the Belleville type, consisting of a numberof iron tubes in which a comparatively small quantity ofwater was being continually converted into steam, whereby asuperheating of some parts of the tubes was likely to arise.According to an official regulation, the pipes had to becoated outside with zinc, but on closer examination a con-siderable amount of this metal was found inside* Sincevery little metallic zinc could be discovered in the sludgefrom one of the tubes used, although a fair quantity of theoxide was present, the author supposes that through thesuperheating of the tubes, water was decomposed bythe metallic zinc and hydrogen gas formed.—S. K.
STONEWARE condensing worms which are unsupported, areJess durable than those which are rigidly fastened to crossstays, though it has been argued that the worms which arethus supported suffer through the strain set up by thedifference of temperature between the inner and outer walls.But in reality free stoneware worms are more liable to
* Any of these specifications may be obtained by post byremitting %d.—the price now fixed for all specifications, postageincluded—to C. N. Dalton, Esq., Comptroller of the Patent Office,Southampton Buildings, Chancery Lane, London, W.C.
fracture in transit and during installation, and to crack, owingto the strain on the spiral when the water covers it to acertain height- Cracks in free worms cannot be patched, asthe worms have not sufficient strength after they havecracked, whereas worms supported by stays may be repairedmany times. Corrugated worms are likewise not durable,as they cannot be repaired when damaged. Worms of thesimplest pattern are the best, and attempts at improvementsshould be directed to the composition and production of thestoneware from which they are made,—J. A. B.
PATENTS.Compressed Gas Vessels. A. Sweetser, Surrey, and
A. Pringle, Kent. Eng. Pat. 19,219, Sept. 9, 1898.VESSELS formed with both ends open are closed by meansof end caps, connected together by a central rod or bolt,which passes through the vessel. When the vessel has onlyone open end, the bolt is attached to a bridge-piece, whichbears against the internal shoulder of the vessel. In eachcase excessive pressure is relieved by the stretching of thebolt, which permits the cap or caps to lift. The caps areprovided with gas-checks, consisting of cupped rings of lead,gutta-percha, &c., threaded on the bolt. The gas outletmay be formed in the bolt, which is then adapted to servefor the attachment of the delivery valve and connections.
—R. A,
Refrigerating and Liquefying Air or other Gases9 Appa-ratus for. E. C. Thrupp, Surrey. Eng. Pat. 26,767,Dec. 19, 1898.
A TURBINE motor, in which the air or gas is expanded andcaused to do external work, is employed in combination withmeans for compressing the air or gas, and cooling it whilstunder pressure. The thrust or guide blocks and bearings ofthe turbine are kept at some distance from the motor parts,for the double purpose of avoiding bearing-friction inproximity to the cold gas, and preventing the lubricant frombeing frozen.—R. A.
Determined Quantities of Liquid Carbonic Acid or Com-pressed Gases or Vapours, Apparatus for Drawing off.VV. P. Thompson, London. From W. F. Fritz, Zurich,and H. A. Alioth, Basle. Eng. Pat. 18,253, Sept. 9, 1899.
THE apparatus consists of a chamber d, of fixed capacity,provided with a spring-controlled inlet-valve c, and a similar
THE JOtfBNAL OF THE SOCIETY OF CHEMICAL INDUSTRY. CJen.8i.iwfc
outlet-valve c1, and with nozzles'to1, a2; which communicate
with the chamber through the said valves, for connection,respectively, with the reservoir of compressed or liquefiedgas, &c, and with the receiving vessel at b. The valves c, cl
are operated by the eccentrics or cams f, fl from the gear-Ing f>, el, so that one valve is closed when the other is opened,and vice versa. The gas is first admitted to the chamber dthrough the valve c, which is then closed, while the valve c1
is opened to deliver the gas into the vessel b. The narrowdelivery passage between fl and b, serves to temporarilyreduce the pressure of the gas entering the vessel.—R. A.
Separating Gases and Vapours from Mixtures, Process for.K. Kubierschky, Aschersleben, Germany. Eng. Pat.17,780, Sept. 2, 1899.
T H E gaseous mixture is caused to enter a chamber underpressure, and so as to meet a current of a solvent liquid,which dissolves the more easily soluble constituents. Theliquid is then passed by a pump into another chamber,where the pressure is reduced and the bulk of the absorbedgas liberated. The liquid next passes into a third chamber,where it meets the " raw g a s " entering the apparatus,which, under diminished pressure, and by mutual interchange,effects a further liberation of the still dissolved gas. Boththe first and the third chambers above mentioned are filledwith coke, &c, or provided with any other suitable arrange-ment for facilitating absorption. A low temperature may beused instead of, or in conjunction with, a high pressure :and a high temperature with, or instead of, a low pressure.
—K. A.Evaporating Water or other Liquids by Means of Steam,
Apparatus for. J. Davie, Glasgow. Eng. Pat. 24,498,Nov. 21, 1898..
THE apparatus consists of a steam-heated coil or coils,preferably of spherical shape, mounted within a sphericalchamber or casing containing the water or other liquidto be evaporated, the ends of the coil or coils beingconnected to the steam inlet and outlet by suitable connec-tions or bearings, which permit the coils to be rotated forthe purpose of being cleaned. A portion of the casing ismade removable, to afford access to the interior. The steamis supplied to the coils through a steam drum, and suitableconnections are provided for admitting the steam to, anddischarging the condensed water from, the coils. Gaugesare also provided for indicating the steam pressure in thedrum and the level of the liquid in the casing.—R. A.
Liquids from Solid Materials, Method of and Apparatusfor Separating. C. E. Kreiss, Hamburg, Germanv.Eng. Pat. 25,296, Xov. 30, 1898.
THE material to be treated is fed on to the lower end of aninclined channel or trough, which is supported or suspendedby rods, springs, &c, and has a reciprocating swingingmotion imparted to it, whereby the material is caused totravel towards the upper end of the trough. In one form ofthe apparatus, the bottom of the trough is perforated, andthe liquid which passes through it is caught in a separatecollecting gutter underneath ; but for coarse materials, &c,the trough may have a closed base, from which the liquidflows off in the backward or downward direction.—It. A.
Filters, Impt. in. C D . Abel, London. From DirektorClaassen and Co., Beuthen, Prussia. Eng. Pat. 1688,Jan. 24, 1899.
A FILTERING body, for the purification of liquids and gases,is constructed of a piece of soft wood, such as poplar, lime,or alder, &c, cut across the grain from one of the homo-geneous quarters of the tree trunk, the lateral surface ofthe wood being rendered impervious by a suitable envelope,such as a metal ring, so that the liquid or £as is compelledto pass through the wood in the longitudinal direction ofthe grain. The filtration is facilitated by means of air-pressure, vacuum, or a suitable combination of both, and anumber of such filtering bodies may be hermetically joinedtogether and secured in a suitable frame, so that no jointallows of any unpurified liquid passing through it. Suitableforms of apparatus for filtering oil, beer, air, and gases, afiltering cock for attachment to a water main, and a filterin
coffee-pot, in all of which these filtering bodies are employed,are described.—K. A.
Filters and Filtering Materials, Manufacture of M.Jolles and A. Jolles, both of Vienna. Eng. Pat. 9276^May 2, 1899.
THE operative filtering material consists of a tissue, prefer-ably of asbestos, covered by or united with a layer ofinsoluble, porous, and fireproof material, such as asbestospowder, talc, kieselguhr, or bone-black, or a mixture of suchsubstances. The tissue may be stretched over a frame ofany desired shape, and the covering layer may be united toit either by means of silicic acid, produced directly on thetissue in insoluble form from alkaline silicates, by the actionof acids and subsequent heating, or by means of insolublefluorides, formed on heating soluble silico-fluorides. Thesolution of the soluble silico-fluoride employed may bemixed with chlorides of the metals of the alkaline earths,with which the solution, or the residue resulting from theevaporation of its solvent, also reacts on heating, to forminsoluble compounds, such as calcium fluoride.—R. A.
Filter Material, Automatically Cleansing. H. Reisert^Cologne, Germany. Eng. Pat. 10,586, May 19, 1899.
THE increasing resistance of the impurities retained in thefiltering material, during the period of filtering, is employedto raise a column of unfiltered water to a height sufficient tostart a siphon arrangement, which sucks a mixture ofcleansing-water and air through the filtering material. Theair is supplied through a perforated pipe, immersed in thewater which passes through the filter, and, by entering thesiphon, ultimately stops the cleansing action, ^on-returnvalves are provided for the escape of the residual air fromthe siphon, and from the closed liquid chamber to which itis connected. The cleansing operation can also be started,,when desired, by means of a float-valve arrangement, whichis brought into action by closing a valve in the ordinarydischarge pipe of the apparatus.—It. A.
Presses for Separating Liquids from Solids. A. J . Boult,London. From L. Heuclin, Dunkerque, France. Eng.Pat. 18,737, Sept. 16, 1899.
THE press chamber is made relatively narrow, and openat either one or both ends according to" whether one or twopressure plates are used. The pressure plates fit between,the sides of the chamber, so that only their edges act on thematerial, and are operated through pistons by hydraulic orother power. ^ The chamber is movable in the direction ofthe force applied, and so equalises the pressure. A seriesof chambers may be arranged longitudinally or transversely,or both, the pressure plates of the whole series being operatedby a single piston, or by a piston at each end. A feedhopper, movable top and bottom plates, and a dischargingplunger are provided for filling and emptying the chamber,which operations may be also facilitated by making the sidesmovable. The press may also be arranged to act vertically.
—R, A.Filtration Purposes, Apparatus and Process for. A. Smith
F. Smith, and A. S. Muir, all of Toronto, Ontario* E n /Pat. 20,850, Oct. 18, 1899. ' b'
THE material to be filtered is introduced into a cylinderhaving a perforated periphery and an inwardly-convexbottom, the cylinder being rotated within an outer imperforate cylinder or casing, which is provided with <*collecting gutter and discharge pipe for the filtered liquidIhe: inner cylinder is lined with a filtering material suitablefor the liquid treated the passage of the liquid through thematerial and the perforations of the inner cylinder bein-effected by the centrifugal action.—R. A. -> i l I l ue r D e i D£
Washing Pyrites, Coal, and other Minerals; AvvaratCleaning or. C. Burnett, Durham, and HNewcastle. Eng. Pat. 25,852, Dec. 7, 1898.*
T H E material is fed on to an endless inclined belt of an o n e n
or porous nature, through which water under ™-PS,2? '
ties from the mineral. The lighter m a S k « i V ? l p U r i ;at the lower end of the belt 4 d th?f * a^ dehveredthe unner end T L lLif Z h o h e a v i e r materials attne upper end. The belt may be constructed of a s
us for
senes
Jan. si, woo.] THE JOUBNAL OF THE SOCIETY OP CHEMICAL INDUSTRY. 31
of suitably-connected grid bars, and is provided with, orworks between, perforated upstanding sides. Perforatedscreens are provided at each end of the apparatus for theoutlet of the materials. Further details relating to theworking of the apparatus, including means for controllingand regulating the water supply, &c, are fully described inthe specification*—R. A.
THESE furnaces are intended for manufacturing processes inwhich it is necessary to heat certain materials gradually,then highly, and finally to cool them gradually. A furnaceof this kind is constructed " so that the goods may bepassed intermittently or continuously" through it, theheat being applied to the furnace by combustion of gasat or near its middle part, " so that the heat is greatestat or near the said part, and diminishes towards theends of the furnace chamber, where the goods arerespectively admitted and discharged"; "the burning gastravelling towards the inlet end of such furnace chamberand passing out, at or near the said end/ , into a return flueor flues. Separate flues are provided for the products ofcombustion, for the air, and, if desired, for the gas also ; suchflues being arranged so that heat from the products of com-bustion is transferred to the air, and, if desired, to the gasalso, before the air and gas meet to burn. The air forcombustion enters at the discharging end, and is heated bythe goods or their containers in the furnace, thereby alsoserving to cool the goods or their containers.—R. S.
IL-FUEL, GAS, AND LIGHT.Iron Carbonyl in Water-Gas, Detection and Removal of
M. van Breukeleveen and A. ter Horst, J. fur Gasbe-leucht. 42, [44], 750—751.
IRON carbonyl in water-gas causes deposition of ferric oxideon mantles when the gas is used for lighting by incandes-cence, the illuminating power rapidly diminishing. Theauthors detected iron carbonyl by the brown deposit whichis produced in a heated glass capillary tube when gas con-taining that compound is passed through it. They concludethat water-gas takes up iron when left in contact with it atordinary temperatures and pressure, and that iron carbonyl isnot formed in the water-gas generating plant. Coal-gas doesnot take up iron in the same manner, probably because thereis less carbonic oxide in coal-gas than in water-gas, and theiron carbonvl results from the action of carbonic oxide on iron.Eor new installations, the authors recommend the adoptionof Dicke's plan of tarring the mains internally in order toprevent the water-gas coming in contact with the iron.They found that damp potassium permanganate abstractedthe iron from gas containing iron carbonyl which waspassed over it.—J. A. B.
Incandescence Gas Burners, White Deposit on SmokeCatchers and Chimneys of, and its relation to theMantle and Gas. C. Killing. J. fiir Gasbeleucht. 42,[50], 841—843.
THE author has analysed the whitish deposit which formsupon the " smoke catchers " which are frequently suspendedabove incandescence burners, obtaining, in two cases, thefollowing results:—
Insoluble in water :—SilicaOxide of ironRare earthsCopper oxide (scales)
Soluble in water: —Rare earthsSulphuric acid.Copper oxideCalcium oxideMagnesium oxideOxide of iron
-Water •• • •>
No. 1.
Per Cent,0'300*210'55
28*70
0*28
28*03
Xo. 2.
Per Cent.0*810'61Trace2*16
'None30-4831-450*700*150-58
32-02
The deposit therefore consists substantially of coppersulphate, the copper being derived from the smoke-shadeitself.
The following are the amounts of SO3 that were foundon one copper smoke-catcher after 100 hours, burning witheach of the burners named, the results being calculated tothe uniform rate of consumption, 100 litres per hour :—
SO*Mgrms*
Flat-flame burner • • • •Argand burnerIncandescence burner without mantle 26*0Incandescence burner with pure thoria mantle 28*1Incandescence burner with ordinary thoria-ceria
mantle *• 29*2
The rare earths found in the first deposit appeared, from*analysis and photometric tests, to consist of thoria andceria in the same proportions as in the mantles from whichit was derived. The author concludes that ceria is notmore easily driven off from the mantle than thoria is.
—H. B.
Acetylene Purification. G. Benz. Zeits. f. angew. Chenu1899, [45], 1083—1084.
THE carbide used, yielded per kilo., 300 litres of acetylene,,containing 0*08 grm. of hydrogen phosphide and 0*25 grm-of sulphuretted hydrogen, i litre of either Frank's solutionof cuprous chloride or Ullmann's chromic acid (see thisJournal, 1899, 568 and 743) sufficed to purify 10 to 14 cb.m-of this acetylene. Loss of acetylene owing to oxidation..attended the use of potassium permanganate and bariumperoxide, both of which almost completely removedhydrogen phosphide, but only partially removed hydro-gen sulphide. Potassium bichromate proved inefficient^Bleaching powder containing 20*95 per cent, of available-chlorine was tried, first on the ordinary acetylene, and after-wards on mixtures of acetylene with hydrogen phosphideevolved from a given weight of calcium phosphide* 40 grms-mixed with cellulose were packed to a depth of 12 to 13 cm.in a vertical cylinder, and the gas from 200 grins, of carbideand small amounts of phosphide was efficiently purifiedthereby. When, however, the gas from 50 grms. of carbideand 3 grms. of phosphide, was subsequently passed throughthe same mass, traces of hydrogen phosphide were found to*have escaped absorption by it. Experiments showed that1 cb. m. of acetylene could be purified by 20 grms. ofbleaching powder, but that the gas thus purified containedtraces of carbonic oxide and chlorine compounds. Thelatter could be subsequently removed by caustic potash orslaked lime, which would also decompose chloride of nitro-gen, if, as has been stated, this compound is really formedin small quantities by the interaction of ammonia in theacetylene on the bleaching powder. Removal of the ammoniaby washing causes a loss of acetylene. It was found thatunder no conditions did the passage of acetylene throughbleaching powder and cellulose cause a dangerous elevationof temperature ; the maximum rise observed with 60 litres-of gas and 40 grms. of bleaching powder was 2^° C.Acetylene purified by means of bleaching powder has "been,stated to corrode metal burners. The corrosive action mustbe due to the chlorine compounds, which may be removedas aforesaid, and not to impurities.—J. A. B.
Mixture of Acetylene and Oil Gas, The Present Position ofRailway Carriage Lighting by a. Bork. J . fiir Gasbe-leucht. 42, [45], 700—761.
OIL-GAS, which is obtained by the gasification of oil dis-tilled from lignite, is usually stored under a pressure of 10atmospheres. The use of acetylene alone (" neat acetylene " ) ,under compression, is attended with danger, but mixturesof oil-gas and acetylene containing as much as 50 percent, of acetylene may be used with safety. A mixtureof 75 per cent, of oil-gas and 25 per cent, of acetylene hasbeen adopted in place of oil-gas alone, on the PrussianState railways. 'Next year, when this mixture will be in usethroughout that railway system, the consumption of carbidefor the production of the acetylene required, will amount to4,500,000 kilos. The mixture is also being adopted on
32 THE JOUBNAL OF THE SOCIETY OF CHEMICAL INDUSTBY. [Jan. si, woo.
other German rail way s. At the present price of carbide,lighting by this mixture or by acetylene is, per candle-power obtained, only half as costly as lighting by theoil-gas formerly used. Thus the average cost of a cubicmetre of gas is :—Oil gas, 30 pf.; mixture, 54 pf.; acetylenealone, 130 pf. At a consumption per hour of 27*5 litres,oil-gas gives a light of five candles (Hefner-units), and themixture a light of 15 candles, whilst acetylene alone, gives15 candles at a consumption of 12 litres per hour. Themaintenance charges and interest on the plant on thewaggons and at the filling stations amount to 0 • 8 pf• perburner, and the total cost of each flame per hour thusbecomes:—Oil-gas, 1*625 ; the mixture, 2*285; acetylene,:2*312 pf. The cost per candle-power per hour thereforeis:—With oil-gas, 0*325; with the mixture, 0*152; andwith acetylene, 0-153 pf.—J. A. B.
Acetylene Lighting for Ships. A. Frank. J. fiirGasbeleucht. 42j [45], 762.
ACETYLENE generators for use on board ships should beso designed that the maximum charge of carbide will yieldno more gas than will fill the gasholder at a single operation,and should be of the type in which carbide is dropped intowater. The gasholder must not be of the floating bellpattern, but should be a closed receiver for the gas, withsuperposed water tank from which a pipe leads nearly tothe bottom of the receiver. The water tank should becovered, but its top should be provided with a vent tube.The pipe by which the gas leaves the receiver should risefrom the top of the latter, and be provided with a devicefor the separation of spray from the gas. The gas intendedfor lighting the interior of the vessel must be adequatelypurified. The services must be so laid that thev mayaccommodate themselves to the movements of the ship'shull. Acetylene may be installed on shipboard with nogreater risk than attends coal-gas or oil-gas lighting, if•the above precautions be observed.—J. A, B.
Calcium Carbide, The Colour of. II. Moissan. Hull.Soc. Chim. 21, 921—922.
CALCIUM: carbide, prepared in a pure condition by heatingwith pure carbon from acetylene, either metallic calcium, itshydride, or nitride, or by the action of heat on the sub-stance CoCa.CoHo.4NHo, is colourless or white, and in thinlamina* or small crystals perfectly transparent. That thecommercial substance owes its opacity and colour to thepresence of iron was shown by melting one of the purespecimens above mentioned with a trace of ferric oxide ;after cooling it presented exactly the appearance of thecommercial substance.—J. T. I).
Calcium Carbide, Composition of some Commercial Speci-mens of. H. Moissan. Hull. Soc. Chira. 1899, 21,865—87L
WHEX calcium carbide first became a commercial product,coke containing much mineral matter was used in its pre-paration, and the lime employed contained aluminiumsilicate, sulphate, and phosphate. The carbide obtained,gave acetylene which was contaminated with hydrogenphosphide and sulphide. Purer carbon and a better quality oflime are now used, yet the carbide always leaves an insolubleresidue when treated with water. A good fused carbideshould show a sharp crystalline structure when broken, andby reflected light should appear reddish-brown. 1 grm. ofcalcium carbide should theoretically yield 349 c.c. of acety-lene ; good specimens, when treated with milk of limepreviously saturated with acetylene, gave from 292# 8 to318*77 c.c. Poorer qualities which were porous and non-crystalline, gave only 228# 6 to 260-3 c.c.
For analysis, the insoluble residue was obtained by decom-posing carbide with a solution of sugar—the lime formedbeing dissolved as calcium sucrate. The residue was washedwith sugar solution, water (both free from carbon dioxide),alcohol, and finally with ether, then being dried at 40° invacuo. A microscopic investigation led to the conclusionthat the residue contains carbon, calcium, and iron silicides,calcium sulphide and graphite. Treated with dilute hydro-chloric acid (1:10) the residue loses in weight, and calcium,aluminium, and phosphorus can be detected in solution.The carbon silicide and graphite are not acted upon. The
residue from the dilute acid, when treated with concentratedhydrochloric acid, undergoes a further loss in weight, calciumand silicon passing into solution.
Silicon.—This is present principally in the form ofcarbon silicide—characteristic green to blue hexagonalcrystals under the microscope. It has the sp. gr. 3 • 12, andmay be isolated by treating the residue with boilingsulphuric acid, then hydrofluoric acid, and separatingfrom graphite by bromoform (sp. gr. 1*9). The siliconlikewise occurs combined with calcium and also free.Silicon hydride has been obtained by acting upon thecarbide residue with concentrated hydrochloric acid, butno carbide has been examined which gave an acetylenespontaneously inflammable in the air, due to the presenceof silicon hydride.
Sulphur.—Calcium sulphide has been detected in theresidue by a microscopic investigation with a dilute solutionof lead acetate and acetic acid. This calcium sulphide inpresence of lime does not give sulphuretted hydrogen withwater. The sulphates present in the lime used for theproduction of the carbide, are reduced, and calcium sul-phide (which does not give hydrogen sulphide) is formed;but if aluminium silicate be also present, then carbon silicideis formed along with aluminium sulphide (Mourlot, ComptesKend. 1895, 123, 55), which with water gives hydrogensulphide- Silicon sulphide cannot be present, for it husbeen shown that this is easily volatile. Carbide which con-tains a certain quantity of sulphide, gives on decompositionwith water a volatile organic sulphur compound. Thesulphur contained in three specimens of carbide was 0*37,0'4!i, and 0*74 per cent, respectively.
Iron.—This is present in the form of silicide or carbo-silicide. The quantity depends on the impurity of thecarbon employed.
Phosphorus is usually found as calcium phosphide, butit also occurs in small metallic-looking lumps containingiron and silicon.
Carbon exists in the carbide in the form of graphite.No carbon in the form of diamond could be found.—J. McC.
Washing Coal Pyrites and other Minerals, Apparatus forCleaning or. C. Burnett, Durham, and H. T. IsTewbigin,Newcastle. Eng. Pat. 25,852, Dec. 7, 1898.
See under I.9page 30.
Coals for Gas Manufacture, Laboratory Method for theAnalysis of. J . G. A. Ti ho din.
See page 12.
PATENTS.Smokeless Combustion in Steam Generator and other Fur-
naces, Method and Means for Effecting. A. KoeppeLeipzig. Eng. Pat. 26,270, Dec. 12, 1898. '
THE ash-pit is closed air-tight, and the air necessary tosupport combustion is admitted at a suitable point abovethe grate surface, so that incandescence may spread throughthe grate from the front thereof, over the "fuel, causing theuppermost layer of such fuel towards the back o f thefurnace to become incandescent, so that passage of thesmoke through the flues of the furnace is obviated. Theair is heated before its admission to the furnace, by passagethrough a pipe arranged in the flues of the furnace Thegrate surface consists of two or more layers of arate bar*of which the front layer is pivoted upon one of its pointsof support, and means are provided to swine or rock thesobars about their point of support.—R. S.
THE claim is for «the production of refractory material[coke, charcoal, &c] , either in a l00Se or in I commctor moulded state, by passing carburetted 4 e s ™ or
substances generating carburetted gases or%apiur«»-through a mixture of carbon and refractory sub?t4eesexposed to a glowing heat in suitable retorts.^—R. s.
Artificial Fuel Process for the Production of A Kernjun., Hamburg. Eog. Pat. 20,745, Oct. 17,
SPIRITS of wine/, or mineral and vegetable oils esnopetroleum, arc absorbed by kieselgShr or other
.Tan. 31,1900.] THE JOURNAL OF THE SOCIETY OF CHEMICAL INDUSTRY.
porous or infusorial material, earth, or artificial imitationthereof, in conjunction with wood, charcoal, or othercombustible material. The result is a solid fuel, which canbe carried about or sent for transit without danger. —K. S.
Gas Producers. M. Taylor, Paris. Eng. Pat. 1574,Jan. 23, 1899.
To minimise resistance between the producer and theengine, the inventor employs a charcoal furnace as gene-rator, and passes the gas through a series of water-jackettedpipes and a set of air-cooled pipes, after which it is passedover water to remove ashes and dust, and thence to theengine. The steam formed in the jacketted pipes, is utilisedfor blowing into the generator along with air, the outlet ofthe steam pipe being in an opposite direction to that of theair inlet, so that when there is no suction through thegenerator, the steam escapes direct into the outer air. Theproportion of steam and air admitted; is regulated byq.djlisting the air tap.—C. S.
Liquid Fuel, Steam-Boiler Furnaces for the Combustion of.R. A. Meyer, Batavia, Java, Eng. Pat. 1962, Jan. 27,1899.
THE inventor claims the combination of the front end of thefurnace, and an air damper, with a device for " conductingand heating the draught of air for assisting the combustion ofthe fuel, consisting of ' a hollow cone-frustum' or cylinderprovided with apertures and having upright vanes or parti-tions traversing its external surface from end to end, leavinga space between each vane, said spaces forming channels forthe passage of the incoming air, and the conducting of it ina hot state to the fuel spray, the said device being eithertightly or movably fitted in the front end of the furnace,and surrounding the injector or injectors of fuel." As analternative, he uses " a series of short tubes fitted in thefront end of the furnace, open at both ends and surroundingthe injectors."—C. S.
Gas, Apparatus for Carhuretting or Enriching. W. Irwin,Manchester. Eng. Pat. 20,792, Oct. 17, 1899.
THE apparatus consists of two vessels or chambers, oneabove or placed at higher level than the other, to holdbenzene or other enriching liquid, and the other divided intocompartments provided with strips of material for absorbingthe enriching liquid. The two chambers are connected bya supply pipe, arranged so that the supply of liquid isregulated, on the " hen fountain " principle, by the amountabsorbed; and the gas pipes are carried up above the levelof the upper chamber, in order to prevent the liquid fromfinding its way into the mains.—C. S.
Injectors or Apparatus for Burning Liquid Fuel. J.Holden, Wanstead, Essex; A. M. Bell and J. C. Taite,London. Eng. Pat. 2950, Feb. 9, 1899.
THE injector has " two or more liquid fuel supply ports orpassages, the outlet ends of which are so arranged as todeliver the liquid fuel at two or more points along theinjector, the arrangement being such that the mixture ofliquid fuel and steam or other spraying fluid, after passingthe first outlet, will come into contact with and spray theliquid fuel flowing through the other outlet or outlets,whereby a larger quantity of liquid fuel than usual can beeffectually sprayed with a given quantity of spraying fluid."Around the main nozzle of the injector is eccentricallyplaced an external steam ring, " the centre of the ring andthe orifices for the exit of steam from the ring beingarranged below the centre of the said nozzle, so that mostof the air induced to flow through the ring by the jets ofsteam issuing from its lower forward portion will passbetween the lower portion of the ring and the main nozzle,and thus be caused to rise upward through and becomeintimately mixed with the sprayed fuel issuing from themain nozzle." The injector may be wrorked by means ofcombustible gas or vapour, supplied under pressure insteadof by steam.—It. S.
Carburetted Gas, Apparatus used in the Production ofB. J. B. Mills, London. From La Societe Anonyme desFontaines a Gaz, Fontaines-sur-Sa6ne, France. Eng.Pat. 1020, Jan. 16, 1899.
THE claim is for " an absorbent material consisting of paperpulp (wood or rag cellulose) in any of its forms, combinedwith an agglutinant and moulded into a convenient formfor use with various kinds of carburetting apparatus," toreplace the wood blocks hitherto in use.—C. S.
Illuminating Gas, Process of and Apparatus for theProduction of W. Knapp and K. Steilberg, Hamburg,Germany. Eng. Pat. 16,619, Aug. 16, 1899.
THE process consists in continuously feeding melted resin—in amount corresponding to the production of gasrequired—into a series of superimposed retorts, filled withiron or steel turnings and set in a furnace, the resin beingvolatilised at a red heat in the upper row, whilst the vapoursare gasified in the under row. The supply of melted resinis regulated automatically by means of rods and leversactuated bv the rise and fall of the gasometer bell.—C. S.
Liquid Fuel Lamps. C. A. Day, London. From E.Miller and Co., Meriden (Conn.), U.S.A. Eng. Pat.16,847, Aug. 19, 1899.
THE claim is for an outer and inner wick-tube, the latterbeing slightly lower than the former at the top; a perforatedcylindrical spreader located within the said outer tube tosupply air to the flame, and movable with relation to bothtubes, the spreader also having an inward bend near itslower part, and carrying a flange located near the bend andserving as an extinguisher. A space is left between theflange and spreader to allow of the escape of vapour ; andan adjustable stop is provided in order to prevent the wickfrom being turned up too high.—C. S.
EEFERENCE is made to Eng. Pat. No. 24,328 of 1897(this Journal, 1898, 1135). The inventor takes " the open-topped shank of an ordinary (flat-flame) gas burner,known in commerce as a ' drawn-through blank,' consistingof a tube closed at one end; but instead of taking outthe bottom, he pierces one or more very small holes inthe bas-e, for the admission of gas." The upper partof the tapered, threaded end is perforated for theadmission of air; the open top of the shank is slottedto receive the crossbar and mantle support referred to inthe above patent; and over the shank thus preparedis slipped the tubular part, also slotted, of a funnel-shapedburner mouth covered with wire gauze. Burner mouths ofother forms are also described. A disc "of metal is screwedon to the shank above the air inlets to'prevent li^htiback ; this disc may take the form of a ffallerv for a ^&c.—H. B. b J *
Incandescence Burners and Mantle Suppo?*ts. J. H HDuncan, London. Eng. Pat. 27,205, Dec. 23, 1898.'
THE improvements may be applied either to Bunsen tubeshaving parallel sides or to those consisting of two co-axialtruncated conical tubes, as in Eng. Pat. 10,497 of 1894There are no arrangements within the burner tube to causeany abrupt change in the upward flow of the <*aseousmixture, the top of the tube being simply covered with adisc perforated with a ring of holes from which narrow slitspoint radially inwards towards the axis of the tube. Thistop plate, which has a socket recessed in it to hold themantle support, is claimed. The plate may form part of acap which can be slipped upon or removed from the mouthof the Bunsen tube at will. The mantle support may becemented into its socket, and the mantle may be fixed to theend of the support, so that the cap, mantle, and supportmay be removable and portable as a whole, to facilitate themounting of mantles upon the burners by unskilled personsThis removable attachment is claimed. H. B.
D
THE JOUBNAL OF THE SOCIETY OF CHEMICAL INDUSTRY.[Jan. 31,1900,
Incandescent Materials and Lamps suitable for ElectricLighting, Manufacture of. L. W. Gans, Frankfort-on-the-Mainc. Eng, Pat. 356, Jan. 6, 1899.
THIS is a development of the use of " lustrous preparationsof the noble metals " (Eng. Pat. 17,896, 1898 ; this Journal,1899, 746) on the lines of Nernst's lamp (see this Journal,1898, 653). An earth, or a mixture of earths, is made into ahollow cylinder or other suitable form by means of a mould.Magnesia, lime, baryta, thoria, zirconia, &c, may be used, thebest results having been obtained from magnesia, mixed withabout 20 per cent, of thoria containing about 1 per cent, ofeeria. After heating the cylinder till red hot and allowingit to cool, the interior is coated with a " ceramic lustrous pre-paration of one or more of the highly infusible metals of theplatinum group, in mixture or solution with an ethereal oil/ ,
such as lavender oil. In the case of rods, the solution maybe applied in a thin strip. The material is then burnt inas usual. When such a body is used for electric lighting,the thin film of metal acts as a conductor from the outset,heating the refractory earths, so that after a minute, thecylinder or rod itself becomes a conductor, and is raised toincandescence. Owing to the highly refractory character ofthe metal film, it is not destroyed; but if it contain muchosmium it should be protected by a bulb that is exhaustedor filled with neutral gas. Osmium has been found to givethe best results. Suitable dimensions for a hollow cylinderare :—Length, 5 to 15 mm. ; thickness of wall, 1 to 5 mm.;internal diameter, 2 to 3 mm H. B.
Burners for Gas-lighting by Incandescence. W. L. Voelkerand The Voelker Incandescent Mantle, Ltd., London.Eng. Pat. 18,750, Sept. 16, 1899.
A BURNER is claimed, the Bunsen tube of which has atits lower end a lenticular enlargement or chamber, pro-vided with air-inlet apertures in its lower or upper wall, anda perforated ring or annular valve adapted to regulate theair-inlets. In the upper part of the gas-inlet nipple there isplaced a perforated diaphragm, covered by a correspondingperforated disc, which may be turned, by means of armsprojecting outside the burner, so as to regulate the flow ofgas. The chimney gallery is provided with guards orshields to protect the mande from draughts.—H. B.
Electric Incandescent Lamps. W. P. Thompson, London.From A. Sinding-Larsen, Fredriksvaern, Norway. Eng.Pat. 18,968, Sept. 20, 1899,
"TUP: glass bulb (of the lamp) is filled with a gas orgases under tolerably high pressure, which gases mustbe of such a nature that they do not attack carbon evenat the highest temperatures, as for instance argon ornitrogen. The glass vessel must be of suitable strength.The minimum pressure in the lamp when the same isin action may be taken to be about four atmospheres.5.
In one modification the lamp consists of a U-shaped tube,provided with a filament; " in the exhausted interior of thetube there is a little drop of quicksilver, which, when thefilament is rendered glowing by means of the current, isquickly evaporated and produces the desired high-pressureatmosphere."—H. B.
Incandescence Oil Lamps. J. C. C. Read, London. Eng.Pat. 21,250, Oct. 24, 1899.
MODIFIED forms of flame-spreaders are described andclaimed for insertion into the wick-tubes of oil lamps of thecircular-wick type, and also a guide tube to ensure theuniform raising of the wick.—H. B.
Acetylene and other Gas; Apparatus for Generating andStoring. W. W. Beech and H. Jones, both of Stockport.Eng. Pat. 24,409, Nov. 18, 1898.
WITHIN the tank of a bell gasholder is fixed a closed waterreceptacle, the top of which has the same curvature as thecrown of the bell, so that when the bell is in its lowermostposition there is practically no air-space between its crownand the top of the receptacle. Water passes from thereceptacle, which has a vent tube for the admission of airthrough a valve controlled by the movements of the bell, toone or other of several generating chambers placed beneath
the tank of the gasholder, into which thepasses after traversing a washer. The pipe bywater enters each generating chamber, and the gas exit pipe,are controlled by valves which are closed au tomat ica lwhen the lid of the generating chamber is opened, m ecarbide in each generating chamber is placed on pertoiateainclines in a container with vertical partitions, so that thewater entering at one end attacks the carbide in the lowerpart of the first compartment, passes upwards, and overeach partition in turn until the whole charge is exhausted.
1 —J. A. i>.
Acetylene Generators. W. Ellen, Manchester. Eng. Pat.24,501, Nov. 21, 1898.
WATER is supplied from the tank of a bell gasholder to thelower end of an inclined generator, through a pipe withvalve controlled by the movements of the bell. The carbideis supported in the generator on a loose tray with partitions,and the tray can be withdrawn for recharging by opening alid which forms the upper end of the generator. This lidis connected with the lever of a tap on the pipe whichconveys the gas from the generator to the gasholder, insuch a manner that the tap is on when the lid is closed, andoff when the lid is removed.—J. A. B.
Acetylene Gas, Apparatus for Generating. C. J . Baileyand J. H. Nicklin, both of Manchester. Eng. Pat. 24,785,Nov. 24, 1898.
A CLOSED vessel, from which the gas produced in thegenerators expels water into an overhead tank, constitutesa gasholder from which a service is supplied. Water isfed from the lower part of the gasholder to the genera-tors, through pipes which lead into larger pipes by whichthe gas escapes from the generators to the gasholder. Thelatter pipes bifurcate from a single pipe which enters thegasholder, and each branch and each of the water-supplypipes is provided with a cock. The generators are usedeither singly or together by manipulation of these cocks.When a generator is exhausted, the water may pass on to asubsidiary generator connected to the upper part of theprimary generator.—J. A. B.
Acetylene Gas, Apparatus for Generating. P. Bucher,Mannheim, Germany. Eng. Pat. 25,297, Nov. 30, 1898.
A TANK containing water has one end covered by a dome,the side of Avhich extends beneath the water. A cylindricalreceptacle containing carbide is attached to a bent armfastened to a spindle, which is rotated in the upper part ofthe open end of the tank by means of an external handle.The rotation of the spindle brings the carbide receptacle underwater beneath the dome, and thereupon gas is evolvedand collects in the dome, Avhence it is conveyed for use. Acontinuous supply of gas is secured by the use of tAvointerchangeable carbide receptacles.—J. A. B.
Acetylene Gas Generators. O. Imray, London. FromC. W. Beck, Chicago, U.S.A. Eng. Pat. 636, Jan. 10,1899.
ABOVE a generating chamber containing water is a cylin-drical chamber in which a carbide hopper is loosely sup-ported. Above the cylindrical chamber, is a chamber inAvhich is a gas bag, loaded by a weight attached to a rod,Avhich passes dowmvards to the mouth of the carbide hopper!The loAver end of the rod is cylindrical and closes againstthe flexible Avails of the mouth of the hopper. Whenhowever, the gas bag is nearly empty, the rod is so fardepressed that a groove on it allows carbide to passthrough into the generating chamber, whence the gas evolvedpasses round the sides of the hopper and inflates the o-asbag thereby raising the rod and stopping the p a s s a g e dcarbide from the hopper. The generating chamber isattached to the cylindrical chamber by eccentrically-setclamps which compress a packing .ring between the flangesof the two chambers.—J. A. B.
A CIRCULAR casing divided into compartments, each ofwhich has a hinged flap as its bottom, is mounted above a
Jan. si, woo.] THE JOURNAL OF THE SOCIETY OF OHEMIOAL INDUSTRY-
shoot leading into water in a bell-shaped receiver. The flapsare held in position by a horizontal plate, which is rotate*]by hand or by gearing actuated by the movements of the bellof the receiving gasholder. In the plate is a slot, whichallows one flap to fall and discharge into the shoot thecarbide with which the compartment has been previouslycharged. As the rotation of the plate continues, the fallenflap is automatically raised to its position, and the flap ofthe next compartment comes over the slot and falls. Thegas generated passes from the dome of the receiver into thegasholder.—J. A. B.
Acetylene Gas ; Apparatus for Generating. H. Berger,Berlin, Eng. Pat. 4223, Eeb. 25, 1899.
A VERTICAL shaft passes through a stuffing box in thebottom of a generating tank containing water, and carries atits top, which is above the level of the water, a horizontaldisc provided with a slot. Boxes containing carbide havehinged bottoms which protrude so that they are supportedby the disc, whilst the opposite ends of the boxes are sup-ported by hooks on the wall of the generating tank. Theshaft and disc are rotated by means of a chain attached tothe gasholder bell, and the hinged bottoms of the carbideboxes drop, and discharge the carbide into the tank, as theslot in the disc passes in turn under the protruding end ofthe bottom of each box. The gas generated passes to thegasholder.—J. A. B.
Acetylene Lamps. E. J. Dolan, Philadelphia, U.S.A.Eng. Pat. 5221, March 9, 1899.
WATER passes from a chamber to a lower chamber contain-ing carbide through a valve controlled by a threaded rod•with milled head. The water is conducted from the nozzleof the valve to the carbide bv one or more small chains.Below the carbide chamber is a chamber for the receptionof the residual lime, which is removed from the carbide bythe rotation of a spindle which carries a grate formingthe base of the carbide chamber. A projection which extendsfrom the wall of the carbide chamber prevents the carbidebeing rotated with the grate, and thereby facilitates theremoval of the lime from the lumps of carbide. A burner,reflector, and lens are provided.—J. A. B.
Acetylene Gas, Apparatus for Generating. C. K. Mills,London. From G. Tabard, Lyons, France. Eng. Pat.10,410, May 17, 1899.
TIIK movements of the bell of the gasholder, into which theacetylene evolved passes, operate a valve on the orifice of acarbide hopper placed above a generating tank containingwater. The valve may be conical and held against anelastic seat until the bell descends nearly to its lowestposition ; or it may be a bent tube, moved by radial armsover a smaller tube similarly curved, which forms the shootfrom the carbide hopper. The smaller tube is provided atits lowermost point with a hole through which the carbidefalls when the outer tube is moved upwards and leaves thehole exposed.—J. A. B.
Acetylene Gas Lamps, A. Gerdes, Berlin. Eng. Pat.14,698. July 17, 1899.
A SCREW conveyor at the base of a carbide receptacle passescarbide into a generating chamber containing water. Theconveyor is rotated through its hollow spindle, which passesup through the carbide receptacle, by clockwork mechanism,which is retarded by a friction brake, actuated by thedistention of a diaphragm, when the gas production exceedsthe consumption. By means of a winged nut the dis-charge of the carbide may also be arrested by hand.
—J. A. B.
Acetylene Lamps, Safety. E. S. Bond, Hands worth, Staffs.Eng. Pat. 15,336, July 26, 1899.
WATER is supplied from an upper chamber to carbide in alower chamber through a passage in a stopcock and anannular passage, provided with perforations in the upperpart of its outer walls, and a distributing flange. The gasgenerated passes through another larger passage in thestopcock to the burner. The passages in the compoundstopcock are so arranged that rotation of the plug of the
cock closes first the water passage, and next the gaspassage also.—J. A. B.
Acetylene Gas, Apparatus for Mailing. A. Dauber,Bochum, Germany. Eng. Pat. 17,343, Aug. 26, 1899.
A HOPPER containing carbide is mounted i ^ the top of abell floating in a tank, and communicates with a verticalshoot provided with a helical guide. This shoot slideswithin a fixed pipe, the lower end of which is a funneldirected so that it discharges into a small tank withperforated sloping bottom, placed within the large tank.The carbide resting on the helical guide falls into thefunnel and thence into the tank, whenever the descent ofthe bell brings the opening in the side of the shoot, inwhich is the helical guide, opposite the mouth of thefunnel. A perforated tube which forms the axis of thehelix carries off any gas which escapes up the shoot.
T A T ?—«J • A . JL>.
Acetylene Gas Machines. F . Matthews, Montreal, Canada,Eng. Pat. 17,406, Aug. 28, 1899.
BUCKETS, charged with carbide, are supported by springcatches on a vertical hollow stem, up the interior of which arod is forced to a certain extent each time the bell of thegasholder descends. The rod in its ascent disengages inturn the catch of each bucket, and the carbide is thusdischarged into a shoot with baffle plate, which leads intothe tank of the gasholder. The gas evolved, escapes into aninner dome sealed in the water in the tank, and thence tothe outer bell and the place of consumption. Taps areprovided for changing the water in the tank, withoutproducing a dangerous mixture of acetylene and air.
Acetylene Gas Generators. F. Ginnasi, New York City,U.S.A. Eng. Pat. 20,256, Oct. 9, 1899.
T H E bell of a gasholder, when it descends to a certainpoint, compresses by means of an arm a flexible waterreservoir, from which water is thereby forced into areceptacle containing carbide, from which gas is evolveduntil the flow of water is arrested by the removal ofpressure from the flexible reservoir, owing to the rise ofthe bell due to the influx of the gas evolved.—J, A. B.
A CARBIDE receptacle, divided into several compartments,has its bottom formed of a flexible band, the free end ofwhich passes over rollers and is loaded by a weight. Theweight causes the receptacle to travel horizontally over thegenerating tank, and an each compartment comes clear ofthe band, its contents fall through a shoot into the water inthe tank, from which the gas evolved passes to a bell gas-holder. The movements of the bell, by means of a cordand pawl gearing, control the travel of the carbide receptacle,so that gas is generated only when the gasholder is nearlyempty.—J. A. B.
Acetylene, Manufacture of C. Kellner, Golling, Austria.Eng. Pat. 21,035, Oct. 20, 1899.
THE carbide is decomposed by a solution of calcium chlorideinstead of by simple water. The rate of generation of erasis said to depend upon the degree of concentration of thesolution, which is varied to suit requirements. With freshsolution, the residual lime produces some calcium oxy-chloridc. The solution may, however, be used repeatedlyby adding to it the amount of water needed to decomposeeach batch of carbide.—J. A. B.
Electrical [Calcium Carbide'] Furnace. E. B. PhillipsLeicester, and W. H. Bray, Bristol. Eng. Pat. 26,214*uec. 12, 1898.
THIS is a furnace of the horizontal, open-hearth type Theelectrodes are held in clips which are connected to rack-andpinion travelling gears fixed on the top of the masonry sothat they can he rapidly adjusted in the hest positions bvmeans of hand wheels. The bottom of the furnace also is amovable block of material carried on a vertical screw rod,
2
THE JOURNAL OF THE SOCIETY OF CHEMICAL INDUSTRY, [Jan. 31,1900.
so that it can be lowered to increase the capacity of theapparatus, and to remove the carbide already formed.
Gas Liquor and Tar, Separation of. G. Ymonet. J. filrGasbeleucht. 42, [48], 814.
I N English and German gasworks a vertical ^ partitionreaching nearly to the bottom of the tar and liquor wellhas been adopted, in order that the tar, which naturallysinks to the bottom of the well, may flow away beneath thepartition, while the liquor remains on the inlet side of thelatter. Melon has recommended this plan, while Brunethas further recommended that water be admitted to thetar side of the partition in order that it may take upammonia from the tar. The author admits weak liquorfrom the last scrubber to the tar side of the well, in placeof clean water, with the same object, and when it hasattained a strength of, say, 1*5° to 2° B., he pumps itfrom the tar well to the first scrubber, where it takes upmore ammonia.—J. A. B.
BY heating benzene with phosphoric anhydride for somehours to 110°—120°, a brick-red mass is obtained, whichafter keeping in a closed glass tube between plugs ofporous kaolin to absorb excess of benzene, gives analyticalfigures pointing to the formula 1^O5.CCHG. The authorregards this as benzene-di-metaphosphoric acid :—
P 2 O 4 (OH)(C e H 5 ).
By passing dry ammonia into the substance diffusedthrough u large excess of benzene, a yellow substance isformed :—P2O.t(< )XII4)(C ( iH5). Alkalis transform the brick-red acid into vellow substances, which no doubt are the alkalisalts, but which the author has been unable to isolate foranalysis.
If the mixture of benzene and phosphoric anhydride beheated to over 200° C , another substance is formed, whichthe author regards from its analysis, as benzene-tridimeta-phosphoric acid, C,?H3 j (l^C^);* • (OH)3.
Similar compounds are formed by other benzene hydro-carbons, by anthracene, &c.—J. T. I).
Picene, Synthesis of. T. Hirn. Ber. 1899, 32, [17],3341—3343.
THAT picene is the phenanthrene of the naphthalene serieswas first suggested by Graebe and Walter (Ber. 14, 175)and subsequently confirmed by Bamberger and Chattaway,who showed that it had a β-fi connection between thenaphthalene nuclei. The position of the dimethin (CH:CH)bridge has, however, not hitherto been defined.
Seeing that naphthalene is not favourably disposedtowards the formation of β1 #> derivatives, Bamberger andChattaway considered that of the three possible formula;,the following was the most probable :—
\
and this view has been further strengthened by a successfulattempt the author has made to obtain picene by synthesisfrom α-dinaphthylethylene in a manner exactly analogousto the formation of phenanthrene from diphenylethylene.
—I). B.
Diatomaceons Wax, and its connection with Petroleum.G. Kraemer and A. Spilker. Her. 32, [15], 2940—2959.
THE authors examined the " lake mud " from an extinctlake in the Uckermark district and found it to consist ofdiatom remains from which an average of 3 • 6 per cent, of
wax couid be extracted with toluene, after prolonged diges -tion of the mass in 5 per cent, hydrochloric^ acid, lhewax resembles ozokerite, being dark brown, with a greasylustre and asphaltic fracture; melting point, 50 —70 ^ C.;sulphur content, 0 • 97 per cent.; ash, 2 • 42 per cent. Com-bustion tests indicate a somewhat large content of oxygen,carbon being 73 • 5 per cent, and hydrogen 10'9—11 • f>,percent. Like ozokerite, the wax is but little affected by coldfuming nitric acid; but is attacked in the warm, as muchas 38 per cent, being dissolved, against 8 per cent, in thecase of ozokerite. The residual, paraffin-like mass, yields,on repeated recrystallisation from alcohol, a body meltingat 79° C, and resembling the lekene isolated by Beilsteinfrom Tscheleken ozokerite (Ber. 16, 1547).
Another specimen of diatomaceous wax, extracted fromIfranzensbad peat, and containing over 10 per cent, of
taining a small quantity of water and of a crystallinehydrocarbon, which, when purified, melted between 51° and60° C. On the other hand, ozokerite is found to almostinvariably yield lekene of m.p. 79° C , and a gas practicallyfree from COo and CO, thus showing a low oxygen content;neither is any water formed during distillation. A furtherdifference between ozokerite and diatomaceous wax is shownin their behaviour towards alcoholic potash, the former beingonly slightly saponified, whereas 10 per cent, of the latter isdissolved, and furnishes a brittle resin when extracted byether*
On repeated distillation under pressure in a Thorpe andYoung apparatus, diatomaceous wax decomposes intogaseous and liquid hydrocarbons, almost destitute of solidparaffin, and resembling the petroleum hydrocarbons,except that the gas contains CO2, CO, and H2S, and wateris found in the distillate. The fraction, boiling point 130°—290° C , contains unsaturated bodies capable of absorbingbromine. For the sake of comparison, carnaiiba wax andJapan wax were distilled under pressure, and yielded afraction, 130°—290° C , identical with Tegernsee petroleumdistillate, with a gas containing carbon monoxide.
The authors regard this diatomaceous wax as a more pro-bable source of petroleum deposits than decomposed animalfats ; ozokerite being the product resulting from saponifica-tion and elimination of carbon dioxide; petroleum rich inparaffin the result of the action of low temperature andslight pressure ; the more viscous kinds of petroleum beingformed by greater heat and pressure ; and asphaltura by thecombined action of oxygen and the sulphur compoundspresent. The absence of diatomaceous remains theyascribe to corrosion of the siliceous skeleton by ammo-nium carbonate, &c, and admixture of the residue withalumina, lime, and other sedirnental matter, a hypothesis,they consider supported by the composition of the siliceouscover rock of petroliferous strata. As an example of thepossible magnitude of diatomaceous deposits, the ancientdried-up lake at Ludwigshof (Uckermark), is referred to,which, though only 900 hectares in area, is of an averagedepth of 7 metres, and is estimated to contain 63 milliontons of mud capable of yielding 200,000 tons of diatomaceouswax. Another point raised in favour of the diatom theoryis the possibility of the continued growth of new generationson the surface of accumulations of their defunct prede-cessors, and the preservation of the latter from decoinposition by reason of the oily matter contained in thediatom cells—phenomena also believed to occur in the* ^ „*___. m o s s e s g e n e r a l l y e ( S e c a l s o t W s J o u m a lof1895, 648.) . S.
PATENTS.
Coking, Process of, with Recovery oBrunck, Dortmund, Germany. ^
. 12*,
aT H E improvement consists in utilising the combustion
roducts In°^0:en%'°r ^ ^ ^ o n T t T ^
Jan. si, woo.] THE JOUBISAL OF TEE SOCIETY OF OHEMIOAL INDUSTRY.
GASES containing ammonium cyanide passed into water inwhich ferrous sulphide is suspended, produce a ferrouscyanide and ammonium sulphide, with reproduction ofammonium cyanide, according to the following equation:—
FeS (NH4)2S.
Hydrogen sulphide and carbonic acid do not interferewith the reaction. The process is stated to give a readymeans of recovering cyanogen compounds from coke andfoundry gases after extraction of ammonia by interposing,after the tar-separating and ammonia-absorption apparatus,another suitable absorption apparatus. Ferrous sulphate isadded to the washings, ferrous sulphide being precipitatedas required, by the hydrogen sulphide present. "Thecyanide of ammonium contained in the gas reacts nowon the sulphide of iron, producing ferrocyanide of ammo-nium, which passes into solution."—E. S.
Meta- and Paracresol, Separation of. F . Raschig, Lud-wigshafen, Germany. Eng.Pat. 18,334, Sept. 11, 1899.
THE process consists in converting the cresols into theirsulphonic acids, by means of concentrated sulphuric acid,in which 7n-cresol sulphonic acid is easily, but the p-com-pound only very sparingly soluble. The mixture maybe allowedto stand for about a week, and the crystals of p-cresol sulphonic acid are then removed ; or, a soluble sodiumsalt, such as the sulphate, may be added, in quantity sufficientto form the sodium compound of para-cresol sulphonic acid.The latter is then separated from the mother liquor, whichconsists of the meta - acid, sulphuric acid and smallquantities of sodium sulphate. The cresols are recoveredby removing the sulphonic acid groups by hydrolysis withsuperheated steam.—1). B.
Wood and Kindred Materials, Dry Distillation of F.Schmidt, Cassel, Germany. Eng. Pat. 19,713, Oct, 2,1899.
IT is proposed to utilise the shrinkage of the charge tocause fresh material to enter the retort from a hopperarranged on the top thereof. In this manner, the injuriouseffects of overheating the walls of the retort, and therebydecomposing the products of distillation are said to beprevented.—D.
Soot or Lamp-Black from Tar and other CarbonaceousSubstances, Manufacture of G. Wegelin, Kalscheuren,Germany. Eng. Pat. 22,337, Nov. 8, 1899.
See under XIII. A., page 56,
IV-COLOUKING MATTEES ANDDYESTUFFS.
Indigo White, Preparation of in a Stable and Con-centrated Form. Comp. Parisienne de Couleurs d. Aniline.French Pat. 287,894, April 15, 1899. Chem. Zeit. 1899,23, [97], 1031.
ACCORDING to this patent the Indigo white is isolated fromthe vat liquors by evaporation or precipitation with acids,and is then mixed with calcium hydrosulphite, or treatedwith alkali hydrosulphites or other reducing agents, suchas stannous chloride, with or without the addition ofalkalis. For example, a bath containing 3 kilos, of Indigowhite dissolved in 100 litres of water in the form of analkali salt is acidified with hydrochloric acid, and theIndigo white which separates out, pressed, stirred up with3 kilos, of calcium hydrosulphite, and kept in closedvessels. The addition of formaldehyde or benzaldehydeis advantageous in the precipitation of Indigo white, whichthen separates in a more stable form, possibly Avith theformation of an aldehydic compound.—C. A. M.
Alizarin Dyestuffs, Recent. G. Stein. Farber Zeit. [23],380—382, and [24], 398—400.
BEFORE reviewing the newer Alizarin dyestufPs, such as"Bordeaux/ ' «Indigo Blue/ ' Sky Blue, Violet, Green,Red, &c, the author briefly considers the older dyestuffs.
Alizarin Red is used with an alumina mordant forTurkey - red dyeing on cotton cloth and yarn, and forcalico printing in red and pink (alumina), brown (chrome),violet (iron) ; also for dyeing silk red on alumina, brownon chrome, and violet on iron, and for dyeing wool redwith alumina. It is also used in slubbing printing. Inpiece and yarn dyeing useful browns are obtained on woolwith chrome mordants. Fine browns are obtained with amixed mordant of alumina and iron. There^ is a longrange of Alizarin Reds from a bluish to a yellowish shade.
Alizarin-Purpurin is used in slubbing printing for redwith an alumina mordant, and in calico printing for brownwith chromium acetate. Discharge patterns on paddedshades of Alizarin-purpurin with chrome mordants arcreadily obtained by means of oxidising agents.
Anthracene Red is largely used for dyeing red on loosewool, and also on cloth and yarn; it is dyed either in anacid bath or on a chrome mordant.
Alizarin Orange is used for loose wool, yarn and cloth,also for silk yarn. It gives a fine fast orange with analumina mordant. It is also used in slubbing printing,calico printing, cotton rainbow printing, and in cotton-yarndyeing. On chrome mordants fine fast browns are obtained.
Alizarin Yellow R gives a useful orange-yellow on woolmordanted with chrome, and a similar shade when printedon cotton with chromium acetate.
Anthracene Yellow is much in demand, in spite of its highprice, owing to its fastness to light and milling ; on chromedwool, piece and yarn, it gives greenish-yellows and the sameresult is obtained in slubbing printing with chromiumfluoride and acetate mordants,
Coerulein gives olive-green shades on chromed wool, andthe same on silk with alumina, chrome, or iron» Goodresults are obtained in slubbing printing, and the dye-stuff is largely used in calico printing, with a chromemordant, although it has recently been replaced in somedegree by Alizarin-viridin. It is also used for dyeingcotton yarn mordanted with chrome and in cotton-silk unionprinting.
Alizarin Blue gives colours on chromed wool fast tomilling, rubbing, wear, and acids. On silk, fine reddishto greenish-blue shades are obtained. For printing calicoand cotton-yarn, as well as dyeing cotton-yarn and silk andprinting silk unions, the bisulphite compound of AlizarinBlue has been successfully used, the mordants beingchromium, nickel, and zinc.
Gallein yields on chromed wool and silk, violet-blueshades. It is occasionally used with chromium acetate incalico and cotton-silk union printing.
Anthracene Brown is one of the fastest and cheapestalizarin dyestuffs. It dyes very evenly on chromed wool,is extremely fast to light and milling, and fairly so to hot-pressing. It is used on chromed wool, silk yarn mor-danted with alumina, iron, and chrome, in silk rainbowprinting, in slabbing printing, in cotton printing (clothand yarn) with chromium acetate, and in discharge work onchrome and alumina mordants with chlorates and prussiates.
Of the more recent alizarin dyestuffs Alizarin Bordeauxmade its way into cotton-yarn dyeing soon after its discoveryin 1890. It gives a fast Bordeaux on alumina by theTurkey-red process, and the same result in calico printingwith an alumina-lime-tin mordant. Alumina prints ofAlizarin Bordeaux B l> are readily discharged by oxidation.With chromium acetate black to pale violet shades arcobtained. The blue obtained on wool with 2 to 4 per cent,of bichromate and 1 to 2 per cent, of tartar is cheaper than*Indigo or Alizarin Blue, faster to rubbing than Indigo, andextremely fast to light and wear.
The Alizarincyanines which were introduced into themarket after the Bordeaux give shades from the reddest tothe greenest shades of blue in the following order:
Alizarincyanine 3 R double, very fast to light and welladapted to wool dyeing and slubbing printing; Alizarin
38 THE JOURNAL OF THE SOCIETY OP CHEMICAL INDUSTRY. [Jan. 31,1900.
cyanine W R R for the same purpose ; Alizarincyanine Rextra gives a very clear colour ; Alizarincyanine 2 R givesvery even dyes; Alizarincyanines W R B> W B, and Gextra; Brilliant AUzarincyanineG; Alizarincyanine G G,which gives shades extremely fast to milling; Alizarin-cyanines N S and N S V; andBHlliant Alizarincyanine 3 G.These dyestuffs are sold in the form of paste or powder.They are used almost exclusively with a bichromate mor-dant in combination with tartar, lactic acid, or oxalic acid,and sometimes with chromium fluoride. The latter givesthe greenest shades of blue. Brilliant Alizarins G and 3 Gdiffer from most other alizarin colours in not only dyeingchromed wool, but in dyeing unmordanted wool in an acidbath, yielding shades which are very fast to light. Inprinting woollen cloth they are successfully fixed as aciddyes. Alizarincyanine It gives on Turkey-red oil prepare incotton printing, a good blue chrome lake, and with aluminaa fine violet. Both lakes can be discharged with chlorates.When dyed on cotton by the Turkey-red process, a fineheliotrope is obtained dischargeable by oxidising agents.The W K S brand is used for wool in an acid bath and issubsequently fixed with chromium fluoride.
Alizarincyanine Green G extra is of great importancein wool dyeing, and must be regarded as the first fast puregreen. It dyes chromed or unmordanted wool (in an acidbath), and gives shades very fast to light and brighter thanthose obtained with Coerulein. A duller and cheaper pro-duct is the E brand. Both are largely used in slubbingprinting, as is also the K brand, which is more soluble anddyes level shades more readily.
Alizarin Viridi?i, in paste, is a similar dyes tuff. Althoughit can be used in wool dyeing, it appears to be almost,exclusively employed in calico printing with a chromemordant. It gives a bright green fast to light.
Alizarincyanine Black G comes into the market both inpaste and powder form, and is used in wool dyeing with abichromate mordant in combination with tartar and withaddition of 10 per cent, of Glauber's salt and 3 per cent, ofacetic acid. Weak mordants give shades from a bluish-grey(bichromate mordant) to a bluish-green (chromium fluorideand oxalic acid). A fine bluish-black is obtained with 25to 30 per cent, of dyestuff. The black is very fast to lightand milling, and is used in printing cotton and woollencloth with chromium acetate as mordant. It is also usedin yarn dyeing and silk printing.
Alizarin Blue Black, although too expensive as a black,is, owing to its extreme fastness, well adapted for the shadingand darkening of colours. It is largely used for wool—piece, yarn, and loose—also in slubbing printing. The woolis mordanted with bichromate and tartar, to which 10 percent, of Glauber's salt and 3 per cent, of acetic acid are added,and it is then dyed ; or the dyestuff is worked in an acid bathand fixed, after dyeing, with chrome. The black obtainedby the second method is deeper and also faster to millingthan that obtained with chromed wool. For calico printingwith chromium acetate the brand B is used in the samemanner as in the case of Alizarincyanine Black G.
Alizarin Fast Black T has come into the market sincethe beginning of 1898. It gives a black on chromed woolfast to light, rubbing, and milling. It is also used in cottonprinting.
Alizarin Saphirol B was introduced into the marketbefore the foregoing colour, and is characterised by extremefastness to light and the property of dyeing extremelylevel shades. Wool dyes very level in an acid bath, thedye-bath is completely exhausted, and a fine bright blueresults. The Green obtained with a chrome mordant is fastto rubbing and stoving with sulphur. It is also used inslubbing printing, woollen cloth printing, and in dyeingwool-silk unions. When used for the latter purpose itbehaves like Indigo Carmine, i.e., it does not dye the silkin a boiling acetic acid bath.
The dyestuffs known as Brilliant Alizarin Blue G andi?, although, strictly speaking, belonging to the Thionineseries, are, owing to their extreme fastness, regarded asAlizarin colours. They surpass the-Cyanines in fastness tolight, rubbing, and milling. Artificial light is without action,and nitric acid gives the Indigo test. They are used indyeing chromed wool, but can also be dyed in one bath if
chromed after dyeing. They are also largely used inslubbing printing with chromium fluoride as mordant.
Brilliant Alizarin Blue S D is of special value as aprinting colour, and is extensively used for furniturematerials in direct printing or in discharge printing for paleIndiffO-blue imitations.
Of recent Alizarin dyestuffs other than those broughtout by the Elberfeld Farbenfabriken and dealt with m theforeo-oino-, Acid Alizarin Blue and Green of the HoechstFarbwerke may be referred to. They are dyed( in an acidbath and subsequently fixed with chromium fluoride.
Alizarin Heliotrope R and B B, brought into the marketquite recently, are dyestuffs used in cotton, silk, and cotton-silk union printing; on Turkey-red oil prepared cotton,with an alumina and lime mordant. With chromium acetate,it gives a blackish-blue lake. The alumina lake can be dis-charged with chlorates. The colours are used also for uooldyeing in an acid bath.—I). B.
Chrome-developing Colours. M. Liebert.J . Soc. Dyers and Colorists, 15, [12], 258—263.
THE prejudice among English dyers formerly attaching tothese colours is gradually being overcome, owing both tothe saving effected by their use and the intrinsic worth ofthe shades obtained.
The alleged difficulty in " matching off " with them existsonly in theory, and has long been overcome by the cottondyer, who uses developed colours (e.g., Primuline lied)very largely, to obtain a variety of shades.
The chrome-developing dyestuffs, like the Alizarins, owetheir dyeing power to the proximity of certain hydroxyls inthe molecule. They are essentially derivatives of " chromo-tropic " acid (dihydroxynaphthalene disulphouic acid, 1:8),the sodium salt of which, under the name of Chromoyen I..was the first colour of this group presented to the trade.Applied to the wool in the usual manner, i.e., in an acidbath with addition of Glauber's salt, it scarcely colours thefibre, and the rich terra-cotta brown only appears on sub-sequently adding to the same bath, " bichromate" asdeveloper. This brown, previously regarded as an ordinary" lake/ , must result in some way from oxidation, since non-oxidising mordants have no developing action on theChromogen I.; and, moreover, the " lake" once formed,cannot be removed from the fibre by any of the simplemethods applicable in the case of the Alizarins.
Chromogen I. must be looked upon as the typicalmember of the group, although the other members differfrom it in already dyeing the wool some colour of littlevalue in the acid bath, this, however, completely changingto the desired shade after developing with the bichrome*
Of this character are " Chrome Brown R O " andthe " Chromotropes," of which « F B " for navy blues and" S " for black are best known. It is, however, only recentlythat these dyestuffs have been applied and in such a manneras to ensure a fastness to milling in any way approachingthat attainable in the case of Chromogen I. The processan apparent contradiction—consists in adding, alono* withthe strongly oxidising bichrome and sulphuric acid employedas developer, lactic acid as a reducing agent. The mode ofprocedure is not changed. Care should be taken to ensurethat the acid dye-bath is quite exhausted before addingthe developer. After boiling with the latter for onehour, the bath should have a slightly greenish appearanceThe shades arc said to be rendered brighter us well usfester by the lactic acid. 3—5 per cent, of bichrome 3 percent, of sulphuric acid, and 3 - 4 per cent, of lactic acid havebeen found to be the most suitable proportions to useBrowns obtained by this method are said to be superior tnany obtainable from the « woods." ^ p u i o i to
But the chrome-developing dyestuffs are up to thepresent only a very limited series ; hence the introductionof various eulphonated Alizarins capable of S Sto the wool like the former in acid bath, andby means of the same chrome mixture which serveftooxidise and develop the dyestuffs of the S
on
Jan. 81,1900.]THE JOURNAL OF THE SOCIETY OF OHEMIOAL INDUSTRY.
chrome mordant. Acid Alizarin Blue also is very usefulin mixture dyeing : tlie initial red shade changes in thechrome hath to a drah, extremely fast to acids and alkalis,to milling, and to light. Acid Alizarin Brown, the latest"Acid Alizarin/, is said to give even better results than
Anthracene Brown.The Chrome Blacks " B " and " T " may he classed along
with the above dyestuffs, since they are also dyed anddeveloped in one bath. Acetic acid should, however,replace the sulphuric in dyeing, and an addition of sulphateof copper must be made to the bichronie in developing(See preceding abstract).
All the above dyestuffs being applied in one bath, anenormous saving in time, steam, and labour is effected;moreover, they easily dye level shades, and the goods maysafely be entered into the hot bath.
Special experiments have shown that the presence oflactic acid in the bath up to 6—7 per cent, has no injuriousaction on the fibre.
Eor " matching off," certain " acid " dyes not sensitiveto oxidation, and rendered faster by application eitherbefore or after the chrome mordant, are recommended.
Such are "Patent Blue A," the "Fast Acid', Blues andViolets, and the Salicylic Yellows.—J. A. P.
Patent Chrome Green « A," Purity of P. iMedlaender.tfarber-Zeit. 10, [22], 357.
T H E usual methods for the examination of dyestuffs forthe admixture of foreign dyestnffs are : - Sprinkling on
oist filter- or blotting-paper; on the surface of water;on cone, sulphuric acid, &c, and also by capillary analysisIn a recent dispute with regard to Patent Chrome Green, it
-ns demonstrated clearly that these tests are not absolutelyconclusive. The accusation against the manufacturers thatthe said Green was a mixed product, and contained a bluedyes'tuff, cannot be sustained, and the author gives thefollowing explanation of the apparently adverse resultsobtained bv the above tests.
Sprinkled on ordinary tap-water, which almost alwayscontains some lime or calcium compounds in solution, thepanicles, in sinking, form green streaks but at the bottom,colour the water immediately surrounding them reddish-brown. Moreover, after standing some time,blue streaksappear intermingled with the green ; thus the impression ofa mixture arises. Similarly an appearance of brown specks,which, however, are largely outnumbered by the green, isnoted when the dyestuff is blown lightly over moist blottingTviDer The formation of this brown or reddish-brown colourw due to a well-marked tendency on the part of this andalmost all « salicylic" azo dyestuffs for calcium salts, andin the case in point the tendency is so strong that if a hot(blue) solution be poured on to ordinary filter-paper-whichcon ains a trace of l ime-tins is clearly indicated by aredxus zone surrounding the blue, due to formation of[he nsoluble reddish-brown lime compound. With acid-extracted filter-paper, this reddish zone does not appear
The formation of the blue streaks depends on a lessgenerally known phenomenon. Under certain conditionsmany dvestuffs can be precipitated from their solutionsIn such a form that when filtered off, dried, and addedo cold water, their particles separate so minutely, and
admix so intimately with the water, as to appear in com-niete solution. Thus Benzidine + /3-naphthoi disulphonic acid,Sves m cold water an apparent solution of this kind,wMch has a blue colour, is quite transparent, and can befiltered • yet on boiling, the colour changes to a reddish-violet and only gradually resumes the blue tint on cooling.
The differences in the colours of the cold and hot« solutions " of « Diamond-Mack " and « -G reen/ though lessstriking are easily noted. The dyestuff in question possessesthe same peculiarity, its cold «solution" being green,whilst the genuine solution in hot water is blue; the latter,however, gradually develops from the green apparentsolution, on long standing, even in the cold; hence the
some of the green " solution" be allowed to drop slowlyinto distilled water (to avoid calcium salts), looking throughthe beaker, the streaks appear green; viewed from abovethey are brownish-red.
There is no such difference when this is repeated with theblue solution.
The change to red which so many blues undergo onironing, is probably attributable to a similar phenomenon.The above-mentioned affinity for lime need not detract fromthe value of capillary analysis for discovering mixtures,provided extracted filter-paper and solutions in distilledwater are always employed, under which conditions PatentChrome Green will be found to show, at most, fractions of aper cent, of a " foreign" colour (presumably a nionazoderivative of the " K acid"—amidonaphthol disulphonicacid).—J. A. P.
I.'d A,-Naphthalene Trisulphonic Acid. H. Erdmann.Ber. 32, [16], 3186—3191.
THE starting point for this acid is the 1. ^/-naphthalenedisulphonic acid obtained by sulphonating naphthalene ata low temperature and separating the sodium salt. Twokilos, of this salt are stirred into 3 kilos, of sulphuricacid monohydrate with good agitation, and cooled ex-ternally with ice so that the temperature of the meltdoes not exceed 50° C. 2*8 kilos, of fuming sulphuricacid (67 per cent. SO:i) are then run in below 50° C , andthe Avhole is finally heated for 3 | hours to 90° C. Themixture is then treated with 400 grms. of ice, and has aspecific gravity of 66° B. After liming, converting intothe sodium salt, and drying at 125° C , a weight of saltis obtained somewhat heavier than that originally startedwith. In order to obtain the free acid, the sodium suit isconverted into the chloride, recrystallised from acetic acid,boiled with spirit, diluted Avith water, and evaporated on thewater-bath. The free 1.3. ^-naphthalene trisulphonic acidhas little tendency to crystallise, and is very hygroscopic. Itpossesses the characteristics of the strongest non-volatile
inese v-uv*^* solutions seem to hold the dyestuffs inthe form of excessively minute crystals since they appeardifferent viewed by transmitted and reflected light Thiss particularly noticeable with Patent Chrome Green, H
mineral acids, carbonising filter-paper and decomposingsodium chloride with effervescence. The aniline, p-toluidme,benzidine, and dianisidine salts have been prepared. Theformation of the first-mentioned salt, C2 SH2 9O9N ; iS3, affordsa method for estimating the amount of 1 • 3. ^-naphthalenetrisulphonic acid present.—T. A. L.
<p-Amidoquinoline and some of its Derivatives.C. Knueppel. Amialen, 310, [1], 75—88.
TIIE ^-amidoquinoline referred to is obtained by reducingp-nitroquinoline in an alcoholic solution with finely groundiron in presence of calcium or magnesium chloride. Theaddition of a small quantity of animal charcoal considerablyfacilitates the reduction. Amongst the derivatives obtained,thio?iyl-p-amidoquinoline melts at 65° C. and crystallisesin sulphur-yellow needles ; p-amidoquinoline thionamic acidseparates as a canary-yellow crystalline powder from anhy-drous ether and melts at 124° C. In the preparation ofthionylamidoquinoline, by acting with thionyl chloride onamidoquinoline, the monohydrochloride of amicloquinoline isformed as a by-product. It can also be obtained by dis-solving a molecular proportion of the base in a strongaqueous solution of the dihydrochloride. On evaporation,the new salt separates out and can be recrystallised fromalcohol, forming golden-yellow needles melting at 109° C ,whilst the dihydrochloride is insoluble in alcohol and meltsat 250° C. Chlorocarbonic ether acts on amidoquinoline,forming γ-quinijlxirethane, Avhich crystallises in brownishplates melting at 168° C. By reacting with the theoreticalquantity of acetic anhydride on a solution of amidoquinoline
j in acetic acid, the author obtained jp-acetamidoquinoline,which crystallises from hot water in white needles meltingat 138° C. The substance possesses strong basic propertiesand gives well characterised salts. The action of benzoylchloride and soda lye yields benzoyl amidoquinoline, whilstthe reduction of the diazo compound with stannous chlorideforms p-quinylhydrazine, which combines with benzalde-hyde, yielding red crystals melting at 203° C , withpotassium cyanate, forming the semicarbazidc, melting at234° C , and with pyruvic acid, the corresponding hydrazonemelting at 189° C. The reduction of p-nitroquinolinc in*
THE JOURNAL OF THE SOCIETY OF OHEMIOAL INDUSTRY. [Jan. 3i,
alcoholic solution with powdered iron in presence of ametallic chloride yields long yellowish-red needles ofp-azoquinoline, melting at 248° C, whilst if reduced in amethyl alcoholic solution with sodium methylate, p-azoxy-diquinyl is obtained, probably some oxyazodiquinyl beingformed as a by-product. This latter is described as a greendyestuff soluble in soda-lye and crystallising from alcohol indark violet needles.—T. A. L.
Triazines from o-Amido-azo Co?npounds. M. Busch.Ber. 32, [15], 2959—2972.
TUB carbanilido-amido-azotoluene obtained by the action ofphenylcyanate on o-amido-azotoluene (Goldschmidt andKosell, Ber. 23, 501; this Journal, 1890, 494) does notyield an inner anhydride, whereas the author finds that thecorresponding derivative from phenylthiocyanate readilygives up sulphuretted hydrogen and condenses to a strongbase, the solutions of which are blue, those of its salts beingwine-red. The condensation products arc derivatives ofα-phentriazine—
CH
N
They are very stable on boiling in hydrochloric acid, aqueousor alcoholic solution, and are reduced by sulphurettedhydrogen, yielding colourless, readily oxidisable leuco pro-ducts. The reaction does not appear to be a general onefor all o-amido-azo compounds, since benzene-azo-£-naph-thylamine does not react with thiocyanates even at 120° C.The keto derivatives described by Goldschmidt and Kosellhave been obtained by the author by acting with phosgeneon o-amido-azo compounds. These keto derivatives arereadily decomposed by bases (alcoholic potash, aniline), theazine ring being broken and a urethane formed ; but evidencein favour of their not having an isocyanate constitution isafforded by the fact that the urethane of beuzene-azo-£-naphthylamine, when carefully treated with alcoholic potash,gives off alcohol and produces naphthophenylketotriazinein quantitative yield.
Thiocarbanilido-amido-azotoluene—
C7H7. NH. N: C7IIG: X. CS. NHC6H3
is obtained by reacting with equimolecular proportions ofo-amido-azo-toluene and phenylthiocyanate in alcoholicsolution. Crystallised from alcohol, the substance formsbrownish-yellow plates melting at 149° C. When boiled inacetic acid solution and neutralised with ammonia or sodalye, a precipitate of α-toluphenylimidotolyltriazine is obtainedhaving the formula—
H,CN
C:N.C f iH5
N.C6H4.CH3Q>)
The substance melts at 127°# 5 C, is readily soluble inbenzene, ether, and chloroform, less so in alcohol, and isinsoluble in water. It has very little tinctorial power, silkbeing dyed a reddish flesh-coloured shade, which appears tobe unaffected by light. The hydrochloride has the formula(C 2 1H l 8N 4) 2(HCl) 3 and melts at 98° C. On reduction withsulphuretted hydrogen in benzene solution, a colourlessnon-basic dihydrotriazine is formed, which melts at 141° C.The action of phosgene on o-amido-azotoluene yields thehydrochloride of α-tolutolylketotriazine, from which thebase, melting at 168° C.
, -
can be obtained by decomposition with ammonia, Ontreating the ketotriazine with alcoholic potash, it is con-verted into .the ethyl arethane of o-amido-azotoluene
-AC. N : C 7H 6 : N . N H . C7H7, orange - yellow needlesmelting at 94° C. This compound can also be obtaineddirectly by acting with chlorocarbonic ethyl ether ono-amido-azotoluene. On warming toluketotriazine withalcoholic ammonia, the carbamide of o-amido-azotoluene,H.NOC. N : C7HG: N. NHC 7H 7, is obtained, melting at 207° C.In a similar manner the carbanilide is formed by heatiugthe ketotriazine with aniline to 130° C. I t melts at 219° C ,and has already been described by Goldschmidt and Kosell.
Phosgene also acts on benzene-azo-£-naphthylamine,yielding naphthophenylketotriazine. This substance meltsat 255° C, and is decomposed by alcoholic potash. In orderto obtain the urethane, benzene-azo-/3-naphthylamine andehlorocarbonic ether were boiled together in benzene _ solu-tion. The product forms flat orange-red needles inciting at110° C, and when treated in alcohol in the cold withalcoholic potash, the solution deposits a mass of yellowneedles of naphthophenylketotriazine.—T. A. L.
Thiazine Dyestuffs, Ortho-A. G. Green. Ber. 32, [16],
WITH reference to Kehrmann's views (Ber. 32, 2601 ; thisJournal, 1899, 1115) the author states that he had alreadypointed out the analogy existing between the azonium,oxazine, and thiazine dyestuffs (Proc. Chem. Soc. 1892,195, and 1896, 226). Accepting the tetravalency of oxygenand sulphur, he is of opinion that the following formula?(I.) are more probable than those proposed by Kehrmann :—
1.
CI
C eH4 C e II, cGr-i,
II.
CI
N\ cj-r
K
CI
Azonium chloride,
CI
0
CI
Oxazine chloride.
C 6 H6 H 4 an, /
o
ci
6
o
an
Thiazine chloride.
since, although these do not agree with the present formulafor Safranine, they are more in harmony with the usuallyaccepted view of the greater basicity of nitrogen comparedwith oxygen or sulphur. It is, however, also possible thatthese substances have a double o-quinonoid structure, as in1L ; and Kehrmann's observation (Ber. 31, 977; this Journal,1898, 570) that certain azonium compounds could be sub-stituted by amines in both rings, lends support to this viewwhich also does not require the assumption that a trans-formation of the quinonoid linkages takes place. At anyrate, the proposed formulae well explain the formation of theSafranine and Kosiuduline compounds ; and, moreover theyrepresent the Eosindones, Safranones, and similar anhydridesas p-anhydro compounds, whilst Kehrmann's formukinvolves the assumption that they are ro-anhydrides.—T A l '
Brasilinand Hematoxylin.-Part III. A . W. Gilbodyand \\. H. Perkm, jun. Proc. Chem. Soc. 15, [216], 241., [],
IN a previous communication (this Journal, 1899,133), an acidobtained from brasilm was described which melted i t 1 Vi"and gave, on analysis, numbers agreeing with the formulaC15H16O6. h s acid, on oxidation with potassium perman-ganate, yielded a dibasic acid molting at 200°-203° whichwhen heated with hydrochloric acid at 160c,waS decomposedwith formation o i catechol. Further investigation1^ has
Jan.3i.ioou.] THE JOURNAL OF THE SOCIETY OF CHEMICAL INDUSTRY. 41
shown that this acid, which at first was thought to have theformula C10H10Oa(CO2H)o, is in reality metahemipinic acidy
CH3O COoH
Tetramethylhxmatoxylin, when oxidised with chromic acid,also yields considerable quantities of metahemipinic acid—aproof that hematoxylin, like brasilin, is a derivative ofcatechol. As this result did not agree with the statementof R. Meyer (Ber. 1379, 12, 1393) that hematoxylin, ondistillation, yields pyrogallol and resorcinol, this work wasrepeated, and it was found that the products of thedestructive distillation of hematoxylin contain considerablequantities of pyrogallol, but, as far as could be determined,no trace of resorcinol.
It follows, therefore, from these experiments, that whereasbrasilin is a derivative of resorcinol and catechol, hema-toxylin is a derivative of pyrogallol and catechol.
The formation of metahemipinic acid from both brasilinand hematoxylin shows that the formule suggested by theauthor for these substances require some modification.
It should be noticed that the melting point of tetramethyl-hematoxylone is incorrectly given as 170° in the previouscommunication; it should be " 183°—186° with vigorousdecomposition."
Luteolin [from Weld] — / / / . A. G. Perkin. Proc. Chem.Soc. 15, [216], 242—243.
PREVIOUS investigations (Trans. Chem. Soc. 1896, 69, 206,799 ; see also this Journal, 1896, 444) indicated that luteolin,C15II10OG, is a tetrahydroxyflavone. The energetic action ofalkali yielded phloroglucinol and prolocatechuic acid, con-firming liochleder's results (Zeits. fur Chem. 1866, 2, 602),and it is now found that, by gentler treatment, phloro-glucinol and a substance having the composition CSH8O^ areformed. The substance (colourless needles, melting point115°—116C C.) gives, with fused alkali, protocatechuic acid,and its properties are identical with those of acetylcatechol,CII ; j .CO.C 6II ; t(OH) 2 (Dzerzgowski, Jour, lluss. Chem. Soc.1893, 25, 157). This confirms the constitution assigned byThe author to luteolin—
(): OH
OH
;;CH
OH CO,
In conjunction with L. H. Horsfall, an investigation isin progress upon certain ethers of luteolin. By partialmethylation, a dimethyl ether, yielding colourless needles,melting point 227°—229° C, is formed in small quantity ;this is almost devoid of dyeing property, and by means ofalkali gives isovanillie acid. There is evidence that, inaddition to luteolin, weld contains a trace of a seconddyestuff.
PATENTS.Indigo Colouring Matters: The Manufacture of New Sul~
phonic Acids. G. B. Ellis, London. From La SocicteChimique des Usines du Rhone anc. Gilliard P. Monnetet Cartier, Lyons, France. Eng. Pat. 26,625, Dec. 16,1898.
ACCORDING to Eng. Pat. 25,634 of 1898 (this Journal, 1899,1117), the nitrotoluie aldehydes melting at 64° C. and 44° C ,on condensation with acetone in alkaline solution and treat-ment with alkali, yield Methyl-indigos. The patentees nowfind that these Indigos (designated by the melting points ofthe nitrotoluie aldehydes) yield mono- and disulphonicacids similar to natural Indigo. Indigo 64° is more readilysulphonatcd than indigo 44°, which requires a more con-centrated acid and a higher temperature. For the prepara-tion of a monosulphonic acid, 5 kilos, of indigo 64° arestirred for some time in 50 kilos, of 98 per cent, sulphuric
acid, and the mixture is then allowed to stand for 10 hoursat about 20° C. After dilution with 500 litres of water, theunaltered Indigo is filtered off, the filtrate precipitated withchalk or barium carbonate, treated with sodium carbonate,and the solution evaporated, or else the sulphonated Indigosodium salt is salted out. It forms a bronzy powder, anddyes wool and silk a very pure blue, whilst the product fromIndigo 44° dyes a more greenish shade. DisulphonatedIndigos are obtained by mixing 5 kilos, of Indigo 64° or 44°with 50 kilos, of fuming sulphuric acid (10 per cent. SO3)and heating the melt for some hours to 20°—30° C. until asample is completely soluble in water. The new dyestuff is thenseparated as already described. The disulphonated Indigos,more especially that from Indigo 44D, dye more greenishshades than the monosulphonated derivatives.—T. A. L.
Eosin and other Halogen Derivatives of the FluoresceinGroup; Preparation of G. B. Ellis, London. From LaSociete Chimique des Usines du Rhone anc, Gilliard P.Monnet et Cartier, Lyons, France. Eng. Pat. 3186, Feb.13, 1899.
T H E patentees make use of an electric current for thepreparation of Eosine from fluorescein. The conversion iseffected at the ordinary temperature, and is carried out inan alkaline carbonate solution, so that the formation ofby-products is avoided. For example, 1 kilo, of fluoresceinis dissolved in 30 litres of water containing 1 kilo, of sodiumcarbonate, and 1 kilo, of bromine is stirred in. The solutionis electrolysed in a vessel provided with diaphragms, thecathode being preferably an iron plate or iron gauzeimmersed in a dilute solution of sodium hydrate orcarbonate, and the anode preferably platinum gauze. Acurrent of 2—3 amperes per sq. dee. may be employed, andthe solution during the operation is kept suitably agitated.The shade obtained, varies according to the duration of theoperation, ranging from orange-yellow to bluish-red. Whenthe desired shade is obtained, the current is interrupted, andthe liquor is worked up for Eosine in the usual manner, anddoes not usually require any further purification.—T. A. L.
Aromatic Oxy aldehydes; Manufacture of T. It. Shillito,London. From J. R. Geigy and Co., Basle, Switzerland.Eng. Pat. 27,236, Dec. 24, 1898.
THE patentees in Eng. Pat. 17,135 of 1898 (this Journal,1899, 577) described a method for introducing the aldehydegroup into aromatic amines by treating them with form-aldehyde and an aromatic hydroxylamine or its sulphouicacid. They now find that the reaction may be applied tophenols of the benzene and naphthalene series and theirderivatives. It is, however, occasionally necessary toemploy other methods for separating the aldehydes, as thefollowing example will show :—A cold solution of 60 kilos,of sodium nitrobenzene sulphonate and 22 kilos, ofresorcinol in 800 litres of water is treated with 50 kilos,of iron filings, and then with 150 kilos, of hydrochloricacid (20° B.) mixed with 16 kilos, of formaldehyde (38 percent.). The solution is allowed to stand 24 hours, whenthe benzylidene compound is filtered off, dissolved 'in hotcaustic soda lye, rapidly filtered, and precipitated by addinglead acetate. The lead compound of the resorcylaldehydeforms a grey precipitate, which is filtered, well washed anddecomposed by wanning with a dilute acid. The reso'rcyl-aldehyde is purified by means of its bisulphite compoundand was found to melt at 134° C. Similarly, α-naphthol-aldehyde may be obtained by heating 15 kilos, of nitro-benzene and 45 kilos, of fuming sulphuric acid to 120°—130° C. until a sample is completely soluble in waterpouring the melt into 250 litres of water, mixing with8 kilos, of formaldehyde (38 per cent.), and running thewhole slowly into 1,000 litres of water containing 13 kilosof caustic soda lye (40° B.) and 14 kilos, of α-naphthol'together with 25 kilos, of iron filings. After 4—5 hours'when the solution is no longer acid to Congo-red paper andhas turned a deep yellow, sodium acetate is added, and thefiltered solution is diluted with a large quantity of waterboiled, and treated with hydrochloric acid, when α-naphthol'aldehyde separates as a crystalline precipitate, and afterpurification by means of its bisulphite compound, melts atIol u in a similar manner, Vanillin melting- at 80° Cmay be obtained from guaiacol.—T A. L.
42 rnHE JOUENAL OF THE SOCIETY OF CHEMICAL INDUSTRY- [Jan. a, woo.
Neio Colouring Matters [Red, Blacli] derived from Para-phenylene Diamine, for Dyeing Wool; Manufacture ofJ. Imray, London. From La Societe L. Durand,Huguenin et Cie., St. Eons, hH.h6ne, France.Pat. 1033, Jan. 16, 1899.
HITHERTO no disazo dye stuff for wool derived fromphenylene diamine has become of technical importance,owing to the feeble resistance to light of this class of dye-stuffs (Ger. Pat. 70,885). The patentees, however, findthat dyestuffs containing the tetrazo derivative of jp-pheny-lene diamine of industrial value, and very fast to light andfulling, are obtained when one of the components is ano-carboxylated phenol or naphthol and the other is asulphonic acid of a- or jS-naphthol or of dihydroxy-naphthalene. For example, 27 kilos, of p-amidobenzene-azosalicvlic acid are diazotised in the usual manner andrun into a solution of 30 kilos, of sodium 1.4-naphtholsulphonate kept alkaline with sodium carbonate. After24 hours the mixture is heated to 70° C, and the dyestuff issalted out, pressed, and dried. It dyes chrome-mordantedwool bluish-red, dissolves in water with a red, and inconcentrated sulphuric acid with a blue colour. If the1.4-naphthol sulphonic acid be replaced by 26 kilos, ofsodium 1. l'^-clihydroxynaphthalcne sulphonate; the re-sulting dyestuff gives black shades on chrome-mordantedwool.—T. A. L.
Black Disazo Colouring Matters, Manufacture of C. IXAbel, London. From The Actien Gesellschaft fxir AnilinFabrikation, lierlin, Germany. Eng. Pat. 2360, Feb. 2, 1899.
ACCORDING to Eng. Pat. 24,527 of 1897 (this Journal,1898,910) black disazo dyestuffs are obtained by combiningthe diazo compounds of ^-amidodiphenylaminc sulphonicacids with α-naphthylaniine, again diazotising, and thencombining with naphthols or naphthol sulphonic acids. Inthe present specification the patentees replace the p-amido-diphenylamine sulphonic acids and their homologucs byother substitution products of these acids, or they employcertain sulphonic acids derived from p -amidophenyl-jB-naphthvlamine. These products are obtained bv reactingwith p-nitrochlorobenzene-o-sulphonie acid on o-, p-, or7rt-chloraniline, acet-p-phenylenediamine, m-amido-^-cresolether, and β-naphthylamine or its sulphonic acids, andreducing the condensation products formed. The operationsfor obtaining the dyestuffs are carried out according to themethods already given in the above-mentioned specification.
—T. A. L.
Substantive Black Colouring Matters, Manufacture ojNew. J. Ira ray, London. From La Societe Anonymedes Matieres Colorantes et Produits Chimiques de St.Denis, Paris, France. Eng. Pat. 3576, Feb. 17, 1899.
INSTEAD of heating up yith sulphur or sulphur and sodiumsulphide, hydroxylated, amidohydroxylated, polyamido, &c.aromatic compounds, the patentees employ mixtures ofthese compounds of different natures, the resulting productspossessing material advantages over those derived from onecompound only. For example, 1 kilo, of p-amidophenol,1*2 kilos, of α-naphthol, and 3 kilos, of sulphur are heatedto 200° C. for three hours in an iron pan. After cooling8 kilos, of crystallised sodium sulphide are added, and thewhole is gradually raised to 180°—200° C, and maintainedat this temperature for 3—4 hours. The product dissolvesin alkalis or alkali sulphides, and dyes a clearer blackthan the dyestuff derived from p-amidophenol treated byitself, whilst α-naphthol, as is known, only gives a weakbrown dyestuff. Other mixtures which have been similarlytreated, are jp-amidophenol and o-nitraniline or o-phenylene-diamine, o-amidophenol and p-phenylenediamine, p-amido-phenol and triamidobenzene, or p-phenylenediamine and adiamidophenol.—T. A. L,
New Anthraquinone Derivatives, Manufacture or Produc-tion of H. E. Xewton, London. From The Farben-fabriken vormals F. Bayer and Co., Elberfeld, GermanyEng. Pat. 256, Jan. 5, 1899.
Ix Eng. Pat. 12,011 of 1897 (this Journal, 1898, 572) thepatentees describe the production of ii^ulphonic acids ofA nth ra rutin and Chrysazin. According to the presentspecification, on heating thuse acids with caustic alkalis they
are converted into new trihydroxyanthraquinone mono-sulphonic acids, which, on further heating with causticalkalis, yield tetraliydroxyanthraquinones, and these onoxidation can be converted into hexahydroxyanthraquinones.For the formation of a trihydroxyanthraquinone sulphonicacid, a solution of 5 kilos, of anthrarufine sodium disul-phonate and 25 kilos, of potassium hydroxide in 25 litres ofwater is heated to 180°—210° C- until the melt suddenlythickens. It is then allowed to cool, and treated with dilutehydrochloric acid, when the acid potassium salt of oxyanthra-rufin (trihydroxyanthraquinone) sulphonic acid separatesas a crystalline precipitate. The pure acid, which crystallisesin golden-yellow crystals from hot weak acid water, dissolvesin sulphuric acid with a red colour, which turns greenish-blue on adding boric acid. It dissolves in alkalis with ablue colour, and gives blue shades on chrome-mordantedand violet-red shades on alumina-mordanted AVOOL By thefurther action of caustic alkalis at higher temperatures, thetrihydroxyanthraquinones are converted into tetrahydroxy-anthraquinones, but it is preferable to obtain them directlyfrom the Anthrarufin or Chrysazin disulphonic acids. Asolution of 5 kilos, of potassium Chrysazin disulphonateand 30 kilos, of potassium hydroxide in 30 litres of wateris heated at 210°—280° C. until a sample dissolves in waterwith a blue colour. After cooling and diluting with water,the free 1.2. l/.2/-tetrahydroxyanthraquinone is precipitatedin orange flakes by adding an excess of dilute hydrochloricacid. It can be purified by recrystallisation from glacialacetic acid, and dissolves in concentrated sulphuric acid witha violet-red colour, which turns blue on adding boric acid.The solutions in sodium carbonate and ammonia are violetand in caustic soda lye blue. The new tetrahydroxyanthra-quinone dyes chrome-mordanted wool crimson and gives redshades on alumina-mordanted wool.—T. A. L.
Anthraquinone Derivatives • Manufacture or Production ofNew. H. E. Newton, London. From The Farbenfabrikenvormals F. Bayer and Co., Elberfeld, Germany. Eno-Pat. 1884, Jan. 26, 1899. **
THIS is an application of the method described in EnffPat. 12,011 of 1897 (this Journal, 1898,572) to 1.2'-di-hydroxyanthraquinone, yielding a diamidodisulphonic acidof 1.2Vlihydroxyanthraquinone. The product dyes woolfrom an acid bath level violet shades, and gives blue shadeson chrome-mordanted wool. A solution of 20 kilos, of1.2'-dihydroxy anthraquinone in 80 kilos, of fuming sul-phuric acid (20 per cent. SO3) is heated at 90°—100° C.until a sample is completely soluble in water. The melt iscooled and^mixed with 120 kilos, of sulphuric acid (66° R ) ,and 25-5 litres of a mixture of nitric and sulphuric acids(containing 0*2 kilo, of nitric acid per litre) are added atabout 25° C. The nitration takes about 4—5 hours, whenthe melt is poured on to ice, and the potassium salt of thedinitro-l^'-dihydroxyanthraquinone disulphonic acid isprecipitated with potassium chloride. This forms a yellowpowder soluble in concentrated sulphuric acid and in waterwith a yellow colour. It dyes wool yellow from an acidbath, andmay be reduced on the fibre. In order to obtainthe diamido compound, a solution of 5 kilos, of the above-described potassium salt in 200 litres of water is mixedwith a solution containing 13 kilos, of stannous chloride30 litres of water, and 30 litres of hydrochloric acid (33 percent. HC1). The reduction takes place immediately and iscompleted by heating to 5O°-8OD C. The dyestuff separatesas a dark powder, which dissolves with a red colour in waterAvhilst dilute alkalis dissolve it with a blue colour. T A i/
V.-TEXTILES: COTTON, WOOL, SILK, Etc.PATENTS.
Vicuna, Camel-Hair, and Alpaca Fibres, MicroscopicAppearance of. K. M. Prideaux.
See page 8.
Vegetable Fibres for the Manufacture of Cellulose, or forSpinning or other Purposes, Treatment of. A. Bouret
i 7 o T ^ r * ' V e r b i 0 S C ' S^^-Etienne; Lille. SPat. 24,768, Nov. 23, 1898. fe*FLAX, hemp, jute, or other vegetable fibre is first subiectedto a retting process by boiling in a sodium carbonate bath
Jan. 31, woo.] t THE JOUBNAL OF THE SOCIETY OF CHEMICAL INDUSTRY. 43
If the fibre has had a preliminary treatment, 5 kilos, percubie metre is a sufficiently strong solution.
Eor raw fibre a much stronger solution is necessary. Thematerial (fibre) is now passed by an endless apron throughsqueezing rollers to another vessel, which is closed. It ishere,boiled in water, and carbonic acid is passed into theboiling liquid. This effects the solution of the resinousgummy matter.
It is now thoroughly washed by passing through a vatof hot water between endless aprons, which are arrangedso that they travel between several rollers.
This washing is repeated several times. If the materialthus produced be intended for spinning, it is now passed intoa tex>id bath containing 1 part of glycerin to 500 parts ofwater, from which it is wrung out and dried.
If intended for the manufacture of cellulose, the materialis then bleached, washed- and dried in the usual way.
Wool and other Animal Fibres, Process and Apparatus forCleaning and otherwise Treating. E. Maertens, Provi-dence, Rhode Island, U.S.A. Eng. Pat. 14,232, July 10,1899.
RAW wool is placed in a digester, and, a vacuum havingbeen produced in the latter, solvent material is allowed torun in, and the steam coils round the digester are set inoperation. After digestion for a suitable time, the solventis volatilised off and passes through a condenser into areservoir. The digester is rinsed out several times withpure solvent till quite dry and inodorous. The temperatureof the wool in the digester should not rise above 60° C. orthe ^ool may be injured.
Tim residual solvent in the digester mav also be removedby steam or air.—C. M.
Treating Yarns with Mercerising or other Liquids, Appa-ratus for. P. S. Holland, Birch Vale, and J. J, Jackson,New Mills, Derby. Eng. Pat. 2211, Jan. 31, 1899.
THE machine consists of two standards bolted together andhollowed so that two beams stretching from one standard tothe other can be raised or lowered at will by means ofbevelled gearing and screws.
On each side of the beams, spindles are journalled, thoseof the top corresponding to those of the bottom. Thewhole of the spindles are geared together by spur wheels.Hanks of yarn are placed over the top and bottom spindles,the lower spindles being supported by the yarn. Thesecan be weighted, if desired, so as to give increased tensionin the hanks. In operation, the two beams are raised, anda trough containing the mercerising or other liquid is placedbeneath; the beams are now lowered until the bottom one,with its spindles, is immersed in the liquor. The spindles arenow made to rotate slowly. When sufficiently treated, thebeams are raised, the trough removed, and one containingwater or other liquid substituted. The whole operation isthen repeated until the hanks are sufficiently washed.—C. M.
Yarns, Apparatus for Treating, tvith Liquids. T. liold,Swinton, near Manchester. Eng. Pat. 4170, Feb. 25,1899.
Two series of rollers in vertical planes are arrangedradially at the ends of a shaft placed above a tank whichcontains the liquid. These radial rollers have bevelledtoothed wheels at their ends, and, as the main shaft, onwhich they are journalled, rotates, the bevelled toothedwheels are made to come in contact with a fixed bevelledwheel, thus giving each radial roller a rotation on its ownaxis, as well as the movement given to it by the motion ofthe main shaft.
The latter is made extensible by a sleeve placed on itbetween the two series of radial rollers. Yarn is stretchedfrom one series to the other, and if the tank be filled with,say, a mercerising liquid, then as each radial roller entersthe liquid, the roller with its yarn is rotated, thus ensuringall portions of the hank coming into contact with theliquid.
The desired tension is maintained by regulating thesleeve on the main shaft.—C. M.
Yarn, Machinewj for Washing, Impregnating, Stretching,and Drying; Specially Applicable for carrying out theMercerising Process. A. Romer and E. Holken, Bar-men, Germany. Eng. Pat. 16,782, Aug. 18, 1899.
T H E patentee claims a machine in which the processes ofwashing, impregnating, squeezing, stretching, and dryingyarn may be performed without tbe yarn being removedfrom the two rollers over which it was originally placed.
One roller is kept stationary, and the other movable bymeans of a lever along which a weight travels so that thepressure may be varied to any desired extent. Arrange-ments are also made whereby the tanks, in which thevarious liquids are placed, are fixed on an endless chainand can be moved into place when desired.—C. M.
Mercerising Cotton Previous to Weaving, Process for.E. Brandts, Munchen-Gladbach., Germany. Eng, Pat.19,936, Oct. 4, 1899.
THIS process relates to the mercerising of cotton undertension, after spinning, and previous to weaving* Thecotton is tightly wound on to bobbins, and the spools thensaturated with soda lye. They are then neutralised withacid and afterwards subjected to a centrifugal action, beingrotated rapidly on their own axes. It is advisable to keepa continuous stream of water playing on the cotton duringthe latter operation.
(See also this Journal, 1898, 149, 240, 345, 452, 573, 756,840, and 1141; 1899, 36, 136, 267, 490, 680, and 911.)
—C. M.
Floor Cloth and Method of Manufacturing the same.F. Gatzsch, Freiberg, Saxony. Eng. Pat. 25,757, Dec. 6,1898.
A SUITABLE felted webbing or fabric is immersed in thefollowing mixture until thoroughly impregnated :—
Water, 7 galls. ; glue, 1 lb. ; w a x , \ \ h . ; lead ochre, ^lb. ;linseed oil, \ lb.; tungstic acid, 1 oz. This mixture is marieat a temperature of about 80° C. Ordinary ochre may beadded to it to give colour.
After impregnation, the cloth is passed through rollersand then taken to the printing machines, where any designmay be printed on.—C. M.
Incombustible Floor-Cloth, Manufacture of J. Snowdon,Milwall. Eng. Pat. 27,606, Dec. 31, 1898.
A FABRIC is woven of asbestos, or canvas rendered incom-bustible by treatment with salts such as ammonium sul-phate, or calcium ammonium sulphate. This "backing ' ,
is then faced with a mixture such as the following :—China clay, 2 lb.; asbestos powder, 2 lb.; cork dust, 1 lb.;
ammonium sulphate, 1 lb.; ochre, 1 lb.; linoleum cement,2~ lb. The quantity of ammonium salt is varied with thequantity of linoleum cement and cork dust present, bein<rincreased as these are increased.—C. M.
VI.-DYEING, CALICO PRINTING, PAPERSTAINING, AND BLEACHING.
Cachou de Laval, Employment of in Dyeing. LeipzigFarber- u. Zeugdr.-Zeit. 1899, 48 , [12], 496—497. *'
CACHOU de Laval (syn. Sulphin, " MercaptofarbstofE")dyes on cotton a dark green colour which changes to abrownish-grey on exposure to air. It is rendered fasterby treatment Avith potassium bichromate or permanganatecopper sulphate, ferric chloride, and various other salts'The first of these renders the shade paler; the secondgives a dark bronze, manganese dioxide being at the sametime deposited upon the fibre ; the third yields a pure greyThe colours produced by means of salts which are withoutoxidising action resemble one another. The colours thusformed by after-treatment with metallic salts are fast toacids, but arc slightly attacked by a boiling solution of sodaat 1 —2 B., and by a cold solution of bleaching powderat 1 B. They are not appreciably affected by a month'sexposure to light. Hydrogen peroxide, in the presence ofalkalis, destroys them.
That the employment of Cachou de Laval is limited ischiefly owing to the existence of a large number of coin'paratively cheap dyestuffs, with which the shades given
THE JOURNAL OF THE SOCIETY OF CHEMICAL INDUSTRY. [Jan. si,woo.
by that dyestuff may readily be obtained, but it is partlydue to the fact that the dyestuff does not keep well, beingdecomposed by damp air.
The dyestuff is of no interest in wool dyeing.—E. B.
Mordanting Cotton with Chrome. Leipziger Fiirber- u.Zeugdr.-Zeit. 1899,48, [12], 483.
WHEN cotton is mordanted with chrome, by the process ofimpregnation Avith a solution of " chromium bisulphite,',
followed by drying and steaming, the mordant is unevenlydeposited, the fibre is attacked by the liberated sulphurdioxide, and the mordanted fibre, owing to its resistance tomoistening with Avater, is apt to become irregularly dyed.The Hadischc Aniliu und Soda Fabrik find (French Patent,283,47 7) that these drawbacks are not met Avith Avhen thecotton, after first being thoroughly moistened Avith Avater,is steeped for 12 hours in a solution of "chromium bisul-phite " and is then hydro-extracted and immersed for 10—15 minutes in a solution of 3 grins, of sodium carbonate perlitre at a temperature of 60° C. The cotton is afterwardswashed, hydro-extracted, and padded in a solution ofTurkey-red oil (1 : 10) and dried. The concentration of themordanting solution is 3°—10° 13., according to the intensityof the shade subsequently to be dyed. The method isapplicable to cotton in the manufactured and unmanu-factured states, as well as to linen, jute, and hemp. Sodiumphosphate and other alkali salts may be used in place ofsodium carbonate for the purpose of fixing the mordant,but the " chromium bisulphite" cannot be replaced bychrome alum or other chromium salts.—E. B.
Yarn Printing. B. Marquardt. Farber-Zeit. 10, [24],397—398.
L.VI'BKR (Zeits. f. d. gesam. Textil-Ind. 31, 32 and 33)recommends Paranitraniline Red for yarn printing, as hefinds that Alizarin Red gives unsatisfactory Avhites. Theauthor objects to the use of Paranitraniline Red, as theyarn prepared with naphthol does not stand the combingprocess so well as oiled yarn, and is therefore liable togive rise to uneven and faulty printing. Another objectionis the necessity of protecting the prepared yarn frommoisture, for should it become wet, mere drying, as in theease of oiled yarn, is not sufficient to preArent the formationof streaks and stains. Moreover, the alizarin printing colour,if sufficiently acid, nun be kept for scAreral days, whilst Avithparanitraniline or even nitrazol this is not possible.
In Austria, yarn printing in blue is almost entirely donewith Alizarin Blue; its application is very simple, com-prising but three operations, viz., printing, steaming, andwashing. Methylene Blue is occasionally used. Forprinting in brown, Limber recommends a mixture oflogwood extract, Persian-berry extract and Alizarin. Apartfrom cost, the author fails to understand Lauber's objectionto the use of cutch, fixed Avith copper sulphate. Forprinting in black Noir reduit is a serviceable colour,especially in combination Avith steam colours. As a singlecolour it is too expensive especially if fastness to acids bedesired. Aniline Black undoubtedly forms the best black.
—I). B.Discharge for [Triphenylme thane] Dyestuffs on Silk.
Leipzig. Fiirber-u. Zeugdr.-Zeit. 1899, 48, [12], r>02.AMMONIUM sulphite acts as a discharge for Malachite(Jiven, Acid Magenta, Corallin and analogous dyes uponsilk and union silk fabrics. The destruction of colourtakes place on drying the printed fabrics, the unchangedsalt being volatilised and the tenacity of the fibres not beingimpaired. As no steaming or washing is necessary, theprocess is suitable for fabrics Avhich are injured by thoseoperations [Bonnet, Ramel, Savigny, Giraud and MarnasFrench Patent 289, 49U].—E. K
PATENTS.Preparing and Dyeing of Tops, Stubbing, Wool, Yarns
Silk, Mohairj Alpaca, Jute, or any other Textile FabricsImpts. in the. J. Rhodes, Bradford. Eng. Pat. 25 823*Dec. 7, 1898. ' ' '
A PERFORATED or open-Avork cage is placed inside a dye-tank leaving narrow spaces on tAvo opposite sides. At thebottom of the cavities thus formed, is fixed a steam-pipe
perforated above. The cage is provided at a certain heightwith a false bottom, consisting of cross bars covered withcanvas upon Avhich the materials to be dyed are placed,being afterwards covered with another layer of canvae.Dye-liquor is introduced into the tank, to the level ot thefalse bottom ; any excess of this is removed by means of anoverflow pipe, the object being to prevent the exertion ot" back pressure " upon the flow of liquor, when the machineis in operation. The tank is covered with a lid whilst thedyeing is proceeding. The steam which is passed into theside spaces, heats the dye-liquor and forces it up overinwardly curved rims on the sides of the tank upon thematerials in the cage. At the same time a partial vacuumis produced underneath the cage and the liquor is caused toflow back more rapidly. To ensure uniform distribution ofthe liquor, "check-guards," consisting of hinged doors, arefitted below the false bottom of the cage. These are openedand closed as required, causing the liquor to traverse thomaterials in a more or less lateral direction.—E. 13.
Decolorising Dyed Fibrous Materials; Process of com-pletely. F . II. Oldroyd, ISTiedergorpc, Germany. Eng.Pat. 16,301, Aug. 10, 1899.
TUP: materials to be decolorised, " after being suitablyreduced" are boiled for 15—20 minutes in a dilute solutionof alkali, soap, or borax. After this they are washed andtreated in a hot bath Avith sodium bisulphite and zincpowder, " until the last residues of dye adhering to the fibreare removed.,,—E. B.
Centrifugal Dyeing Machinery or Apparatus. O. Gruhne,Gorlitz, Germany. Eng. Pat. 21,090, Oct. 21, 1899.
T H E materials to be dyed are packed round a perforatedcylinder, Avhich forms an inner chamber in a horizontallydriven centrifugal machine. An air-tight cover is thenplaced over the machine, which, by means of a pump, isput into communication Avith a dye-vat. The dye-liquor isforced through the materials from the top, passing throughthe inner chamber, and thence through a pipe to the vat.After a time, the action of the pump is reversed, and theliquor is made to flow in the opposite direction. When thishas been done for a sufficient length of time, the pump isstopped, the excess of liquor floAving back to the vat Thecage of the centrifugal machine is then set in motion. Moreliquor is thus expelled, and this also passes back to the vat.Finally, air is admitted, and driven by the centrifugal actionthrough the materials, thus completing the dyefno- whenair-oxidation is required. °
Considerable economy is effected, it is stated, in dyeingwool with Indigo, by the use of this machine. The savingin dyestuff amounts to \2\ per cent. Sodium hydrosulphite,steam, water, and labour, are also saved.—E. B.
Dyeing Yarns, Machines for use in. L. Weldon, Amsterdam,Montgomery, U.S.A. Eng. Pat. 21,189, Oct. 27, 1899.
THK object of this invention is to provide mechanism bymeans of Avhich, in the dyeing of woollen and worstedyarns, violent ebullition may be prevented from takingplace, and by Avhich the distance between the yarn-stickbearings in circular frames in reel dyeing machines may bereadily altered.
A dye-vessel Avith curved sides and bottom, has a curvedpartition fixed near one side, and extending almost fromtop to bottom, underneath which, near the bottom, is a per-forated steam pipe with its perforations pointing downwards.Above the vessel a reel is placed, carry in o- two sets ofrevolvable bearings for the reception of the yarn sticksupon Avhich the skeins of yarn to be dyed are put Motionis imparted to the inner set of bearings as the reel isrevolved Mechanism is also provided for adjusting thedistance between the two sets of bearings, and for kcemnerthese in position after the skeins have been placed on thSyarn sticks and have been made sufficiently tight.—E.
TZtl^faniC8PT°rr Sisi?9' Dudn^ S<™ri»9> Filling,or the like; Treating. C. Smith, W. Smith, and JHodkmson Todmorden, Lancashire ; and J. C. ChorlcyUewsey, Warnngton. Eng. Pat. 1974, Jan. 28,1899.
TEXTILE fabrics, to undergo either of the above treatmentsare previously passed round a drum heated by steam!
Jan. 3i,woo.] THE JOURNAL OF THE SOOIETt OF OHEMIOAL INDUSTRY.
The drum is placed as near as possible to the bath, so thatthe cloth enters the latter warm. It is claimed that in thisway, the fibres expand and open freely in all directions, andenter the bath in a better condition for the varioustreatments than when cold.—C. M.
YII.-ACIDS, ALKALIS, AND SALTS.Chromic Acid from Materials containing Chromic Oxide ;
The Regeneration of. E. Eegelsberger. Zeits. f. angew.Chem. 1899 [47], 1123—1128.
T H E author refers briefly to some of the numerous methodswhich have been proposed for utilising waste products con-taining chromium. Electrolytic processes appear to effectthe desired conversion to chromic acid or bichromate in themost economical way, and the author enlarges on somerecently proposed methods by the light of his own work inthe same direction. Regeneration of chromium solutionsby electrolysis, divides itself naturally into two main lines,which the author designates as " oxidation in alkalinesolution " and " oxidation in acid solution/'
1. Oxidation in Alkaline Solution.—By the action ofhypochlorites or of chlorine gas in presence of alkalis, theoxides of chromium are converted almost completely intobichromate, but the same end is attained in one operationby electrolysis, provided that an alkaline chloride be presentin the solution, an alkaline sulphate for instance not servingthe purpose. It appears that electrolysis in this case reallyacts indirectly, by producing a hypochlorite, which at onceoxidises the chromic oxide to bichromate, and the re-formedchloride serves again for the electrolysis. The yield ofchromic acid is not quite equivalent to the current used, butis highest when the solution contains a chromic salt, muchlower when the chromium is present as hydrate, and stilllower when frae alkali is present. It is noticeable that nodiaphragm is necessary in the electrolytic cell, which mayhe a box lined with metal to serve as cathode, whilst ananode formed of woven platinum wire is suspended in theelectrolyte. The best results cited gave a yield of chromicacid equivalent to 80—88 per cent, of the current used.This method might form an advantageous after-treatmentof the product obtained, by calcining chromic oxide andlime, but it has the disadvantage of requiring the costlyplatinum anodes, and the solution must be free from organicmatter, which would use up current unprofitably.
2. Oxidation in Acid Solution.—This method possessesseveral advantages over the foregoing, and is said to be insuccessful operation on a large scale. Instead of platinum,the anodes may be formed of lead, and it is in fact theperoxide of lead formed by the current on the anode surfacewhich takes the place of the hypochlorite as the intermediateao-ent in the oxidation of chromic oxide to chromic acid.There is an advantage in working without a diaphragm, asany local accumulation of free acid or alkali is avoided,and by working with hot solutions an economy of currenttension is obtained, as well as an apparently higher yield ofproduct. The apparatus is therefore of very simple con-struction, a lead lined box sufficing as electrolytic cell andthe concentration of the electrolyte may be equivalent to100 grms. of O 2 0 3 per litre. The author reckons that thecost of regeneration of 100 kilos, of Na2Cr207 by this processwill not exceed 20 marks. It may serve for the profitableworking up of many waste liquors and may influence theuse of chromic acid batteries.—G. H. B.
THE processes for the electrolysis of alkali chlorides in whichcement diaphragms are employed, are extensively appliedat the present time, but they have three faults, viz.: —(1) the relatively low current density attainable, (2) thatthe percentage of caustic in the cathode chamber cannotbecome high without a considerable decrease of efficiencyensuing, (3) that pure solutions of caustic are not obtained.The processes in which molten lead and zinc are employedas cathodes cannot be practically used on a large scale.
The early processes in which mercury was used as thecathode were likewise unsuccessful. But the improvements
introduced by Kellner, Gastner and others, made it possibleto use high current densities, and obtain solutions of causticof 20 per cent, strength free from the electrolyte and prac-tically pure. The amalgam of the alkali-metal, however,did not decompose at the same rate as it was formed, andthe loss of mercury was very considerable. Kellner over-came the difficulty by employing a third electrode andthereby securing decomposition of the amalgam at the samerate at which it was formed, whilst the hydrogen wasliberated at the secondary electrode in place of at the
• mercury. Loss of mercury with the evolved hydrogen wasthus avoided. This process has worked satisfactorily onthe industrial scale.
In England the Castner-Kellner Co. obtain yields of90 per cent. The loss arises chiefly from recombination ofthe chlorine with the sodium of the amalgam. Solvay andCo. of Brussels, working under Kellner's patents, useCastner's patent graphitic anodes, which are more durablethan the ordinary carbon anodes. Extensive industrialapplication has proved that the use of mercury as thecathode in the production of caustic and chlorine is superiorto all other methods.—J. A. B.
Hydrochloric Acidy Electrolysis of D. Tommasi,Elect. Rev. 1899, 45 , 469—470.
ON submitting hydrochloric acid to electrolysis with currentsat l#02, 1*42, and 2*04 volts, it was observed that theplatinum anode is dissolved only in acid of density 1-2.With diluted acids, oxides of chlorine were formed.—A. S.
Potassium Chlorate, The Explosion of I). Berthelot.Comptes rend. 129, [23], 926—929.
THOUGH potassium chlorate is an endothermic compound, itcannot be detonated by simply heating, but decomposesquietly, though with increasing rapidity in proportion asthe temperature of the mass is raised by the heat evolvedduring the decomposition. If, however, a little ball, gatheredon the end of a thin glass rod by dipping it several timesinto fused potassium chlorate, when at a temperaturejust above its solidifying point, be brought within 20 mm*of the bottom of an empty tube of hard glass which hasbeen raised to a bright red heat by a large gas-flame, theneach drop of the chlorate on the end of the rod, as it ismelted by the heat of the enclosure and falls upon thebottom of the tube, explodes with distinct detonation, andproduction of white clouds of potassium chloride- Referringto the late explosion at St. Helens, the author points outthat the conditions of his experiment might be realised onthe large scale in the case of the walls of a chamber whichhave become heated by a fire to a temperature far abovethat needed to decompose potassium chlorate, and intowhich chamber the chlorate is introduced in quantitiesinsufficient to sensibly reduce its temperature. Picric acidoffers another instance of the same phenomenon, as doesalso dynamite, a small amount of which burns away quietlywhen a light is applied, whilst a larger quantity, especially ifheated to start with, detonates.—J. T. D.
Fluorperborates. P. Melikoff and S. LordkipanidzeBer. 32, [17], 3349—3351.
HITHERTO no salt-like compounds have been preparedfrom perboric acid, H 0 . B : 0 2 , by replacing the H of the-OH group by a metal peroxide, MO or MOo, though suchbodies have been given by the other per-acids examined(this Journal, 1898, 579, 1194). The authors have pre-pared such salt-like compounds from fluorine derivatives ofperboric acid.
Potassium fluorborate, B2O3.2KFl,was dissolved in waterhydrogen peroxide solution and a few drops of KOH solutionwere added, and then alcohol. A gelatinous precipitatewhich assumed a crystalline form on trituration, was pro'duced; it was washed with alcohol and ether, dissolved inwater, reprecipitated with H2O2, KOH, and alcohol andagain rubbed to a powder. Analysis showed its compositionto be K4B4F14OU + H2O ; its structural formula represents 'it as the potassium salt of fluorpyroperboric acid, the H ofwhich has been replaced by the peroxide radicle KO Itdissolves readily in water; the solution, which has analkaline reaction, gives off oxygen energetically on warmin * .
46 THE JOURNAL OF THE SOCIETY OF CHEMICAL INDUSTRY. [Jan. 31,1000.
at ordinary temperatures the decomposition is very slow.With dilute sulphuric acid, Ho02 is formed ; from the drysalt concentrated sulphuric acid liberates ozonised oxygen.The dry salt is fairly stable. With Ag]SrO3 a yellow pre-cipitate of the silver salt is produced, decomposing withliberation of oxygen and metallic silver.
The same potassium fluorperborate was obtained frompotassium ortho-fluorborate (KO)oBFl (prepared by meltingtogether BX>3.2KF1 and KoCO.^ by dissolving the moltenmass in water, adding 4 molecules of H2O2 and precipi-tating with alcohol, when the above-mentioned stickyprecipitate was obtained, passing into the granular form ontrituration,—H. B.
Potassium Ferroeyanide and Sulphuric Acid; The Reactionbetween. R. H. Adie and K. C. Browning. Proc. Chem.Soc. 1899, 15, [215], 226.
THE authors have made a quantitative investigation of theaction of sulphuric acid of concentrations represented bycompositions varying between HoSOj (98 per cent.) andH2SO4, 8H2O, on potassium ferroeyanide with the followingresults.
Formation of Ilydroferrocy attic Acid. — The saltdissolves in acid of strengths corresponding to EUSO4 andHoS04,ILO, with the formation of potassium sulphate andhydroferrocyanic acid ; there is only a slow and incompleteformation of carbon monoxide.
Formation of Carbonic Oxide.—In acid of the strengthrepresented by H2SO4, 2H2O, the decomposition of the saltresults in the formation of carbon monoxide ; this reactionaccounts for all the cyanogen in the salt.
Formation of Hydrocyanic Acid and EveritVs Salt.—With more dilute acid of the composition of from H2SO4,4H2O to H2SO4, 10H2O, the products are hydrocyanicacid and Everitt's salt, KoFeoCyfl. At the latter dilution,all the cyanogen in the salt appears as hydrocyanic acid,while the formation of carbon monoxide practically ceaseswith acid of H.>SO4,4H2O strength.
The authors discuss the mechanism of the reaction (i)through the formation and hydrolysis of hydroferrocyanicacid by means of the dilute sulphuric acid ; (ii) through theaction of the potassium sulphate first formed, on thehydroferrocyanic acid, with the intermediate formation ofEveritt's salt. The latter reaction only takes place infairly concentrated solutions, whilst the former alone occurswith acids more dilute than that represented by H2SO4,lOHoO. Other conditions influencing the reactions are alsofully discussed.
The Reactions of Mg, Z?it and Fe, ivith Solutions ofCuSO4. R. M. Caveii.
See page 18.Carbon Dioxide from Fermentation, Collection of.
Washing Pyrites, Coal, and other Minerals, Apparatus forCleaning or. C. Burnett, Durham, and H. T. Newbigin,Newcastle. Eng. Pat. 25,852, Dec. 7, 1898.
See under I., page 30.
Drying Bricks, Earthenware, Cement, Slurry* and thelike before Burning, or for Drying Salt, Whiting, andthe like. W. Allison and J. English, both of Birtley,Durham. Eng. Pat. 19,192, Sept. 23, 1899.
See under IX., page 50.
PATENTS.Roasting Furnaces, more especially intended for Roasting
Pyrites or the like, for the Direct Production of SulphuricAnhydride from the Gases evolved. G. W. Johnson,London. From The Verein Chemischer Fabriken ofMannheim, Germany. Eng. Pat. 1859, Jan. 26, 1899.
THE pyrites to be roasted is contained in air-tight chambers,to which air, dried by passage through sulphuric acid dryingtowers, is admitted. Other close chambers contain contactmaterial, such as spent ore, through which the roastergases are drawn at a red heat, and transformed into sul-phuric anhydride, which is conducted for absorption toconcentrated sulphuric acid. The chambers containing the
contact material have revolving grates, by which it may beremoved when spent. The apparatus generally is armouredby iron plates and provided with charging and otherdevices so as to exclude all air except that which isdesiccated as described. Two varieties of furnace areshown.—E. S.
Sulphuric Anhydride, Manufacture of G. W. Johnson,London. From The Verein Chemischer Fabriken ofMannheim, Germany. Eng. Pat. 3185, Feb. 13, 1899.
THIS invention is an improvement on Eng. Pat. 1859;(see preceding abstract). The furnace is similar to thatthere described, except that more air is supplied to theroaster gases, and consequently more heat also. The roastergases, assumed to contain normally from 6 to 8 per cent, byvolume of sulphurous acid, are to be diluted with desiccatedair, either when in the reaction chamber or before enteringit, so as to produce a gas mixture containing from 2 to 3 percent, by volume of sulphurous acid. The production ofsulphuric anhydride is stated to be thus considerablyenhanced.—E. S,
Treating Solids with Gases, as in Decomposing CertainChlorides, Method and Apparatus for. P. JNaef, XewBrighton, U.S.A. Eng. Pat. 17,852, Aug. 19, 1898.
IN the production of chlorine from magnesium chloride,revolving furnaces are used, into the upper of which amixture of magnesium chloride and magnesia is con-tinuously fed : it descends against a current of heated airinto another inclined furnace, supplied with weak chlorinefrom the former, and issues as oxide. Two hot air stovesare used alternately to supply the heated air necessaryto the reaction, to the revolving furnace, each stovebeing successively heated by combustion of fuel within it,to prepare it for the passage of the air. The dilutechlorine from the lower furnace enters one or other ofanother pair of heaters working in the same way as theformer pair, and which are so constructed that the dilutechlorine gas cannot come into contact with any metallicsurfaces. The heated gas and air then pass to the upperfurnace to become strengthened by more chlorine, the pro-cess thus proceeding continuously. The chlorine is conductedthrough suitable apparatus to be cooled and washed free fromacid, and is afterwards led over slaked lime for conversioninto bleaching powder.
The apparatus is also available generally for treatingsolids with gases, as in the decomposition of sulphur oresto obtain sulphurous acid, &c.—E. 8.
Sodium Cyanide, Mamifacture of. G. W. Johnson, London.From Deutsche Gold und Silber Scheide-Anstalt vormalslioessler, Frankfort-on-Mainc, Germany. Eng. Pat. 279,Jan. 5, 1899.
THE inventors have discovered that sodium cyanide precipi-tates sodium carbonate from strong solutions, and on thisproperty they base their process of obtaining the formersalt free from the latter. A sodium cyanide solution, or" lye/ , nearly free from carbonate is obtained by systematicextraction at about 33° C. of a mixture of the two salts,"using the second solution from the previous operation',being poor in cyanide and rich in carbonate, for thepurpose of ^ extracting a fresh charge, whereby the sodiumcarbonate is displaced from solution by the sodiumcyanide." According to the second claim, the mixedsalts are dissolved in a minimum of water, and sodiumcyanide is added at 33° C , to precipitate the carbonateOr the mixed solution is concentrated in a vacuum untilonly carbonate separates. The hydrated sodium cyanidecrystals thus obtained may be dried over desiccators in avacuum to obtain the anhydrous salt. Sodium cyanide withtwo atoms of water of crystallisation, on , fusion, yields adeposit of the anhydrous salt; and by saturating causticsoda solution at 33° C. with hydrocyanic acid, aShydroussodium cyanide separates immediately.—E. S.
Lifting Acids or Acid Liquors; Construction of Centrifugal
:ty ~^A ^ ^ " " i i u g a i p u m p tor lilting acids oacid liquors, constructed with a bucket formed of a disc, i
Jan.3i,im] THE JOURNAL OF THE SOCIETY OF CHEMICAL INDUSTRY.
which is an open central space, provided with alternatelylong and short vanes radiating from the centre, the longvanes extending from the circumference to the boss crossingthe open central space, and the short vanes extending fromthe circumference to the edge of the open central space."There are " suitably shaped stones having a recess forenclosing a centrifugal bucket and inlet and outlet passagesformed in said stones, which are united by metal bolts andclamps coated with an acid-resisting composition" ; thebucket is of brass coated with ebonite or the like, as are allother parts exposed to the action of acids or acid liquids.
—E.S.Salts of the Ozyhcfiogen Acids, such as Chlorates and
Hypochlorites and the like; Manufacture of P. Imhoffand the United Alkali Company, Ltd., Liverpool* Eng.Pat. 1017, Jan. 16, 1899.
IN the electrolytic process for the treatment of alkalichlorides to obtain the products named in the title, secondaryreactions occur, which it is the object of the invention toprevent by the addition of small portions of sodium phos-phate or of " a body belonging to these oxides which arecapable of either basic or acid reaction, according to thenature of the substances with which they are in contact.'.
Such bodies are alumina, boric anhydride* silica, and the like,and the following equations exemplify the reactions : —
The particular oxide added is thus continuously absorbedand regenerated. Sodium phosphate acts similarly.—E. S.
Cyanides, Manufacturing. A. Dziuk, Hanover, Germany.Eng. Pat. 5758, March 16, 1899.
CARBIDES of the alkaline earthy metals, inclusive of thatof magnesium, are converted into cyanides by heating tofrom 1,300° to 3,000° C. in an electric furnace in a currentof pure, dry, previously heated nitrogen. u The corre-sponding ferrocyanides of such metals can be prepared byadding iron or iron compounds to the mixture to bemelted."—E. S.
Caustic Alkali and Halogen Gas, Manufacture of andApparatus therefor [Molten Cathode']. C. E. Ackers,New York, U.S.A. Eng. Pat. 16,935, Aug. 21, 1899.
THE fused salt of an alkali metal is decomposed electro-lytically while resting on a cathode of molten lead in afurnace with two laterally extending conduits, communi-cating with the different sides of the furnace, and thereis an upright conduit making connection between thetwo, which contains a mechanical circulator for effectingcirculation of the molten cathode and resulting alloythrough the furnace and the laterally extending conduits,and past an anode or anodes placed in one of the branches,whilst a current of steam is introduced into the moltencathode metal in the other branch in such a direction asto help the circulation.—G. H. K.
Caustic Alkali and Halogen Gas, Manufacture of andApparatus therefor [Molten Cathode]. C. E. Ackers,New York, U.S.A. Eng. Pat. 16,947, Aug. 21, 1899.
THE process and apparatus are essentially the same asthose described in the preceding patent and that following.The heat of combination of the alkali metal with oxygenis used to conserve the heat energy of the process by the in-jection of a proper quantity of steam under pressure througha separate body of the alloy in fluid communication withthe cathode metal, and returning the resulting lead orimpoverished alloy at a higher temperature to the pointwhere it again takes up the alkali metal. The anodepasses through an opening in the top of the furnace, and
is surrounded by a cover on which rests a body of salt, andthere is an auxiliary cover which is.fctlso sealed with salt.
—G. H. I
Caustic Alkali and Halogen Gas, Manufacture of andApparatus therefor [Molten Cathode]. C. E. Ackers,New York, U.S.A. Eng. Pat. 16,963, Aug. 21, 1899.
THE process consists in electrolytically decomposing amolten salt of an alkali metal whilst resting on a body ofmolten lead constituting the cathode, and thereby formingan alloy of lead and the alkali metal, introducing steaminto the alloy, and burning the resulting hydrogen incontact with the salt required in the process, and therebymelting such salt.—G. H. R.
Arsenious Acid, Metallic Fumes, and the like, Process andApparatus for Condensing. W. P. Thompson, London.From A. Froment, Tavagnasco, Italy. Eng. Pat. 7357,Nov. 11, J 899.
THIS is a compact absorbing apparatus, intended to replacethe lengthy flues ordinarily used in collecting arsenious andother fumes. According to the first claim, the apparatusconsists " essentially of a sheet-iron cylinder with a doublecasing, in which works an Archimedian screw or hollowspiral, surrounding a hollow axis, between the walls ofAvhich cylinder, spiral screw, and axis respectively, coldwater continually circulates, the spiral being set in motionby means of a hydraulic wheel or other suitable motor,capable of using the condensing water as motive power.9'There is also a high-pressure steam-heating device with aconical filter communicating with the interior of the cylinder,for heating the gases coming out of the cylinder, which passto a Glover tower. For collecting volatilised gold orparticles carried away by the gases, there are smallfragments of wood charcoal resting on leaden wire gratings.
—E.S.Lime and Carbonic Acid ; Producing. H. C. Bull,
Lambeth, A. C. Oakes, Putney, and T. M. Thorn, WoodGreen. Eng. Pat. 24,643, Nov. 22, 1899.
THE process consists " in charging a kiln, from which air islargely excluded, with limestone and carbonaceous fuelmaterial, supplying oxygen to the kiln at the lower partof the charge, drawing off the resulting gases and productsof combustion from the upper part of the kiln at a pointabove the charge, through the incandescent fuel materialand limestone, whereby some or all of the carbonic acidpresent is converted into carbonic oxide, drawing the wholeof the gases " • . . . "through a closed vchamber, andsupplying oxygen to the gases on their passage through thesaid chamber, thereby effecting the combustion of > thecarbonic oxide and converting the same into carbonic acid,and collecting the same in a suitable receptacle."—E. S.
Zinc Solutions, Obtaining Free from Iron and ManganeseCompounds. F. A. Gasch, Honningen-on-the-Khine,Germany. Eng. Pat. 21,871, Dec. 9, 1899.
ZINCIFEROUS spent pyrites is treated with concentratedsulphuric acid^ with or without the addition of sodiumchloride, or with strong hydrochloric acid and ferrouschloride, and, after remaining in heaps for a time, the massis roasted at a low red heat. After withdrawal from thefurnace, but whilst still nearly red hot, sodium nitrate orother oxidising agent and lime are added. The ferrous andmanganese compounds are thus oxidised and remain undis-solved on leaching, a zinc solution being obtained. Theresidue is available as an iron ore.—E. S.
TEL-GLASS, POTTEEY, ENAMELS.GICLSS, Action of Hydrofluoric Acid and Fluorine on.
Ji. Moissan. Comptes Rend. 129, [21], 799—804.HYDROFLUORIC acid, prepared from potassium hydrogenfluoride^ and absolutely free from moisture, attacks glassrapidly in the cold. The attack of glass by hydrofluoric acidis, therefore, not dependent on the presence of moisture.
Fluorine, prepared by electrolysis of a hydrofluoric acidsolution of potassium fluoride, and deprived of all trace of
THE JOURNAL OF THE SOCIETY OF CHEMICAL INDUSTRY. LJan. »i.
hydrofluoric acid by passing through a copper spiral im-mersed in a bath of liquid air or of liquid carbon dioxideand acetone, was found to be without action on any sort ofglass, even at 100° C.; bat the least trace of hydrofluoricacid, or of organic matter on the glass (yielding hydrofluoricacid when attacked by the fluorine) is enough to determinethe corrosion of the glass. —J. T. D.
Glass, The Decolorisation of. B. Moser, Karlsbad, BohemiaEng. Pat. 1880, Jan. 26, 1899.
A MIXTURE of manganese peroxide, selenium, bismuthoxide, nickel hydrate, and arsenious acid, in specified pro-portions, is added to molten glass in order to remove orneutralise the green tint, due to iron, which is so oftenpresent in glass,— G. H. B.
Glass ; Process for the Total or Partial Hardening of.(.'). Imray, London. From The Societe des Verreries deBruxelles, Brussels, Belgium. Eng. Pat. 17,339, Aug.26, 18D9.
THIS process is to be applied to glass articles during theoperation of " cutting/, and consists, after a preliminaryannealing, in reheating the articles after the first roughg,grinding, and in then quenching them quickly in hot greaseapplied in a convenient way. The subsequent fine grindingand polishing of the articles thus hardened can be effectedwith little loss from breakage.—G. H. B.
GLASS in a hot and plastic condition is passed betweenrevolving rollers which have been shaped or engraved in asuitable way for pressing out the glass in the form ofribbons, lenses, tubes, &c. The claim includes the methodof engraving or shaping the rollers.—G. EL B.
IX.-BUILDING MATEKIALS, CLAYS,MORTARS, AND CEMENTS.
Bricks of Lime and Sand L. C. Wolff.Thonind. Zeit. 23, [61], 854—859.
IN reviewing the various processes, patented in Germany,for manufacturing artificial stone bricks from lime and sand,the author points out that, almost without exception, themethods employed must result in the presence of a largeproportion of residual caustic lime which leaves the stonssoft and of low tensile strength; and, through the increasein volume consequent on the subsequent absorption of CO2,the cohesion of the mass will be reduced. From his pointof view, as engineer to the Magdeburg Boiler InspectionAssociation, the use of these bricks must be regarded withsome suspicion until satisfactory proof of their durabilityhas been produced, and he recommends the demand ofguarantees that the articles will meet the requirements of thetests prescribed by the Charlottenburg Testing Institute.
Portland Cement and Trass Mortar ; Influence of CarbonDioxide on. Schiffner. Thonind. Zeit. 23, [64], 909—911.
THE result of the experiments made with samples immersedfor some time (10—30 months) in the well at the BonnWaterworks pumping station, show that:—
1. No calcareous cement is capable of permanently re-sisting the destructive influence of free carbon dioxidepresent in water;
2. Trass mortar is inferior in resisting power to Portlandcement mortar, the loss sustained by the former in 28 months
being given as 24*75 per cent., compared with 12*10 percent, for the latter in 30 months ;
3. Marble also—even the hardest—is more corroded thanPortland cement mortar, the loss being 10*99 per cent, in10 months, against 5-53 per cent, for the mortar ( 1 : 1 ) ;
4. So far as the tests have extended, no increase mresistance has been found to result from the addition oftrass to Portland cement mortar;
5. Old trass mortar is more resistant than fresh ;6. Treatment with fluorine compounds appears to offer
the best protection against corrosion; whether the lead,magnesium, or zinc compound be used, seems immaterial inpoint of efficacy.—C. 8.
Portland Cement • from Basic Slag, von ForeWs Processfor the Production of Karamerer. Stahl u. Eisen, 1899,19, 1088; through Chem. Zeit. Rep. 1899, 23 , [37],366-
THE slag is calcined with lime in a specially constructedfurnace, after which the mixture is ground and burnt in thepowdered condition by means of small coal. The clinkerproduced is of small size and grinds readily. If necessary,the slag is desulphurised in the preliminary calcining process.The method is in use at Lollar (Hessen), and is said tofurnish a normal Portland cement of excellent quality,while effecting considerable economy in labour and cost ofplant, the usual operation of making into bricks beingdispensed with.—H. H. B. S.
Hydraulic Cement, Constitution of O. Kebuffat. Thonind.Zeit. 23 , [64], 900—903; [70], 989—991. (See alsothis Journal, 1899, 761.)
Calcium Silicates and Calcium Aluminates,—A series ofthree aluminates and three silicates, treated with sugarsolution (1 grm. of substance and 200 c.c. of solution), gavethe following results :—-
J)^s- i o$!
1340
4-50e-408'70
10-70
A L>2CaO.'
is-oo20'3027*0083'80
AloO,3CaO.
32*5031*2040-0047-00
SiO.CaO.
0*801-201-20
SiO22CaO.
3 • eo4*004-00
SiO.,30aO.
12-GO11-80uroo
The percentage of lime remaining in the aluminate residueis fairly constant ^27*7—28-87 per cent.), and indicates thepresence of the hydrated aluminate 3Al2O;j2CaO 4- aq.In the case of the silicates, the results are regarded asapproximating to those of theoretical calculation.
On mixing the aluminates and silicates together andtreating with sugar solution as before, the results obtainedindicate that the bicalcium and tricalcium silicates remainindifferent towards the aluminates, but that monocalciunisilicate combines with the aluminate, the reaction beino*accompanied by separation of CaO, since the amount (8 • 00)of this body extracted in 53 days exceeded the calculatedquantity (5-95). This result was confirmed by addino- toeach aluminate sufficient hydrated SiO2 to combine withthe liberated CaO and form calcium monosilicate :
Days.1 grm.
+ 0'176 tfhydrated Silica,
. A12O3 2CaO+ 0*55 grin.
hydrated Silica.
6-6010 • 00
18*0025'20
lgrm.Al 20 s3Ca0+ 0*77 prm,
hydrated Silica.
38-8038-80
thus showing that the silicate in question is able to combinewith these alummatos, with liberation of CaO. On the basisof the amount thus set free the composition of the residual
ftv ™mfUmlS, W ? ^ u l a t e d , and a series of six wasestablished, two of which correspond to Thompsonite andAnorthite respectively.
With regard to the action of distilled water on the calciumdstilled water on the calcium
O S S ' % ( w f f i o ^ l t i ° n Pr°dUCtS wero Obt<™cd ''2O3CaO, 7H2O ; Al2O32CaO, 5H2O s Al2O33CaO, GHX> •
Jan. si i9oo.] THE JOUENAL OF THE SOOIEW OF OHEMtOAL INDUSTRY. 49'
the first being semi-liquid and produced by two stages, whilstthe others are solid.
An examination of the result of treating the anhydrousaluminates with a large volume of water, led the author todisagree with Le Chatelier's assumption of supersaturation,and to believe that alumina is liberated in the colloid formand afterwards deposited.
In lime water, on the other hand, no solution takes place,only hydration, the monocalcium aluminate increasing involume and solidifying, whilst the diealcium salt neitherswells nor sets, and the other merely increases in bulkwithout setting. The percentages of combined water afterthree days' digestion were 27 • 44,11 • 25, and 21 • 97 per cent.respectively, and a bright red heat was required to effectdehydration.
About 5*48 per cent, of water was found to be absorbedby the orthosilicate in setting.
The author's conclusions with reference to the compositionof the cement after setting, are that all hydraulic cementsconsist of calcium hydroxide, hyclrated calcium aluminate,hydrated calcium orthosilicate (2(SiCh>, 2CaO), H2O), and,when a large proportion of silica is present, anhydrouscalcium metasilicate, which forms a double salt with thealuminate—a circumstance explaining the resistance offeredby cement to sea water—and a small quantity of inertmatter. The aluminate is generally the mono- or bi-salt,except when the cement is rich in lime or the conditions ofpreparation favour the production of the tri-aluminate.The amount of water of hydration depends on the methodemployed, and cannot be determined beforehand.
The author would divide the hydraulic cements into twogroups : (1) the non-crystalline hydraulic limes and quick-setting cements, composed of a mixture of calcium oxide(sometimes absent), calcium orthosilicate, and calcium alu-minate ; (2) the crystalline Portland and siliceous cements,consisting of a compound of crystalline SiO2 2CaO, withCaO and a calcium aluminate. The phenomenon of settingis chiefly due to the conjoint hydration of the orthosilicateand the aluminate present, the amorphous silicate in non-crystalline cements becoming crystalline when hydrated, andthe anhydrous aluminates accelerating the solidification ofthe mass when present in quantity. In the case of crystal-line cements, it is assumed that the orthosilicate is unitedwith CaO and a crystalline (usually mono-) calciumaluminate, the silicate and oxide being separated duringhydration. That cement can be heated to bright rednessand still retain its form, though the pure orthosilicateundergoes disintegration when thus treated, is ascribed tothe action of the aluminates.—C. S.
Hydraulic Cement, Note on liebuffafs Researches on theConstitution of. W. Michaelis. Thonind. Zeit. 23, [61],853.
W I T H regard to the employment of sugar solution (thisJournal, 1899, 761), the author states that he used thisreagent some 30 years ago, and found that the proportionof lime extracted bv the same from Koman cements,Portland cements, and calcium aluminates varied accordingto the concentration of the solvent (8—20 per cent.) andthe quantity taken. Calcium aluminate, equivalent to asmuch as 0*25 grm. of Al2O;i per litre of solvent, was alsoextracted; and further quantities of lime could be dissolvedout of the residue from the first extraction Avhen washedwith distilled water and treated anew with sugar solution—which considerations convinced him of the unsuitability ofthe reagent for the purpose in view.—C. S.
Hydraulic Cements, Action of Sea Water on. — Schuliat-schenko. Thonind. Zeit. 23 , [64], 913—915; [671,948—950.
THE author points out that none of the researches hithertomade have afforded satisfactory proof of unsuitability onthe part of hydraulic mortar to withstand any chemicalaction that may be exerted by sea water. Further, thatPortland cement possesses a decided advantage over othercements in that it is not merely a local production, but canbe manufactured wherever lime and clay are found, is offairly uniform composition and quality, and—by reason of
the numerous investigations of which it has been the sub-ject—can be relied on for use in marine work, providedordinary care be exercised in applying it, and controlling thequality by normal tests.
He also confirms the utility of the proposal made byMichaelis (this Journal, 1897,915) to improve Portlandcement by the addition of trass, though experience hasshown that such additions are not indispensable.—C. S.
PATENTS.
Vulcanite, Hard Woods, or other Hard Materials, or forany other Uses or Purposes to which same may be^ up-plicable ; Manufacture of a Substitute for. S. L\ Earle,Mitcham, Surrey. From P. W. Wierdsma and J. Kuipers,both of Holland. Eng. Pat. 18,340, Aug. 26, 1898.
!FIBHOTTS waste materials arc cleansed and then boiled witha solution of resin or other soap, which is afterwardsmade insoluble by precipitation with alum or other suitablesalt, The mixture of fibrous material and insoluble soap isafterwards consolidated by heat and pressure in suitablemoulds.—G. IL B.
Wood, Process for Preserving. G. K. Sebioda, Boulogne-sur-Seine, France. Eng. Pat. 21,814, Oct. 31, 1899.
IN this process the wood is saturated with a dilute solutionof formaldehyde, either by sprinkling, immersion, impreg-nation under pressure, or in any other suitable manner.The formaldehyde unites with the albumin of the sap to forminsoluble compounds, which resist the attacks of, or destroy,all living organisms which prey upon the wood. In case thewood does not naturally contain a sufficiency of albuminoussubstances, solutions of agar-agar, or other substances whichcontain chondrin or albumin, are employed. The formalde-hyde is added thereto, and the wood is treated with themixture and then dried. It is claimed that a protectinglayer is thus formed round each fibre of the wood. If railwaysleepers be thus treated, and are air-dried, when in contactwith damp earth they would constantly give off a portion ofthe formaldehyde to the latter, and thus become surroundedby a protective zone. Wood intended for use in marineconstructions must, after treatment, be more thoroughlydried by heating to 110° C.; the protective formaldehydecompounds are thus rendered quite insoluble.—L. A.
Artificial Marble, Granite, and the like, Manufacture of.T. W. James, Smethwick, Stafford. Eng. Pat. 25,155,Nov. 29, 1898.
FOR the production of white marble, calcined chalk, micadust, ground borax, and soluble silicate are made up withhot water, and the mixture run into moulds. The blocksare allowed to become about half-dry, and are then stampedto represent veins, grain, or other figuring. The recessesthus produced are filled with oxide of manganese and finelyground or soluble slag, after which the surfaces aresmoothed and polished with a bevelled glass tool. Uardilla,Kilkenny, and Devonshire marbles, and Aberdeen or Port-land granites, are also imitated in a similar way, the variousmixtures for which form the subject of separate claims.
II. H. B."Artificial Stone; Process of Manufacturing. R. Haddan,
London. From R. Koepp and Co., Oestrich-on-the-Khinc, Germany. Eng. Pat. 25,304, Nov. 30, 1898.
ROOM for the expansion of the mass in the setting ofcement in the mould is provided for by aspirating away theexcess of the water used, so as to replace it by air. Thematerial then forms a sounder, and therefore stronger blockon setting hard.—G. H. B. *
Artificial Stone for Lithographic and other Purposes •Producing. P . G, Bate and A. C. Oakes, both of London'
< and T. M. Thorn, Wood Green, Middlesex. Eno- P a /27,327, Dec. 27, 1898. *
MAKBLM chips are calcined in a close kiln burning carbonicoxide and hydrogen supplied from a gas producer, thecarbonic acid disengaged being washed, cooled, and storedThe quicklime produced is slaked, sieved, and moulded intoslabs, which are then dried and impregnated under pressure
K
50 THE "JOURNAL OP THE SOCIETY OF CHEMICAL INDUSTRY
with the carbonic acid gas produced in the calcination of themarble.— H, H. B. S.
Bricks, Slabs, Blocks, Flagstones, and the like ; The Manu-facture of. G. A. Boisselier, Puteaux, and X. C. Laurent,Paris, Eng. Pat. 1664, Jan, 24, 1899.
A MIXTURE containing lead and magnesium carbonates,alumina, felspar, and sodium hydrate in specified proportion,is mixed with an acid solution of magnesium chloride andzinc sulphate, to form a cement for binding together wastematerials into solid blocks.—G. H. B.
Kilns, Continuous-burning, for Hurning Bricks and otherClay Goods, and also for Limes and Cements. H.K. Vaughan, Belfast. Eng. Pat. 19,168, Sept. 23, 1899.
CERTAIX modifications are introduced into patentee's priorspecification, Eng. Pat. 20,540, Oct. 31, 1895 (this Journal,1896, 810), consisting in alterations to certain of the flues,the provision of additional ones, and the construction ofopenings in the side walls of the kiln for the reception ofportable furnaces.—II. XL B. S.
Drying Bricks, Earthenware, Cement, Slurry, and the like,before Burning, or Drying Salt, Whiting, Sfc, Methodfor. W. Allison and J. English, both of Birtley, Durham.Eng. Pat. 19,192, Sept. 23, 1899.
T H E materials to be dried are loaded upon trucks andpassed through tunnels supplied with heated air, derivedeither from the cooling of goods which have been previouslybaked or from a special furnace.—H. H. B. S.
Kihis for Burning Cement-making Materials, and forsimilar Purposes. J . C. Swan, Newcastle-on-Tyne.Eng. Pat. 17,696, Aug. 16, 1898.
THK raw material is fed in at the top of the kiln throughiron tubes, and descends to a brickwork chamber con-structed wider at the top than at the bottom. Beneath thisis a jacketed continuation wider at the bottom than at thetop, and provided with means for allowing a current ofwater to flow through the jacket. The kiln is fired bymeans of an inlet into the jacketed continuation connectedwith a gas producer or furnace. At the bottom is achamber for cooling and withdrawing the burnt material.
——H. H. B. S.
(Jements, Impts. in. L. Grabau, Dahlbruch, Germany.Eng. Pat. 1302, Jan. 19, 1899.
ST,ATE powder is mixed with pulverised limestone andinferior or partly burnt cement. The mixture is slightlymoistened and moulded into blocks, which are then burntand pulverised.—H. H. B. S.
Drying Apparatus applicable for Use in the Manufac-ture of Portland Cement and for Analogous Purposes.P. Davies, Southfields, Surrey, and E. J. V. Earle,London. Eng. Pat. 1756, Jan. 25, 1899.
T H I S is an apparatus for drying slurry. It consists of arotating cylinder, heated internally by means of a liquidfuel burner or by other means. Enveloping the cylinderand at a distance from it, a easing is fixed, which thusencloses an annular space into which the slurry is fedthrough a hopper. The hot gases, after heating thecylinder, pass through openings into the annular space, andfrom thence are exhausted by means of a fan. The slurrydries on the periphery of the cylinder, from which it isdetached by a scraper and falls through an opening intotrucks or into a receptacle* connected with a conveyor.
—H. II. B. S.
Portland Cement from Blast-Furnace Slag and Lime andthe like. C. von Eorell, Giessen, Germany. Eng. Pat.16,050, Aug. 5, 1899.
BLAST-furnace slag and limestone, chalk3 or similar materialare first burnt at a clear red heat, and then ground andburnt together to clinker* The usual operation of makingup the raw materials into bricks before burning is thusdispensed with.—H. H. B. S.
Preservation of Natural or Artificial Siliceous, Argil-laceous, and Calcareous Substances; Process for the. M.Dumas, Niort, Trance. Eng, Pat. 21,185, Oct. 24, 1899.
THE preservation is effected by covering the substanceswith a hot mixture of bituminous and resinous materials,which is made to penetrate well under pressure, and whichbecomes solid on cooling.—G. H. B.
X.-METALLUEGY.The Cripple Creek Goldfield, Colorado. T. A. Eickard.
Trans. Inst, of Min. and Met., Nov. 15, 1899.T H E gold occurs sometimes in the native state, but chieflyin the form of tellurides, the minerals consisting of thedouble tellurides of gold and silver, sylvanite and petzite,and the single gold telluride, calaverite. The first-named issilvery-white in colour, the second from steel-grey to iron-black, and the third similar to iron pyrites in appearancebut differing as to brittlencss. The ores have averaged 3 oz.per ton until recently, when the milling of large quantitiesof low-grade material has reduced it to 2 oz. Its treatmentwas originally by stamps and amalgamation, but the extrac-tion was low, owing to the non-amalgamation of the goldtelluride and of the native gold coated with iron telluride.The 270 stamps started in 1892 and 1893 are consequentlynow idle, and the extraction is divided between barrelchlorination and cyaniding in the ratio of about six mills ofthe former to two mills of the latter.
There is a tendency towards favouring chlorination forfuture developments, since it is now considered necessaryto roast the ore for the cyanide process in the sameway as for the chlorination process, thus removing thechief advantage which was claimed for the cyanide inits ability to extract the gold from the raw ore. Thechlorination process, in its typical barrel form, has remainedpractically unchanged, any alterations consisting of largerand improved mechanical arrangements rather than of anychemical changes. The total cost for treatment bv chlorina-tion approximates to 4 dols. per ton.
Until 1892 silver mining was the all-important industryin this district, but owing to the discovery of the exten-sive rich telluride deposits in 1891, together with thedemoralisation of the silver market at the time of theclosing of the Indian mints in 1893, a great development ofthe goldfields has taken place, with the result that gold-mining is now the more important. The gold productionof Colorado has increased from 256,410 oz. in 1892 to1,138,584 oz. in 1898, the output of the Cripple Creekdistrict increasing rapidly from 100 oz. in 1891, 2,821 oz. in1892, 10,400 oz. in 1893, to 65,341 oz. in 1898. The richerore goes to the smelters, whilst the poorer material, con-taining less than 2 oz. per ton, is treated in the mills forchlorination and cyaniding. The result is that the goldoutput is about equally divided between smelting andmilling, although the greater proportion of the ore comesunder the latter treatment. The author treats the wholesubject commercially, and anticipates a large and successfuldevelopment in the future.—A. W.
Cyanide Process. H. H, Greenway. Trans. Inst, ofMin. and Met., Nov. 15, 1899.
ALTHOUGH having no real bearing on the practical cyanideprocess, the results of Eisner, published in 1846 in the./. prakt. Chem., yielded the following qualitative facts •—Ql) Platinum, tin, and mercury are insoluble in potassiumcyanide; (2) Copper, iron, zinc, and nickel arc solublewith evolution of gas, probably hydrogen; and m Gold'silver, and cadmium are soluble provided that free o x y e nbe present. J. he quantitative results since obtained, showthat 197 parts by weight of gold arc dissolved by 130 partsof potassium cyanide with 8 parts of oxygen and thi twater saturated with dissolved oxygen c o n t a £ f 8 pa ts permillion by weight. Allowing 700 lb. of solution to con-veniently saturate and cover 1 ton of ore, it follows thatthis quantity of a 0; 013 per cent, cyanide solutionsaturated with oxygen, is theoretically capable of d L S2 oz. of gold, and tha t such a liquid i
Pth
y g , heoretically capable of d L s o S2 oz. of gold, and that such a liquid i s
Pthe s t r o ™S
g°™*
Jan. 3i, 1900.] THE JOUENAL OF THE SOCIETY OF CHEMICAL INDUSTKY.
can be of use in dissolving gold, unless more oxygen isavailable than that contained in a saturated solution. Thestronger the cyanide up to this point, the more rapid is itsaction on the gold, but such a solution simultaneouslydissolves the baser metals, and practically an allowancehas to be made for a certain amount of waste.
In its bearing on the question of " selective action/' it ispointed out that an excessive quantity of cyanide cannotact on the gold, owing to insufficiency of oxygen. Con-sequently the excess, if any, attacks and dissolves onlybaser metals which require no oxygen, with the result thatthe relative proportion of these metals in the resultingliquid increases with the strength of the cyanide after itssolution has passed the above limit. Hence the apparentselective action of strong solutions for base metals andweak solutions for gold.
The author has tried experiments with a few differentkinds of New Zealand ore in order to discover the amountof cyanide consumed in solutions of increasing strength,with the result that the consumption, relative to the weightof ore treated, increases with the strength until the solutionreaches saturation, when it rapidly drops. As an example,the figures obtained, ranged from 0*03 per cent, cyanideconsumed with a 0*11 per cent, solution, to 1*76 per cent,with a 20 per cent, solution; but when saturated, theconsumption fell to 0'48 per cent. Other examplesindicate that the amount consumed with saturated solutionswas almost incapable of estimation, even with an ore con-taining much copper. In one case, the gold extraction after42 hours was 68 per cent, and the silver 57 per cent., sothat there would appear, after all, to be a selective action,—a solution for dissolving gold and silver, and for notdissolving the base metals, being not a very weak solution,but a saturated one.—A. W.
Sampling Ore Deposits. Eng. and Mining J. 1899, 68,[23], 672.
FOUR general systems are followed in taking samples of oredeposits :—
(1.) A great number of small samples are roughly takenalong lines at short intervals across the face of each planesection of ore exposed. The specimens should be takensystematically—for instance, by making a continuous groovethe length of the section, or by chipping off small pieces ofore at intervals of an inch or so.
(2.) A lesser number of large samples are carefully takenfrom along lines at wider intervals.
(3.) " Mill runs " are made, i.e., a few samples are taken,so large that each can be " milled " by itself, and furnishenough bullion to " clean up." Each sample should betaken from ore from several parts of the vein, in order thatit may be representative.
(1.) In the case of free milling ores, a rough method ofascertaining the value of gold veins is to take a large numberof very small samples, pulverise them, and estimate theamount of gold by " panning/ .
The first method is adapted for sampling ore deposits thatmust be mined on a large scale ; also where rich ore is in athin sheet; and in cases where quick approximations areneeded; since although the samples have to be assayed separ-ately, they are quickly collected. Where the rock varies inhardness, and the bits chipped off are of different sizes, andalso where thin streaks of very high-grade ore lie in a widebody of low-grade rock, this method is untrustworthy.
The second method is specially suited for ores which areso hard as to require blasting, arid for ores which varygreatly in value, and have the values distributed withoutsystem. The sample, which should be large enough torepresent all variations along the line of the cut, is reducedby pulverising and dividing by successive quarterings to asuitable size. It is advisable to assay two independentsamples from the last quartering.
The third system is only practicable when there is amill or sampling works close at hand, and even in suchcase, is better suited for determining the proper processof treatment for the ore, than the actual value of thelatter. It is stated that mill runs are not very trust-worthy, as the samples are takeu from a few points
along the vein, and it is almost impossible to get the rightproportions of the different grades of ore in each; also,the nearest available mill may be totally unsuited for theore.—A. S.
Fume from Molten Slag in Lead Smelting, Compositionof. M. W. lies. Eng. and Mining J. 1899, 68 , [25],729.
THE author has made an examination of a very large andrepresentative sample of the "slag fume," collected bywithdrawing it, by means of a 3-in. pipe, 3 ft. from thetop of a 60-ft. brick stack which conducted the fumes fromthe lies patent slag settler. At the discharge end of thepipe there was connected a specially constructed heavytin box, 3 ft. x 3 ft. x 5 ft., to the top of which wasattached a circular thimble, to which was tied a flannelbag, 18 in. in diameter when distended, and 10 ft. long.The fume was thus filtered through the meshes of thecloth, and the attendant would from time to time shakethe has: in accordance with the observed resistance topressure.
The chemical composition of the fume was as follows :—Silica (SiO2), 1 • 70; iron as Fe2O3, 1 • 00 ; zinc as ZnO,21-00; sulphur as SO2, 1*60; sulphur as >SO3, 9*75; lime(CaO), 0 #60; arsenic as As2O3, 0 # l 8 ; alumina (A12OH),1-20; potassium as K>O, 0*60; sodium as Na2O, 0*85;carbon (C), 24-40; lead as PbS, 14-64; lead as PbO,21-64; ammonia (NH3), distinct trace. Not even tracesof barium, magnesium, antimony, cadmium, bismuth,phosphoric acid, titanic acid, chlorine, fluorine, and copper,could be discovered. The following results Avere obtainedby a fire assay:—gold, trace; silver, 7*4 oz. per ton of2,000 lb. j lead, 30-2 per cent.—A. S.
Blast Heater, The Bretherton. Eng. and Mining J. 1899,68, [24], 698.
A DESCRIPTION is given of a method, devised by H. E.Bretherton, of heating blast by utilising the heat of theslag from the furnace.
The blast is trapped and the slag and matte flow con-tinuously over a jacketed spout into a forehearth orsettler placed within a brick chamber, and which is largecompared to the size of the furnace. The slag flows fromthe settler continuously and the matte is tapped at intervalsfrom the bottom spout. Over the settler is a large rect-angular sheet-iron box, which has vertical flues passingthrough it; the larger portion of the box is directly overthe settler. The heat radiated from the molten slag passesupwards through those flues situated directly overhead,downwards through the other flues, then under and aroundthe settler, and out through the chimney. The rectangularbox is placed between the blower and the wind-box of thefurnace, and the blast is made to traverse twice throughthe box by means of a vertical diaphragm contained in thesame. When desired, sticks of wood may be introducedthrough a small door in the brick wall over the settler,for the purpose of keeping a small fire on the surface of theslag; this^ also assists in heating the blast. It is statedthat by this method the blast is heated up to 500°—600° F*
The following advantages are claimed for the system:—By using hot blast, the sulphur is burnt as fuel and re-places part of the coke ; also the ore begins to smeltquicker and closer to the tuyeres, keeping them brighter.The capacity of the furnace is increased, and in& con-sequence of the fast running, it is possible to trap theblast, and have a continuous stream of slag runningthrough the trapping-box and into the spout, which givesthe matte better opportunity to settle from the slag. Theautomatic tapping of the slag and matte does away withthe danger of getting slag up in the tuyfcres, and alsosaves the furnacemen much labour.
It is estimated that on one 60-ton furnace (using 60 tonsof ore and flux) a total of 152 dols. per day is saved bymeans of the arrangement, without including the economyeffected m having cleaner slag. In the above estimate alsothe economy is ignored which is effected in original cost ofplant, occasioned by the fact that no fine-crushing machineryand roasting furnaces are required.—A. S.
2
52 TflM JODENAL OV THE SOCIETY OF CHEMICAL INDUSTRY.[Jan. 8J, 1900-
Calcium Carbide, A Neiv Application of. [MetallicReduction.'] FrShlich. J. fur Gasbelcucht. 42, [45J,762.
METALS may be directly obtained by gently heating amixture of calcium carbide with the metallic compoundsordinarily obtained by the roasting and extraction of ores.Thus, copper is obtained from the roasted ore mixed withcarbide, by warming the mixture to start the reaction,which thereupon proceeds violently- 0*1 to 0#25 ton orcarbide is required for the production of a ton of metal mthis manner. The new method, by which such results areattained, fully utilises the energy of combination of thecarbide. Copper-, lead- and aluminium-bronze and otheralloys have been produced by the method.—J. A. 13.
Tungsten, Preparation of. A. Stavenhagen. Ber. 1899,32, [16], 3064—3065.
THE method of preparation previously described (thisJournal, 1899, 687), is improved by adding about one-thirdof its volume of liquid air to the mixture of tungstic acidand aluminiuia contained in a clay crucible^ When thereaction is over, a regulus of tungsten containing a smallquantity of aluminium is obtained. When lithium para-tungstiite, fused at about 1,000° C., is electrolysed, well-formed crystals of lithium tungsten bronze are obtained,and not metallic tungsten as stated by Hallopeau.—T. E.
Molybdenum and Uranium, Preparation of A. Staven-hagen. Ber. 1899, 32, [16], 3065.
A MIXTUHE of uranic acid and aluminium of the compositionUrO3 + 2A1, 30 grms., is treated with 20 ex. of liquid airand ignited. When the violent reaction which supervenes isat an end, a regulus of metallic uranium is obtained.
Molybdenum is obtained in a similar way, but the yield isnot so good, on account of the volatility of the molybdenumoxide.—T. E.
Copper Alloys, Durability of the most frequently used, inSea-Water. Diegel. Verhandl. Ver. z. Before!, d.Gewerbfl. 1899, 313; Chem. Zeit. Rep. 1899, 23, [37],366.
CORROSION by sea-water is chiefly experienced in the caseof copper alloys rich in zinc, and is traceable to the destruc-tion of the alloy by the extraction of the zinc. When twometals are in contact in sea-water a voltaic current is set up,that metal being especially attacked which stands highest inthe electro-motive series—in the case of copper alloys,therefore, those richest in zinc. As a rule, the greater thedifference between the alloy and the metal in contact with itin their electro-motive order, the greater is the corrosion.
—H. H. B. S.
" Magnalium" [Magnesium-Aluminium Alloy']. L. Mach.Eng. and Mining J. 1899, 68, [23], 664.
THE author has prepared alloys of magnesium and alumi-nium, which are lighter than aluminium, and can be workedlike brass. The metallurgical properties depend upon thecomposition of the alloy. An alloy containing 10 per cent.of magnesium resembles zinc in appearance, one containing15 per cent. " is like brass/ , and one containing 25 per cent." like a compound bronze.,. The alloys keep well in dry anddamp air, and give good castings.
A scientific instrument maker, who has examined somesamples of " magnalium " containing from 10 to 12 per cent.of magnesium, reports that the alloy is almost as white assilver, and can be turned, bored, &c, quite as well as brass.Clean and neat threads of 0'25 mm. pitch can be cut on thealloy with ease. It cannot be filed so readily as brass but issuperior in this respect to copper, zinc, and aluminium. Ifbought by volume, magnalium is a little less expensive thanbrass.—A. S.
Cadmium and Copper Alloys. A. A. Baikow. Chem 7eit1899, [86], 931.
THESE alloys have a maximum freezing point at 565° C,corresponding to the formula Cd2Cu with 22 per cent, ofcopper. There are two minimum freezing points: the one at315° corresponds to a eutectic alloy of the compound Cd Cu
and cadmium containing 7 per cent, of copper, the other-at540° corresponds to a eutectic alloy of the compound CdXuand copper containing 40 per cent, of copper.
Determinations of §io electro-motive forces of these alloys,and examination of their micro-structure, confirmed theseconclusions.—T. E.Cyanide Process at Yalwal, N.S. Wales. Alfred Chiddey.
See page 25.
Iron Ore; Oxidation of Ammonia by. W. CarnckAnderson and Geo. Lean.
See page 28.
Gold, Iodometric Determination of. F. A. Gooch andF. H. Morley. Amer. J. Science, Silliman, 8, [4] , 261.
See under XXIII., page 72.
Pig Iron, Determination of Sulphur in. M. J. Moore.J. Amer. Chem. Soc. 1899, 21, [11], (J?2.
Crucibles, hnpts. in. J. W. Woolford, London. Eng. Pat.24,479, Nov. 19,1898.
PLUMBAGO crucibles are lined inside with clay.— J. H. C.
Moulds for Casting Metal, Coating of. H. Stanning andT. Aldcroft, London. Eng. Pat. 25,305, Nov. 30, 1898.
THE moulds are coated with a finely ground mixture offour-fifths of asbestos, one-tenth of clay, one-tenth of car-bonate of soda. This may be applied either as a powderor mixed with water.—J. H. C.
Sulphurous Ores containing Arsenic, Antimony, or Tel-lurium; Treatment of W. T. Whiteman, Middlesex.From E. Petersson, Brussels. Eng. Pat. 21,138, Oct. 7,1898.
THE ores are pulverised, mixed with 10 per cent., more orless, of powdered carbon, and heated in a muffle furnace toabout 800° C , to expel the arsenic ; they are then calcined,washed with acids to remove antimony and tellurium, andsubsequently treated by ordinary processes for the extractionof gold or other metals present.—J. H. C.
Roasting Ores, Furnaces for, and the like. W. A. Kone-man and W. H. Hartley, Moorfields, Middlesex. Eng.Pat. 21,213, April 28, 1899.
THE improvements consist of variously arranged valvedflues, flame and suction chambers, exhausters, exhaustpassages with baffles, pockets, screens, &c, which arefully described in detail.—J. H. C.
Carburising Steel for Armour Plates and other purposesW. C. Johnson, Liverpool. From J. S. Unger, Pennsyl-vania, U.S.A. Eng. Pat. 19,093, Sept. 22, 1899.
HYDROCARBON gas is brought into contact with the plateswhile they are at a temperature of about 550° C thereby
? T $ a i nn?2SipOf C ai r b O n J -he . t e m P e r a t u i * * then raisedto 8/5 - 1 0 0 0 C , and so maintained for six days or more
additional gas being admitted from time to time.-—J. H C '
Brazing or Soldering, of Objects made of Aluminium or of
Nov £°1898 g ° 1 U ' Pa r iS ' E D S - P a t ™>W>THE parts to be joined are coated with a solution composedof ethyhc alcohol, 95 parts , Venetian turpentine! aTartsessence of lavender 2 parts. They are then heated to a tem-perature of about 150° to 300° C , during which operation thTyare coated with a thin layer of solder ?omposed^f (1) from10 to 20 per cent, of an aluminium alloy, and (2} from ftnto 90 per cent, of tin. This is prepared ^ y first m e S thetin and then pouring the melted aluminium alloy into ^ s t i r -ring until the mixture begins to solidify. The aliLhuum al o y
Jan. si, woo.] THE JOURNAL OF THE SOCIETY OF CHEMICAL INDUSTRY. *>
is made by melting in a non-silicious crucible 98 per cent,of pure aluminium and 2 per cent, of the special alloy. Thespecial alloy is composed of copper, 2 to 6 parts ; nickel,1 to 3 par ts ; fine cast steel, 1 to 2 parts ; and purealuminium, 1 part.
After the parts to be joined have been prepared asdescribed, they are placed together and heated so as to meltthe thin coating of solder, more solder being added ifnecessary.—J. H. C.
Solderi7ig Aluminium and its Alloys. G. E. Bourgoin, Paris.Eng. Pat. 23,902, Nov. 12, 1898.
T H E articles to be soldered together are dipped into orcoated with a mixture of ethylic alcohol, 95 parts ; Venetianturpentine, 3 parts; essence of lavender, 2 parts ; and thenplaced in a cavity in some fire-resisting material. Theyare then made about red hot by means of the blowpipe, andmolten aluminium or aluminium alloy is poured over thejoint through a suitably formed " runner."—J. H. C.
Aluminium Alloys : Method of Casting them. W. A.McAdams and D. D. Book, Brooklyn, U.S.A. Eng. Pat.21,137, Oct. 23, 1899.
THE improved alloy is composed of aluminium, 70 per cent.;zinc, 23 per cent. ; copper, 7 per cent, with or without asmall percentage of nickel. The improvement in casting iseffected by artificially cooling the metal more rapidly thanhas hitherto been usual, e.g., at a rate of not less than one-fifth of a calorie and not more than two calories per secondfor a sphere of 1 in. diameter.—J. II* C.
White Lead, Process for the Manufacture of, and for theRecovery of Silver in said Process. A. C. J. Charlier,Glasgow. ^Eng. Pat. 552, Jan. 10, 1899.
See under XIII. A,, page 5o.
Portland Cement from Blast-Furnace Slag and Lime, andthe like; Production of C. von Forell, Giessen, Germany.Eng. Pat. 16,050, Aug. 5, 1899.
Aluminium and Magnesium, The Fluorescence of, in Wateror Alcohol, under the Discharge of the Induction CoiLPerreau. Comptes Rend. 129, [23], 957—959.
WIIKN an electrode of magnesium or aluminium, immersedin distilled water, is made the terminal of an induction coil,the other terminal being either a second piece of the samemetal or a strip of platinum, the magnesium or aluminiumbecomes feeblv luminous when the coil is in action. Theeffect takes place only at the anode, and is really analternating phenomenon, though it appears continuous tothe eye. Other metals do not show it, nor is it shown byany metal in petroleum or other insulating liquid. Theauthor is disposed to attribute it to an action between themetal and the liquid across the thin dielectric coating ofoxide formed.—J. T. !)•
Electrolysis of Metallic Phosphate Sohitions. H. M. Fern-berger and E. E. Smith. J . Amer. Chem. Soc. 1899, 21,[11], 1001—1007.
THE authors illustrate the modifications of the differentfactors (current, density, voltage, &c.) which they havefound satisfactory, by a series of experimental examples,from which the following may be quoted : —
Copper from Iron.—60 c.c. of a disodium hydrogenphosphate solution (sp. gr. 1 • 0358) were added to 25 c.c. ofa copper sulphate solution ( = 0*1239 grm. of copper) and50 c.c. of a ferric ammonium sulphate solution (0-2002grm. of iron). The resulting precipitate was dissolved in10 c.c. of phosphoric acid (sp. gr. 1 -347). The conditionsduring the electrolysis were ND100, 0-4 ampere; voltage,2-4; dilution, 225 c.c.; temperature, 53° C.; time, 7 hours.The copper deposit weighed 0-1237 grm., and was freefrom iron.
Copper from Aluminium. —The solution contained 0 ' 1239grm. of copper, and 0-1 grm. of aluminium. 60 c.c. ofdisodium hydrogen phosphate (sp. gr. 1-0338) and 5 c.c. ofphosphoric acid (sp. gr. 1*347) were added, and the liquidelectrolysed under the following conditions :—ND100, 0-068ampere; voltage, 2 -6 ; dilution, 225 c . c ; temperature,77° C.; time, 6 hours. Copper precipitated, 0* 1240 grm.
Copper from Chromium.— 60 c.c. of disodium hydrogenphosphate solution (sp. gr. 1*033) and 8 c.c. of phosphoricacid (sp. 1*347) were added to a solution containing 0*1239grm. of copper and 0-1403 of chromium. Conditions ofelectrolysis :—ND100, 0*062 ampere ; voltage, 2*5 ; dilution,225 c.c.; temperature, 64C C.; time, 6 hours. The depositweighed 0* 1243 grm., and was free from chromium.
Copper from Cobalt—The same quantities of the copperand of the phosphate and phosphoric acid solutions wereelectrolysed with ND100, 0*035 ampere; voltage, 1*5;dilution, 225 c.c.; temperature, 62° C.; time, 6 hours.Copper found, 0*1243 grm. No trace of the cobalt taken(0-1 grm.) was found in the precipitate.
Copper from Zinc.—The proportions of metals, phos-phate, and phosphoric acid as before. Conditions ofelectrolysis :—ND100, 0*035 ampere ; voltage, 2*5 ; dilution,225 c.c. ; temperature, 60° C. ; time, 5 hours. Copperfound, 0-1244 grm., free from zinc.
Copper from Nickel—Copper as before. Nickel nitrate(=0-1366 grm. of nickel). Sodium phosphate solution,75 c.c.; phosphoric acid, 5 c.c. Conditions of electrolysis :—ND100, 0*072 ampere; voltage, 2*45; dilution, 225 c.c.;temperature, 66° C. ; time, 6 hours. Copper found,0*1241 grm.
Copper from Iron, Cobalt, and Zinc.—To the solutionof the metallic salts, 30 c.c. of the phosphate solution and15 c.c. of phosphoric acid were added. Conditions ofelectrolysis:—ND100, 0*04 to 0*05 ampere; voltage, 2 - 3 ;dilution, 225 c.c. ; temperature, 57° C.; time, 6 hours.The deposit of copper weighed 0* 1240 grm., and wras freefrom other metals.
Copper front Manganese.—A solution containing aboutequal amounts of the two metals, with 60 c.c. of phosphatesolution (sp. gr. 1*038) and 10 c.c. of phosphoric acid, waselectrolysed with NI)100, 0*05 ampere ; voltage, 2*5 ;dilution, 225 c.c. ; temperature, 56° C. ; time, 6 hours.Copper found, 0*1236 grm.
Nickel.—A solution of nickel containing 0*070 grm. ofthe metal was mixed with 30 c.c. of disodium hydrogenphosphate solution, and the precipitate dissolved in justsufficient phosphoric acid (sp. gr. 1*347) for the purpose,with a few drops in excess, and the solution electrolysedwith ND100, 0*50 ampere ; voltage, 7—8 ; dilution, 225 c.c.;temperature, 68° C. ; time, 3^ hours. Nickel found,0-0703 grm.
Attempts to separate nickel in this way from manganeseand chromium were unsuccessful, owing to phosphorusbeing simultaneously deposited.
Mercury.—25 c.c. of mercuric chloride solution ( — 0 • 1159grm. of mercury), 30 c.c. of the phosphate solution, and 5c.c. of phosphoric acid were electrolysed with ND100, 0*04ampere; voltage, 1*6; dilution, 175 c . c ; temperature,50° C.; time, 4 hours. The precipitated mercury weighed0-1162 grm.
Mercury from Zinc.—A solution of mercuric chlorideand of zinc sulphate containing about equal amounts of themetals, was mixed with 60 c.c. of the phosphate solutionand 10 c.c. of phosphoric acid, and electrolysed with ND10Q,0*01 ampere ; voltage, l f 5 ; dilution, 175 c.c.; temperature,60° C.; time 4—5 hours. The mercury deposited weighed0* 1163 grm., and was free from zinc.—C. A. M.
Alkali Chlorides, Electrolysis of. K. Kellner.angew. Chem. 1899, [45], 1080.
See under VII., page 45,
Zeits. f.
PATENTS.
Electric Batteries. [Fused Electrolyte.] W. S. RawsonLondon. Eng. Pat. 24,570, Nov. 22, 1898.
IN a voltaic battery operating with fused materials, thelatter are heated by introducing combustible gas or vapour
THE JOUBNAL OF THE SOCIETY OF CHEMICAL INDUSTRY. rJan. si, woo.
under pressure with a regulated quantity of oxygen, andcombustion is effected within the cell. The compressingpumps are driven by an electric motor supplied with currentfrom the cell—G. IT. K.
Primary Electric Batteries [Daniell Type']. C. D. Abel,London. From La Societe d'Etude des Piles Electriques,Paris, France- Eng. P a t 2748, Feb. 7, 1899.
BETWEEN the negative and positive electrodes two or moredialysing porous diaphragms are interposed, so as to main-tain in the neighbourhood of the negative electrode as weaka solution as possible of the electrolyte (such as sulphateof copper), in order to prevent the deposit of copper uponthe zinc, while at the same time the electrolyte near thepositive electrode is maintained as concentrated as possible.To assist in weakening the electrolyte near the negativeelectrode, a frame is employed in its vicinity of the samematerial as the positive electrode, with which it is connected,so that a deposit of copper takes place on it.—G. H. R.
Gases and Liquids, Electric Ajyparatus for AutomaticallyRegulating the Physical Condition, suck as Heat, Pres-sure* Hygrometric State, and Density of. JEL Schultz,Berlin, Germany. Eng. Pat. 7144, April 5, 1899.
Ix this electric apparatus for automatically regulating thephysical condition, such as heat, pressure, vacuum, density,or hygrometric state of gaseous or liquid fluids, the indicatorhand of the electric regulator receives a forward motion, and,by means of an intermittent contact with the indicator handof a thermometer, pressure or vacuum gauge, areometer,hygrometer, or similar instrument, is made to complete orbreak an electric circuit, therebv effecting the automaticoperation of a fluid-mixing device, by aid of which thephysical state of the fluid, corresponding to the electricindicator, is being produced or regulated. A descriptionof the requisite mechanism is given, and of a modificationin which the time piece and contact device are omitted, andthe regulation is worked by hydraulic pressure.—G. II. R.
Diaphragms, Porous, for Electrolytic Cells, and Methodsfor Producing the same. [Electrolytic Formation.'] H.H. Dow, Michigan, U.S.A. Eng. Pat. 6687, May 28,1899.
BY this process a two-layered diaphragm is formed byelectrolysing a solution containing sodium, magnesium, andcalcium chlorides, and introducing into the neighbourhoodof the anode a soluble iron salt, whereby the hydrate of iron,calcium, and magnesium are precipitated to form a coherentporous diaphragm, and the calcium and magnesium hydratesare dissolved out of the anode side of the diaphragm by theaction of electrolytic chlorine, the method being carried outwith solutions of such composition that a coherent diaphragmis formed wholly of hydrates in the position where it is tobe used.—G. H. R.
Electrolytic Apparatus. [Mercury Cathode.'] T. Michel,I. W. and H. Richard, Aix, France. Eng. Pat. 11,930,June 8, 1899.
THIS apparatus consists of a vat divided into two compart-ments by a partition, which does not extend to the bottomof the vessel, but which dips into a layer of mercury,rendering the two compartments water-tight. An endlessmetallic band, which forms an intermediary electrode, passesfrom one compartment to the other through the mercury,carrying the anions with it, so that useless reactions areprevented, and the energy which results from the reactions(foreseen and predetermined to take place in the secondcompartment) assist in the electrolytic work.—G. H. B.
Electrical Resistances and Heating Bodies composed ofMetallic Oxides. V. I. Feeny, London. From TheAllgemeine Elektricitats Gesellschaft, Berlin, GermanyEng. Pat. 16,140, Aug. 8, 1899. ' * *
To electrical resistances and heating bodies consisting ofmaterials strongly contracted by an incandescence process.such as oxides of iron, manganese, nickel, cobalt, chromium'zinc, titanium, and allied oxides or mixtures of the same anaddition is made of some strongly contracting material suchas porcelain earth, manganese, &c, for the purpose of
augmenting the contracting effect or area, and the negativetemperature-coefficient of the heating body is counter-balanced or compensated for by the arrangement ot areducer or rheostat,—G. H. R.
Galvanic Batteries [Zinc-Carbon]. A. J . Boult, London.From J. Trillet, Paris, France. Eng. Pat. 17,258, Aug.25, 1899.
T H E cell comprises an exciting and depolarising solution,and a positive electrode consisting of two annular groups ofcarbon plates of different diameters, which are united attheir ends by crowns of metal, whilst the negative plate isformed by an annular cylinder of zinc standing in an annularporous vessel with double walls, which is placed betweentwo groups of the positive electrode; or the arrangement maybe reversed, one of the zinc cylinders being in the centre,and the other round the outside of the porous pot.
—G. H. R.
Chemical Electrical Excitants. J. Post, New York, U.S.A.Eng. Pat. 22,384, Nov. 9, 1899.
THK excitant is composed of pulverised charcoal, glucose,hydrochloric acid, and sucrose, in approximately equal parts,and water 98 per cent.—G. H. R*
ACCORDING to an official report of investigations made byMilliau for the French Ministry of Agriculture, u LoucMuc "-seed oil is derived from the seeds of a tree found inAnnam, 36 per cent, of oil being extractible by petroleumspirit. The oil is highly coloured, very viscous, and isreadily dissolved by the usual solvents, especially byalcohol, with which it is miscible in all proportions, thusdiffering from all other vegetable oils except castor oil andcotton-seed oil. The fatty acids solidify at 12-5° C , theyield of glycerin is 9 • 02 per cent, and the iodine value is87—approximately that of olive oil and the oils fromcruciferous plants. Apart, however, from its solubility inalcohol, the oil does not exhibit any special characteristicswhich would distinguish it, for technical or commercialpurposes from colza and similar oils,—C. S.
Butter-Fat, Chemistry of Rancidity in.—///. C. A.Brown, jun. J. Amer. Chem. Soc. 1899, 21 f i l l #97«i
I N studying the effect of rancidity on the chemical andphysical constants of butter-fat, the author only madeexperiments under the conditions of warmth and exposureto light and air most favourable to the production ofchemical change, and did not attempt to isolate thecompounds formed.
The table ^iven at the top of next page shows the change inthe composition of four different samples brought about byrancidity. Of these, sample No. 1 was exposed for threemonths to the influence of light and air in a cold roomduring winter; a represents the lower unoxidised and un-altered portion; b the upper part, which was bleached, andhad an abnormal taste and smell. The other three sampleswere allowed to become rancid in a warm place', beino-freely exposed to air and light. * to
From these and similar results, the author finds that withthe advancement of rancidity there is a decided increasein the acid, saponification, acetyl, and Reichert values • islight increase in the ether value; and a decrease in theiodine value and percentages of insoluble acids andglycerin. The increase in the ether value is attributed tothe presence of the aldehydic bodies formed, and to tliodecomposition of these into acids by the alcoholic potassiumhydroxide. * m , u
As regards the physical characteristics, it was found thatthe specific gravity, which ranged from 0-9050 to 0-9102a t if*5 C - i n f r c s h b u t t e r-fat , was considerably increased onbecoming rancid, and then varied from 0*9195 to 0-9*no
In the earlier stages of rancidity, the melting pointshowed a slight increase, ranging from 0-1° to 1 -0° C l
Jan. si, loou.] THE JOURNAL OF THE SOCIETY OF OHEMIOAL INDUSTRY.
Butter-Fat. Condition. Acid Value. Saponification
Value.
\a
26
36Aα46
PreshRancid1
EreshRancid (1 month)FreshRancid (2 months)"FreshRancid (S months)
0'451*220*507*090*55
11*730*51
14*80
229'9232-3223*9233232217225245
76703
Ether Value. Iodine Value.
229*5231*1223*4220232286225230
1015
33*9329*9634*4928*6929*5619*7634*9222*55
Acetyl Value.Insoluble
Acids. Glycerin.
4'87'63*5
10-94-1
15-18-8
18*0
Per Cent.87'2086*8088*9685*0686*4180*4288*4681*15
Per Cent.12*5412*4012*2112*0212*6912*8512*3311*67
in some cases the rancid fat had a double melting point.One sample, for example, melted at 24*2° C , and, afterkeeping the temperature at this point for a few minutes,solidified, and did not re-melt until 33*4° C. Samples of agreater degree of rancidity did not show this phenomenon.They usually melted at from 22° to 24° C, hut did notbecome perfectly clear until the temperature reached 35° to40° 0. The author considers that this may explain thepeculiar semi-fluid consistency acquired by rancid fats, andis probably due to the presence of two classes of decom-position products of different melting points, such as fattyaldehydes and oxy-acids.
The mean critical temperature of solution (Crismer, thisJournal, 1897, 70) was found to be 57° C. in the case offresh butter-fat, whilst, rancid fats gave from 45° to 50° C ,according to the degree of acidity.
The mean refractive index determined with the sodiumlight in a Pulfrich refractometer at 30° C. was 1*45897 forfresh butter-fat and 1*45987 for rancid butter-fat. Thespecific refractive powers calculated from the formula
—-~ (in which N represents the observed refractive index
and D the specific gravity) were 0*50292, and 0*49677 forthe fresh and rancid fat respectively.
As was to be expected, there was a marked decrease inthe calories of the combustion of the fat after becomingrancid, of which the following case is an example :—
Rape-seed Cakes, Volatile Mustard Oils from VariousCommercial. G. Jorgensen. Landw. Vers. Stat. 52,269.
See under XVIII. A., page 65.
Cotton-seed Oil, Becchi's and Tfalphen's Tests for. I5. N.Raikow and N. Ischerweniwanow. Chem. Zeit. 1899,23, [97], 1025.
See under XXIII., page 73.
Acetyl Value, Meaning of, in Fat Analysis. J . Lew-kowitsch. Analyst, 1899, 24, [285], 319.
See under XXIII., page 74.
PATENT.
Fat and other Constituents from Animal Carcases, Impts.in the Process and Apparatus for Extracting. A. vonPodewils, Munich, Germany. Eng. Pat. 20,575, Oct. 13,1899.
"IMPROVED process for separating animal carcases intoconstituent parts, in which the quantity of heat required
for the process is transferred to the carcase material byliquid [such as water], repeatedly heated in a special vesselto over 100° C, and continuously or intermittently ledthrough the substance.,,—A, C, W.
XIH-PIGMENTS, PAINTS; RESINS,VARNISHES; INDIA-KUBBEK, Etc.
040—PIGMENTS, PAINTS.
PATENTS.
White Lead, Drying. The East Ferry Road EngineeringWorks Co., Ltd.; F. S. Tuckett, Locke, Lancaster; andW. W. and R. Johnson and Sons, Ltd., and E. M. John-son, all of London. Eng. Pat. 24,211, Nov. 16, 1898.
A CLOSED apparatus is described for drying white lead bymeans of a current of air heated to about 100a C. Thevessel consists of a cylindrical chamber containing a seriesof horizontal trays, which are supported and capable ofbeing revolved by a vertical shaft driven by any suitablemotor. Hot air is introduced into the vessel at one sidefrom a shaft, openings being provided at a level with eachof the trays; on the opposite side is another shaft whichserves for the escape of the air, while the lower part thereofis employed to remove the dried pigment. A set of scrapersis fixed in such positions that they collect the material fromthe trays and throw it into the outlet; during the desiccationthey are kept out of gear by external clutches. The traysare loaded with the damp white lead through lateral doors,which are afterwards closed; and the whole machine enablesthe pigment to be dried and run into casks, &c, withoutmanual labour. Two or more of these chambers may beworked in rotation with the same current of hot air.
—F, H. L.
White Lead; Apparatus for Use in Dicing. H. C,Webster and T. French, Glasgow* Eng. Pat. 26,434,Dec. 14, 1898.
A BRICK chamber, heated with flues in the usual manner,is fitted up horizontally with rails on which small truckscan travel, the rails being placed side by side across thewhole width of the chamber, and also at different levelsfrom top to bottom. Apertures in the front wall providedwith sliding doors permit access to the different " sidings/,
and outside is arranged a hoist and turntables to bring thetrolleys filled with moist white lead under a neighbouringshoot in line with the several sets of rails. When thematerial is dry, the same hoist serves to lift the trucks onto the top of the chamber, where they run along anotherrailway, and finally empty themselves by tipping in someconvenient situation. By this device human contact withthe dusty pigment is avoided.—F. H. L.
White Lead; Process for the Manufacture of, and for theRecovery of Silver in said Process. A. C. J, Charlier,Glasgow. Eng. Pat. 552, Jan. 10, 1899.
I F noi etallic lead be heated to a temperature just below itsmelting point in a current of moist carbonic acid, a basiccarbonate is formed directly, and can be collected in suitablevessels. Any description of shallow pan is employed tohold^ the metal, which is fed in, in the liquid state, asrequired; the pan is maintained at about 427° C. by meansof a fire underneath, and moist carbon dioxide is blownthrough the mass. The proportion of hydroxide in the
56 THE JOURNAL OF THE SOCIETY OF CHEMICAL INDUSTRY, [Jan. 31,1800,
white lead depends primarily upon the temperature ofoperation. By cleaning out the pan at intervals, any silverin the metal is recovered; but care must be taken that theheat does not rise sufficiently to volatilise the latter.
—F. H. L.
Iron Oxides, Process for Obtaining. H. J. Haddan,London. From A. S. Eamage, Cleveland, Ohio, U.S.A.Eng. Pat. 21,224, Oct. 24, 1899.
SULPHATE of iron is freed from its water of crystallisation,then mixed with about 20 per cent, of magnesia, placed in akind of Leblanc soda furnace, and heated to dull rednessin a partial vacuum till the reaction is complete, andfor a time varying between 2 and 12 hours, according tothe shade of the desired product. The mass is finallyground in water to separate the pigment from the mag-nesium salt. In order to obtain the deeper shades of red(Indian- or purple-reds), 2 to 10 per cent, of sodiumchloride are added to the mixture ; and for the manu-facture of the cheaper grades of Venetian red, the purervarieties of magnesia are replaced by ground or calcineddolomite. Great stress is laid on the use of a partialvacuum within the furnace, which permits the furnaeingto be carried out at a lower temperature and more rapidlythan heretofore.—F. II. L.
Soot or Lamp-Black from Tar and other CarbonaceousSubstances; Manufacture of G. Wegelin, Kalscheuren,Germany. Eng. Pat. 22,337, Nov. 8, 1899.
THE waste heat given off in burning tar distillates is utilisedfor heating the tar distilling apparatus, whereby, on the onehand, the cost of fuel is saved, and on the other hand, thecombined working of the processes of tar distillation andsoot or lamp-black production is effected automatically bycausing the distillation products to flow either entirely orpartially into a receptacle for their combustion to form sootor lamp-black.—D. B.
Fireproof Paint or Composition. A. J. Boult, London.From P. Carre, Paris. Eng. Pat. 25,275, Nov. 30, 1898.
FOUR to 8 parts of boric acid, 15 to 50 parts of ammoniumsulphate, chloride, and [or] carbonate, and 1 to 5 parts ofborax are dissolved in 100 parts of water ; the mixturebeing used at a temperature of 70° or 80° C. to renderfabrics, &c. fireproof. When it is desired to employ thecomposition as a distemper as well, the solids are dissolvedin a mixture of " 100 parts of water and 50 parts of hideglue," and pigments are added as desired. "The aboveingredients" can also be incorporated with pigments andlinseed oil so as to form an oil paint.—F. H. L.
Fire-proof Compositions for Painting or Covering theSurfaces of Wood or other Materials. H. V. Simpsonand The British Non-inflammable Wood Co., Ltd.,London. Eng. Pat. 345, Jan 6, 1899.
FIRKPKOOF paints in which the essential ingredient (asbestos,&c) is simply non-inflammable, have the defect of injuringthe appearance of the pigment added; those in which theessential ingredient (ammonium sulphate) volatilises by heat,tend to form blisters and leave part of the material un-protected. By combining the two classes together in onecomposition, these defects are said to be avoided. 2 oz. of"silicate powder/, 2 oz. of borax, 1 oz. of ammonium phos-phate, and 1 oz. of sodium chloride are ground in oil andmixed with 30 oz. of either zinc white or white lead paint.Another formula consists of u silicate powder,,, 2 oz. • borax'H oz.; aluminium^ hydroxide, 1 oz.; ammonium phosphateand sodium chloride each \ oz.; to be used as before.Either composition may be tinted with any desirable pig-ment ; and as the lead paint has considerably greater fire-resisting qualities than that made with zinc white it shouldbe employed wherever possible. The ammonium phosphateis apt to cause slight lumpiness, and can be replaced byammonium chloride ; the sodium chloride is omitted forfine work lest it produce efflorescence. As a distemperwhitewash is substituted for the oil paint, 2 oz. of size and2 oz. of linseed oil being added to make the material adhereThe silicate powder is obtained by pulverising ordinary slagwool.—F. H. L. b
Oil Colours [Matt Surface Paints-], Process for theManufacture of. A. Turski, Warsaw. Ung. Pat. 11,95/,June 8, 1899.
ORDINARY glossy oil paints are not suitable for applicationto ceilings and walls, because the reflections they^ producemask their proper effect from certain points of view. Bymixing with an oil paint, 20 to 40 per cent, of kaolin in finepowder, and 20 to 30 per cent, of turpentine, a perfectlymatt-surfaced material is produced, which may be usedinstead of a water distemper, or for the staining of commonwall-papers. The latter can be fixed in position, as usual,with paste $ or the colours may be applied to fabrics. Theresults are much more permanent than when the pigmentvehicle is size.—F. H. L.
(B0— RESINS, VARNISHES.PATENTS.
[Waterproof Insulating, Sfc] Compositions having as aBasis Oxidised Oil or Oxidised Oil and Fibrous Material,Manufacture of C. J. Grist, London. Eng. Pat. 25,286,Nov. 30, 1898.
SLIGHT modifications are described in the processes recordedin Eng. Pats. 21,742 and 22,574, 1895 (this Journal, 1896,284 and 278). The operations of moistening the fibre withboiled oil, draining in a centrifugal machine, and drying inthe air, are repeated six or ten times ; or the fibres aresprinkled with oil as they lie in the hydro-extractor.According to the purpose for which it is required, thecomposition may be mixed with more or less powderedsulphur, any indifferent loading material, resin, gutta-percha,&c—F, H. L.
Varnish, Manufacture of A. J. Smith, Greenwich.Eng. Pat. 2848, Feb. 8, 1899.
LINSEED oil and the selected resin are heated together underpressure in a closed vessel to a temperature of 150° C. orhigher, if necessary, for several hours, and the product iscooled, mixed with driers, turpentine, &c, as usual. Thereis no loss of material by volatilisation, and no unpleasantodour.—F. H. L.
(C\)— INDIA-RUBBER, &c.
Almeidina Rubber in Portuguese Africa. Bd. of Trade J .Jan. 4, 1900.
H.M. CONSUL at St. Paul de Loanda states that one of themost interesting articles of export from Angola is therubber or gum called " almeidina." This commodity hasalready been referred to in previous consular reports fromthis district, in one of which (Annual Series, No. 1105 for1892, C. 6812) it is spoken of as having been submittedto experiments which proved, at the trial, commerciallyunsatisfactory.
To-day, the product would seem to have a future of somepromise, for it is already quoted as being worth from Id. to8d. per lb. on the London market.
Almeidina, or Euphorbia or potato gum, as it is various^termed, is the juice of the plant Euphorbia tirucalli. Thisshrub is a weed in the maritime districts of Angola, and itis to be met with on every hand.
Wherever around the city of Loanda there is a patch ofarid land there the Euphorbia tirucalli flourishes greenand fresh all the year round, its finger-like stems teemingwith a sap which flows at the slightest bruise or puncture
The juice is extracted by cuts made in the branches 7aplant of E. tirucalli appears generally as consisting onlyof branches, which in most cases entirely conceal theparent stem) ; the resin flows quickly in a milky-colouredfluid, which, for trade purposes, is boiled until it hardensIt is then made into balls and put in the sun, and these*when ready for export, somewhat resemble it is said insize and colour, an ordinary potato. This article has beenknown m Europe for several years, but hitherto dealings init have proved unprofitable. °
The export of almeidina amounted to 72 748 kiln* in1897 valued at the.Angola^Custom houses'at 3 , T l ^ Sreis (5o6/ 15s 10d) which would represent a declaredvalue ot less than id. per ib. Of this quantity 85940
Jan. si. woo.] THE JOURNAL OF THE SOCIETY OF CHEMICAL INDUSTRY. 57
kilos, were shipped from Mossamedes, 32,215 kilos, fromBenguela, and 4,593 kilos, from Loanda.
The 1898 returns show an increased export amounting tonearly 100 metric tons (99,682 kilos.), valued at 4,905,933reis, of which Mossamedes contributed 54,710 kilos, of avalue of 2,755,535 reis. I t is probable the present yearwill see this amount increased.
Caoutchouc Cuttings, Utilising, in the Preparation ofRubber Solutions. ~- Caselmann. Kev. Prod. Chim. 2*[22], 339.
T H E cuttings, reduced to fine powder, are dissolved inphenol by heating in a closed, jacketted vessel or autoclave,the quantity of solvent varying from 2—3 times the weightof rubber employed.
The temperature required ranges between 120° and 125° C.according to the quality of the cuttings, and the pressure upto 4 atmospheres.—C. S.
PATENTS.India It ubber and Allied Products, Apparatus for Treating
Latex for the Separation of T. Christy, London. PromJ. Hart, Trinidad. Eng. Pat. 26,093, Dec. 10, 1898.
THE latex is agitated with water, dilute spirit, or othersuitable liquid in a cylindrical vessel, the blades of thestirring device being so constructed as to force the substancedownwards through a piece of wire gauze, which acts as afilter, and which forms the bottom of the apparatus. This isclamped on the top of a receiver full of water into which thefiltered juice passes, and in which a current of water ismaintained in an upward direction. Near the top of thelatter an overflow is provided to permit the escape of thepurified latex, whilst, a cock is fixed at the bottom to allowany solid matter that passes the sieve to be removedperiodically.—Y. PI. L.
Gutta-Percha, Composition to serve as a Szibstitute for.H. Schneider, Stnisburg, Germany. Eng. Pat. 19,464,Sept. 27, 1899.
THIS substitute is composed of asphaltum, 45 per cent.;resin, 40 per cent.; turpentine, 10 per cent.; and liuseed oil,5 per cent.: mixed together and boiled.—Y. H. L.
XIV — TANNING, LEATHEE, GLUE, SIZE.Mangrove Bark. Leather Trades' Review, 32, [713], 1090.SKVERAL varieties of mangrove bark have already beenimported from the German possessions in East Africa.Mangrove bark containing from 35 to 40 per cent, of tanninis now being sold in Germany at from 5/. 10.s\ to 6Z. per ton.It is, therefore, one of the cheapest tanning materials ofcommerce at the present time. The bark is analysed inAfrica, and parcels with less than the average tannin con-tents will not be shipped. Certain qualities contain as muchas from 46 to 54 per cent. The leaching of the bark is saidto be easily effected, and the action of the extract upon thehide is exceedingly rapid. The bark imparts a reddish colourto the leather, and hides tanned exclusively with it have theappearance of Valdivia leather. The colour may, of course,be improved by the addition during the process of lightercoloured tanning materials. The bark may be used forthe tannage of harness and upper leathers, or in combinationwith other materials for the tanning of sole leather. Forthis purpose the following proportions are recommended: —40 parts of fir bark, 20 parts of oak bark, 30 parts of man*grove bark and 10 parts of mimosa bark. When the barksare mixed in this manner, a leather which is of a good colourand quality is produced.—J. G. P.
Tanning, Electricity in. J. Buse. Industrie Electrique ;through Leather Trades' Kev. 32, [713], 1077.
THAT the electric current acts upon hides and skins is anincontestable fact. Thus, if a hide which has been soaked,be placed in a saline solution which is being traversed by anelectric current, the salts will be rapidly absorbed by thehide.
In 1849 Grosse made use of galvanism in the tanning ofleather. Zinc plates were employed for conducting the
current; they were plunged into a vat containing the hidesto be tanned, and from time to time, the liquor wasstrengthened with fresh tanning material Ten years laterWard passed a current through an ordinary tanning vat. In1861, liebu, finding the electric current and tannin insuf-ficient, added metallic salts to the liquor. In 1874,De Meritens, at Petersburg, introduced his method in over600 tan pits. At the bottom of each was placed a bed ofcarbon, which constituted the positive electrode ; over thisthe hides, separated from one another by intermediate layersof tan, were placed, and upon the top of all the zinc cathode.The two electrodes were then connected with the respectiveterminal screws of a dynamo. This is an exceedinglysimple arrangement, which any tanner could use, asit is now common property. Two years later Messrs.Gaulard and Kresser proposed another system • plates ofcarbon and hides were placed alternately in the liquor; thecurrent conducted bv the carbon plates traversed the con-tents of the vat, and made its exit by an electrode speciallyfitted up for the purpose. Leather tanned by this methodwas exhibited at the Inventions Exhibition in London in1885. The quality of the leather was perfect, but it did notmeet with due appreciation.
Recently, two new systems of electric tanning have beenintroduced, one by Messrs. Worms and Bale, and theother by Mr. Groth. The Worms and 13ale system in-volves the use of an immense drum mounted upon anaxis, around which it rotates. The hides are suspendedinside from various parts of the circumference ; the drum isencircled by electrodes, aud filled within, up to two-thirds ofits height, with tanning liquor. Groth's apparatus consistsof a rectangular vat 2 metres long by 1 • 5 metres broad and1*6 metres in depth, which is furnished with a frame fromwhich the hides are suspended : this frame is mounted upona moveable carriage to which a backwards and forwardsmotion is imparted. The strength of the current to beemployed is one of the difficulties of all systems of electricaltannage, and authorities differ, giving figures varying from1 to 30 amperes. The writer would restrict it to front 2 to4 amperes, and for density a would give the figures 0*035to 0*001 ampere per square centimetre of the transversesection of the vat." The resistance of a vat of the dimen-sions mentioned when employing a current of 1*3 to 2*3amperes, and a liquor at 9° C. of a density of 1 M)l, whichis equivalent to from 3 to 4 per cent, of tannic acid, wouldbe 8*7 ohms. If the current be passed through a liquorin which no hides are suspended, no diminution in thequantity of tannin is noticed. Deducting 1*6 volts forpolarisation, the quantity of the current expended in theliquor amounts to 36'8 volts. As a current of 2 amperesdecomposes in the space of one hour, only 0*675 ^rm. ofwater, the effect of electrolysis is unimportant, and neednot be taken into account, since throughout the wholeoperation not more than 1 grm. of hydrogen is produced.In the rectangular vat, when the hides are immersed in it*the diminution of the quantity of tannin per hour equals0-533 per 10,000 parts, that is with the use of the electriccurrent and mechanical agitation. Without these the lossof tannin amounts to 0-338, thus conclusively provino- thatelectricity combined with mechanical agitation acceferatesthe absorption of the tannin to a very considerable extentHides subjected to electrical tannage do not absorb auniform quantity of tannin each day; it is found that theabsorption of tannin ceased altogether after the 14th davand during the first five days the quantity absorbed wasrelatively large. In the Worms' and Bale system theweight to be moved by the engine is as follows :—The drum4,000 kilos.; water, 9,135 kilos.; tanning materials1,522 kilos.; turpentine, 9-9 kilos.; hides, 1,015 kilo*"'making about 15-8 tons. In the rectangular vat t Ware only about 1,500 kilos. The writer discusses thefollowing three questions :—In the electric tannage is it thoturpentine, the current, or the mechanical agitation whiohaccelerates the tanning? He states that the turpentineplays only a secondary part, and is not alwavs employedIt only facilitates the expulsion of the fatty" matters contamed in the pores of the hide, and possibly adds Xsuppleness of the finished leather. As regards ethe electro-capillary phenomena here play an iDart, and it may be said that the modification?} the
58 THE JOURNAL OF THE SOCIETY OF CHEMICAL INDUSTRY. [Jan. si. woo.
tension of the surface of the hide resulting from itspolarisation are the causes to which may be attributed theaccelerated penetration of the tannin into the interiorportion of the hide. In a word, in order to make goodleather quickly, recourse must be had to the aid of theelectric current; therefore, the tannage of the future willbe electrolytic. The effect of mechanical agitation must notbe ignored. Its object is to maintain the bath in a state ofperfect uniformity as regards strength of tannin, and tocontinuously bring the hides in contact with fresh tanningfluid.
G. D. Burton has adopted a system of electric tannage, inwhich vats are arranged with paddles so as to protect thehides from all possible contact with the electrodes, whilst atthe same time the liquor is kept in a state of agitation.In conducting the process two other points are deserving ofnotice, viz., the depilation of the hides and the leaching ofthe bark are effected also by means of electricity. In thedepilating process the hides are placed in a shallow rect-angular vat containing a solution of lime and zinc. At oneend there enters a cathode of lead and at the other an anodeof carbon. Burton employs a difference of potential offrom 16 to 20 volts, and tans calf skins in two or three days,cow hides in 12 days. The leaching of the bark is effectedin 30 minutes. It is placed in a rectangular vat filled withwater, and an extremely strong electric current is thenpassed through the mixture, which rapidly raises the waterto boiling temperature, at the end of which time the barkis found to be completely exhausted.—J. G. P.
Tanning with Sulphate of Chromium. J. Krutwig andM. Dalimier. Rev. Universelle des Mines, 48 , [3], 23.
THIS is a preliminary notice of a research undertaken toascertain if " chrome " tannage is based on a chemicalreaction between the skin and the tanning matter, or if itbe due to absorption.
Pieces of hide, carefully washed after the liming process,were suspended in solutions of chromium sulphate of variousstrengths, made hy diluting a solution of 700 grms. ofchromium sulphate in 5 litres of distilled water. The firsttable gives the composition of the solutions. The trialslasted 10 days, temperature 18° C.
Table II . shows the results obtained.in the residual liquor was unchanged,
showing that the sulphate had been absorbed without de-composition, it was also uniformly distributed in the skin.
Washing the skins in distilled water for three daysremoved no chromium sulphate. On washing for two hoursin water at 100° C, none of the salt was dissolved, nor did theskin gelatinise.
Table III . shows the influence of time on the absorption*
The relation SO;Cr.
TABLE III.
Solution I,
Weight I Weightof Dry ; of O 2 0 ; iSkin. Absorbed.
Jan. 81,1900.] THE JOUENAL OF THE SOOIETY OF OHEMIOAL INDUSTRY,
Table IV, shows the results of experiments to determinethe limit of absorption of the skin for chromium sulphate.This is attained after 30 days. The chromium sulphateabsorbed after 10—15 days is given up again on washingwith water; the excess exercises an injurious influence onthe skin, causing it to undergo slow decomposition. Theauthors conclude from the results of the investigation, thatthe chromium sulphate is absorbed by skin without decom-position and is retained by an unknown force which Knappcalled surface attraction.—J. T. W.
Leather, Examination of. T. Palmer and M. Willenz.Ann. Chim. anal. appl. 4 , 297—301.
T H E authors sought a method for valuing leather by theexamination of a piece when actually fit for use. Theybelieve they have found a measure or standard in therelation of volume to weight. Circular pieces of about17 mm. diameter are cut uniformly from all parts of theleather, the pieces weighed and their volume ascertained.100 c.c. of a good leather weighs more than 124 grnis., thevalue of the leather sinks with this number, until with badleathers, 100 c.c. weighs 85—87 grms. Leather weighing110—115 grms. should be regarded with suspicion.
On the contrary, bad leathers show a greater capacity forabsorbing moisture, and the authors believe thev have dis-covered a definite relationship which may be quantitativelyapplied, and this problem they are now endeavouring tosolve.—A. S.
Leather Making, Chrome Process in. Leather Trades' Rev.32, [717], 1165.
Splits and the Chrome Tannage. — Hides intended forupper leather and to be chrome-tanned, should be split onleaving the beam-house in the raw state, the operation beingcarried out with a belt knife splitting machine. The grainscan then be tanned by the chrome process and the splitstanned in bark. Experiments have shown that the lessagitation the hide or skin is subjected to whilst tanning, thefirmer and plumper are the bellies and flanks produced.In using the one-bath tannage on hides, calf and sheepskins, a suspended tannage is considered the best, as thefibres of the hides or skins are not subjected to any poundingor paddling process.—J. G. P.
Upper Leather by the One-Bath Chrome Method^Manufac-ture of. M. Chas. Lamb. Leather Trades' Rev. 32,[717], 1163.
IT is stated that at the present time more chrome-tannedleather is being manufactured in the British Isles than everbefore. Chrome tanning being an " empty tannage/ , aslittle weight as possible must be taken out of the skins inthe early stages of the wet work, otherwise an exceedinglyflat, thin, light-weighing leather will be the result.
" Calf Skins.',—The goods are soaked for from 24 to 48hours until soft and pliable. Salted skins should be soakedlonger in several changes of water. The skins are thenlimed in " plumping limes " for six to seven days, the goodsbeing drawn daily. When unhaired and fleshed they arewell washed in a drum or paddle with a sufficiency of softwater for half an hour, after which they are bated mildly,generally from 8 to 12 hours in a fresh hen-dung batebeing sufficient. They should then be washed in soft water,lightly drenched for two or three hours, and again washed,preferably in the paddle, for about half an hour. Theyare then ready for tanning.
" Box Calf" — In tanning box calf, the author hasobtained the best results from a liquor made of 16 lb. ofchrome alum, l^ lb. of ordinary alum, and £ lb. of iron alum,dissolved in 18 galls, of cold water, mixed with a solutionof 5 lb. of soda crystals in 2 galls, of water. Thequantities given will make about 22 galls, of stock liquor,which will be found sufficient for the tannage of aboutthree dozen medium calf skins prepared as above. Intothe drum or paddle wheel in which the skins are to beentered, a sufficiency of water is added to cover them,adding to the water 20 lb. of salt, together with 2 lb. ofalum for each three dozen calf skins to be tanned. Whenthis is dissolved, the skins are entered and the drum is runfor an hour. A gallon of stock liquor is now added and
the skins run for another half hour, when an addition ismade of a second gallon of the stock liquor; 2 galls, ofthe stock liquor are afterwards added at intervals of anhour. The skins should not require more than 12 hourstannage. The half-used liquor may then be applied to thetannage of a fresh batch. The skins when tanned, andwhilst still Avet with the liquor, are allowed to lie in pileover night; they are then washed in a drum with cold ortepid water and subsequently " boraxed," l£ lb. of boraxdissolved in enough water to cover the goods being sufficientfor three dozen skins. The goods are run in this solutionfor about half an hour, and are again washed in Avater for15 minutes; they are then struck out by machine andfat-liquored.
For a common class of goods, 5 lb. of glucose maybe substituted for the glycerin. The soap, finely sliced,should be boiled in 2 galls, of water until dissolved; theother ingredients are then added, and the whole thoroughlyemulsified. The skins are then placed in a properly-fittedstuffing drum with a sufficiencv of water at 60° C., and thethoroughly emulsified fat liquor added whilst the drum isrotating. The skins are run in the fat liquor until thewhole of it has been absorbed, this generally requiring halfan hour. They are then taken out and laid in pile for a fewhours, drained on boards, and hung up in a stove to drjr.The skins may be kept for any desired length of time intheir present crust state, and improve on keeping for two orthree months. If desired to be immediately finished, theyare damped back in wet sawdust, staked by machine, thenwetted back in hot water at about 60° C. until thoroughlywet, and run in a drum or paddle through liquor made bydissolving 5 lb. of good logwood extract with 2 oz. of washingsoda in sufficient hot water. They are passed through thissolution for two or three hours, starting with a temperature of60° C. They are then taken out, allowed to " sammy," andthen inked with a good curriers' ink. The author has usedthe following preparation with good results :—6 oz. of ferroussulphate, l^ oz. of copper sulphate, dissolved together in7 pints of water, to which is added 1 pint of stale beer. Afterblacking, the goods are topped with a solution of -J lb. oflogwood extract with \\ oz. of Naphthylamine Black 4 B(Cassella) or Leather Black V (Bayer), in 1 gall, of boilingwater. If the blacks be not sufficiently intense, they may bere-topped with \ per cent, solution of Corvoline B (B.A.S.F.).They are then seasoned ; for example, with a mixturecomposed of 4 quarts of logwood liquor, 1 pint of blood,l^ gill of orchil, 1 gill of milk, and <} oz. of prussiate ofpotash, steamed up until the ingredients are dissolved.After seasoning, the goods are hung up in a stove untildry, glazed by machine, staked, boarded up by hand,re-seasoned, dried out, glazed twice round, and againboarded, two ways, in order to produce the well-knownbox-grain, and finally polished with a flannel. If the skinsdo not give a clear face on glazing, the glaze may b<>improved by rubbing the skins with a dilute solution oftartaric acid on the grain surface, then drying and re-glazing.
" Coloured Calf:9—A good tanning liquor may be madewith 16 lb. of chrome alum and 2 lb. of ordinary alum dis-solved in 18 galls, of cold water, and mixed with a solution of8 lb. of soda crystals in 2 galls, of water. The preparation ofthe skin, as well as the boraxing and tanning are then thesame as for box calf. The following fat liquor was foundto give the best results.
Kourlb. of white curd or castile soap are dissolved byboiling in 2 galls, of water; 12 oz. of castor oil 4 oz ofTurkey-red oil and 7 lb. of glycerin are then added, and thewhole thoroughly mixed and emulsified.
The fat-liquoring process is the same as for boxcalfThe skins are dried out, strained, damped back and staked *and then wetted by tumbling in hot water, after which thevare ready to be dyed. ^
"Dyeing of Coloured CaZ/"-Chrome-tanned leathertakes the dye exceedingly well before it has been fatliquored, but this method of working is objectionable
60 'HE•Tan. 3 1 , J100.
because the subsequent fat-liquoring takes the greater partof the dye out of the skin, thus making it practicallyimpossible to dye to shade. The main objection to dyeingafter fat-liquoring is the great amount of dyestuff whichmust be used in order to produce a full shade, particularlywith the acid dyestuffs, as sulphuric acid cannot be added tothe bath. The author, after long researches, found thatchrome leather which had been fat-liquored could be dyedto full shade with the so-called acid dyestuffs in a bath towhich a small quantity of sodium bisulphate had beenadded, and recommends the following procedure.
The dyestuff having been carefully weighed out anddissolved in about 50 times its weight of boiling water, anamount of bisulphate of soda equal in weight to the dyestuffis dissolved in water in a separate vessel. Half of theconcentrated solution of dyestuff is added, together with thewhole of the solution of bisulphate of soda, to a sufficientquantity of water (at 60° C.) in the drum to cover theskins, the goods are entered and the drum started. After15 minutes' running, the remainder of the solution of thedyestuff is added, and the dyeing continued for at least 30minutes longer, or until the goods have attained the depthof shade required. The quantities of dyestuff and bisulphateof soda necessarv for each dozen of skins would be 8 to 10oz., according to the desired depth of shade. The authorgives a list of different dyestuffs which he has found towork well on chrome leather.
After dyeing, the skins are washed in warm water, setout, dried, and strained on boards. If in a suitable condition,they are staked, soft-boarded, and a thin coat of linseedmucilage is applied, the skins being dried out and strained.The following seasoning works well :—
One pound of linseed is boiled with 3 galls, of waterfor an hour, the solution then filtered through canvas ; 1 oz.of gelatin is added, and the boiling is continued untilsolution is complete ; the mixture is then allowed to cool.
The skins being damped with a little milk, the seasoningis applied, after which they are dried out in the stove,glazed twice round, re-seasoned and t.gain glazed, afterwhich they are boarded up from neck to tail in order toraise the popular straight grain peculiar to " willow calf/3
and finally rubbed up with a flannel.If the goods require shaving, it is best to do this after
they have been dried out after fat-liquoring rather thanbefore this process, the knife cutting much better on thefat-liquored skin.—J. G. P.
East India Kips. Leather Trades' Kev. 32, [713], 1085,[717], 1169. (See this Journal, 1899, 1036.)
BKFORK passing the skins on to bateing, there are someminor details which require consideration.
"Grain cracking" is generally caused by the goods beingstocked before they become perfectly soft, the grain bcincrtoo hard or tight. This can be avoided by opening theskins on returning them to the soaks. Thus, the water α-ctsat both sides, and a more thorough softening of the skinstakes place.
"Shrinking" in the necks and shoulders, which sometanners attribute to blood binding, is also caused to a laro-eextent by insufficient soaking, or by not stocking enou<&.This can be remedied by having a constant supply of plentyof tepid water running into the stocks whilst stocking thegoods. In washing through the tumbler the same pre-caution is necessary, plenty of tepid water being allowed torun through the goods for 20 to 30 minutes.
A quarter of a pint of cod oil per stockful must be used,the goods being freely sprinkled at intervals whilst in thestocks, otherwise the friction caused by the stocks is liableto cause damaged grain.
After the skins are carefully washed from the fleshingbeam to rid them from superfluous lime, dirt, &c., they areready for bateing. This is generally carried out in a set ofthree pits, at a temperature of from 60° to 90° F, regularlythrough winter and summer. By this means a constantbateing is produced, and the workmen get the goods into anearly regular and mechanical system, and can thereforewith a little practice, bring them down to the requiredcondition, whereas, with a change of temperature, some arebrought too low, and others not low enough. In making
up a bate, two bushels of pigeon dung, and half a bushel ofhen dung is placed in a tub or half cask, and scalded over-night. The cask is fitted with a loose perforated falsebottom, about two inches from the bottom, the perfora-tions being very fine. Between the original and m thefalse bottom is* placed a bung, so that the bate liquor,when ready, can be run out into the pit it is intended for,the sand and heavy ingredients falling on the bottom, andthe straw, feathers, &c, which remain on the false bottom,being easily removed. When making a bate for the goods,it should be prepared the day before it is to be used,by scalding the dung with water at about 180° F.The kips should be put into the pit at a temperatureof about 85° to 90° F., allowed to remain for two hours,then, if sufficiently low, passed out; if not, time must beallowed to reduce to required " feel/. They are stockedfor about half an hour, using sawdust instead of water.After the goods are stocked, they are washed througha tumbler, allowing plenty of tepid water, and afterwardsare passed through another pit of clean tepid water con-taining about 2 lb. of boric acid. They are sorted outof this pic for the liquors.
The tannage in general use for English East Indiakips is a mixed one, comprising English bark, valonia,gambier, sumach, myrobalans, and mimosa. The composi-tion varies in every tannery, but the largest proportion ofmaterials used are gambier, myrobalans, and sumach. Inthe first place, the goods are placed in a paddle, into whichis pumped the fifth liquor from the handlers ; this is.strengthened with gambier and sumach or myrobalans, forevery dozen kips, 3 lb. of gambier and 3 lb. of eithersumach or myrobalans being added. If the paddles arelarge and will run 300 kips, 75 lb. of gambier and 75 lb. ofsumach or myrobalans are divided into four parts, and eachportion arlded at intervals of 15 minutes.—J, G. P.
Hides, Treatment of. J . Dunn and G. II. James, London.Eng. Pat. 921, Jan. 14, 1899.
T H E hides selected for imitation morocco for bag and port-manteau work are first degreased, then re-tanned and dried.Secondly, scoured with water or a solution of ammonia orsoda, cleansed with a solution of sulphuric acid and water,boarded out, and painted or dyed. They are then pressed'shaved, strained, and dried. After drying, they are seasoned,embossed, and again dried ; and finally, re-seasoned, rolled^and glazed.—J. T. W.
Leather, Manufacture of M. Brumm, O. Srpek, E. Haas,and F. Kornacher, Frankfort-on-Maine. Eng. Pat. 3111Feb. 11, 1899.
SHEEP-skins and " bastard " sheep-skins are quarter or halftanned, and whilst in the moist condition are struck outblacked or dyed, and grained. After this the tanning pro-cess is completed and the leather finished. Or the comple-tion of the tanning process and the finishing may becombined, the leather being coated on the flesh side with asuitable tanning medium and spread out flat for 12 to 24hours. I3y this means a grained leather is said to beobtained equal to the most valuable kinds of leather atpresent known.—J. T. W.
Extracting Tannin from Leather, and Preparing the latterfor Glue-making. K. Brauer, Liineberg, GermanvPat. 10,408, May 17, 1899. ^
T H E tannin is extracted from leather cuttings and waste bvtreating these with ammonia under a pressure of from120—150 lb. to the square inch in the presence of sufficientwater to obtain a 4 0 - 5 0 per cent, solution of tannin Theammonia is afterwards driven off by heat. The remainingtannin in the leather is washed out with warm water andthe skin thus obtained used for glue-making — J T \V
Jim. 3i, woo.] THE JOUBNAL OF THE SOCIEl?Y OF CHEMICAL INDUSTRY.
Hides and Skins, Treatment and Tanning of L. Con-sonno, Como. Eng. Pat. 13,307, June 27, 1899.
T H E hides or skins are unliairecl in drums at a temperatureof 50°—60° (J. by means of a solution of sodium sulphideand soda crystals, or of these salts and lime, the time occu-pied being only ~ hour. To prepare the skins for tanning,they are now washed in clean water and drummed with amixture of 2 per cent, of soda crystals, 0 * 5 per cent, of liquorammonia, and 0*5 per cent, of "benzine " ; or they may betreated with water saturated with carbonic acid gas. Theyare then ready for the tanning proper, which is conductedin drums rotating alternately in opposite directions, andwith tanning extract of 25° B. in quantity not exceeding1,200 grms. for each kilo, of fresh hide. —J. T. W.
Tanning, Improved Process of. G\ S. Dolley and A. E.Crank, Philadelphia. Eng. Pat. 14,775, July 18, 1899.
BADLY tanned skins or skins partially or completely tannedby various towing or tanning agents, such as alum, salt,argol, eggs, flour, vegetable extractives, gambier, and cntch,are subjected to the action of formic aldehyde, preferably insolution, although it may be employed in the state of gas.Three pounds of commercial 40 per cent, formaldehydesolution are used for every 100 lb. of wet hide, the amountof water being just sufficient to keep the skins well wettedin the drum. Sheep- or goat-skins are permeated by theformaldehyde in three hours. The temperature of the bathis maintained at 80° to 120° E. The leather is then washedand is ready for the usual treatment in finishing. Insteadof being treated with the liquid formaldehyde in a drum,the prepared skins may be hung in a closed chamber at atemperature of 110° to 120° F. and subjected to the actionof the gaseous formaldehyde in the presence of aqueousvapour.—J. T. W.
Leather Manufactured from the Intestinal Coatings ofAnimals; Impts. in, and in Gloves Mann fact tired fromsuch Leather. B. Trenckmann, Berlin. Eng. Pat.19,540, Sept. 28, 1899.
THK mucous membrane of animals is tanned or tawed bythe usual methods. Gloves made from such leather, whenmoist, lie close to the skin of the hand, effectually protect-ing the latter against the penetration of infectious or othermatter, whilst not interfering with the free movement of thehand or sense of touch.—J. T. W.
XV—MANURES. Etc.Humus in Soils, and the Percentage of Nitrogen in the
Humus. H, J. Wheeler, C. L» Sargent, and B. L. Hart-well. J. Amer. Chein. Soc. 1899, 21, [11], 1032—1037.
THIS is an account of an investigation of the soil at theKhode Island Agricultural Experiment Station in its naturalstate and under the influence of air-slaked lime. A numberof galvanised iron ash-pails were embedded in soil towithin 2 ins. of the top, a hole being made in the bottom ofeach for drainage, and agricultural tiles placed beneath to jprevent the ingress of surrounding soil water. In each 'of these were placed 154 lb. of subsoil thoroughly mixedwith 100 lb. of surface soil In 1893 and 1894 eachmanured pot received 7*36 grms. of potassium chloride and22 • 07 grms. of dissolved bone-black, these amounts beingincreased to 10 and 25 grms. respectively in the succeedingyears. Whenever nitrogen was added, the amount was atthe rate of 2*65 grms. Gypsum was applied to furnish thesame amount of calcium oxide as the air-slaked lime.Maize was grown in the pots in 1893, oats in 1894, andspring-rye in 1895, the soil for the examination being takensome weeks after the rye harvest.
In the analyses, the humus was determined by extracting20 grms. of soil first with dilute hydrochloric acid, andsubsequently treating it with ammonia, as in the Hustonand McBride modification of the Grandeau method (Wiley's"Agricultural Analysis," I., 327—328). For the determi-nation of the nitrogen in the humus, the .soil was extractedwith a 2 • 5 per cent, solution of potassium hydroxide andaliquot portions of the extract used. The results obtained,
calculated to percentages of dry soil, are summarised in thesubjoined table:—
Ammonium sulphate, cal-cium sulphate (landplaster), at a rate equi-valent in CaO to 4 tonsper acre.
"Without nitrogen and limeAir-slaked lime (4 tons
per acre).Sodium nitrateSodium nitrate and air-
slaked lime (4t tons peracre).
HumusNitrogenin Dry
Soil.
0-1300*1280-133
0*126
0'139
Humusin Dry
Soil.
I Nitrogenin Dry
Humus,
2ft 2723, 24
e, 137,14
0-1290-139
0*1430-133
3'8fi3*933'77
3'63
3T>5
3-753*51
3*933*42
3-373-263-53
3*47
3*81
3'89
With the exception of No. 21, all the pots received thesame amount of potash and phosphoric acid.
From these results it appeared that the addition of air-slaked lime or gypsum caused, in every instance, a decreasein the total amount of humus, but an increase in the per-centage of nitrogen in the humus, even when no nitrogenhad been added (pots 23 and 24).
Where sodium nitrate was used without lime, the per-centage of humus nitrogen was greatest, and the amount ofhumus as great as in the case of the pots containingammonium sulphate. In the author's opinion this mayindicate a storage of some of the nitrate nitrogen withinthe soil in the form of organic matter which can beclassified under the complex term " humus." This mayprobably be due to denitrifying organisms—a view whichreceives support from the facts that the activity of theseorganisms is reduced by lime, and that there were nomarked indications of the storage of nitrate nitrogen whenlime was used.—C. A. M.
PATENT.Distillery Refuse [for Manure], commonly called "Pot
Ale" or "Burnt Ale,'9 Treatment of T. Storer andR. McAlley, Falkirk, Scotland. Eng. Pat. 6348, March23, 1899.
See undei* XVII., page 65.
XVL—SUGAR, STARCH, GUM, Etc.Diffusion Juice [ Sugar'], Purification of. Bull. de 1'Assoc,
cles Chim. de Sucr. et de Dist. 1899, 17 [3], 255—257.From Deutsch. Zuckerind. 24, 35.
ALL the processes for the purification of raw juice consistin the precipitation or decomposition of the non-su«niv
oneleaving the sugar in solution in the purified juice. _ _of these methods give a coefficient of purity greater than92 to 94. B
Diffusion juice treated, on the laboratory scale, by thelime-separation process gave a purity of 95*60, and, aftera previous defecation at 85° C. with 0*2 per cent of limegave 96*76 as coefficient of purity. '
The Steffen separation was now applied on the largescale. After carbonating the diluted unwashed sucrate to0-01 percent, of CaO and concentrating the filtered juicein the laboratory to a syrup, the purity was 96 • 00. Thescum contained 0 • 80 per cent, of sugar.^ The above experiment was made with diluted diffusionjuice ; an experiment with 400 hectolitres of undiluted iuicegave a syrup of purity 96*00. The total loss, howeverreached 0*4 to 0*5 per cent, of the beetroots. In orderto reduce the loss, diffusion was conducted so as to have0-08 of sugar in the exhausted pulp and 0*03 in thediffusion water, or a total loss of 0* 106 per cent, on thebeetroots in diffusion.
THE JOURNAL OF THE SOCIETY OF OHEMlOAL INDUSTRY. [Jan. 31,
After defecating with -| per cent* of lime, the cooledjuice was treated by separation, and a syrup obtained of apurity of 95-51, The loss due to separation was 0* 40 percent, of the beetroots, or a total loss of 0*506,
Although the results are not perfectly satisfactory, theloss is scarcely more than in the ordinary diffusion; and itseems possible to obtain, using 7 to 8 per cent, of lime onthe beetroots, and working slowly enough, massecuites whichwould yield refined sugar directly.—L. J. de W.
Beetroot, Estimation of Sugar in. J. Weisberg. Bull, del,Assoc, des Chim. de Sucr. et de Dist. 1899, 17, [3],237.
See under XXIII., page 76.
Rhumninose : A Saccharose from Xanthrorhamnin* C. andG. Tanret. Comptes Eend. 129, [19], 725.
See under XXIV., page 79.
Starch, New ^ Method for the Rapid Determination qIX Oispo. Ann. Chim. anal. appl. 4, 289.
See under XXIII., page 76.
PATENTS.Sweetening Liquids, Production of P. Porchere, Lyons,
France. Eng. Pat. 7190, April 5, 1899.See under XX., page 70.
Sugar Candy, Process and Apparatus for Manufacturing.H. Flesche, Rheinbrohl, Germany. Eng. Pat. 20,355,Oct. 10, 1899.
THE vessels in which the crystallisation of the massecuitetakes place are cooled in receivers under diminishedatmospheric pressure, whereby the contents are cooledquickly and uniformly, and the formation of invert sugaravoided. A claim is also made for the use of a specialapparatus, which consists of a cylindrical air-tight vesselcalled a receiver, containing the crystallisation vesselssupported on rails, and which can be heated by meansof steam pipes.—J. L. B.
XVII.-BEEWINQ, WINES, SPIRITS, Etc.Maltj Hard and Mealy ; Morphological and Physiological
Phenomena in the Preparation of J . Griiss. Woch. f iirBrail. 1899, 16, [47], 621— 631.
THE kilning process may be divided theoretically into fourphases: (1) The physiological processes still continue inthe green malt, as testified by continued growth, depletionof the scutellnm of carbohydrates, transference of sugar,respiration, &c. (2) At about 44° C. the former cease andenzymatic processes predominate. (3) With rising tem-perature the enzymes are weakened and chemico-physicalchanges are set up, such as coagulation of prote'ids andtransformation of hemicellulofles. (4) Completion of kilning.A hard or a mealy malt may be prepared from one and thesame green malt, according to the conditions: the formerresults from quick kilning without an air current in presenceof moisture during the greater part of the process ; a mealymalt results under conditions which provide for the earlyremoval of the moisture by aeration and an initially slowrise of temperature. In no case could the cause of a steelymalt be traced to incipient gelatinisation of the starchgranules, although the conditions would suggest it. Thesugar-content attains a maximum at the stage when thephysiological work in the corn is most intense. The greatestdifferences, caused by the manner in which the moisture isremoved, in preparing hard and mealy malt, are manifestedwhen the conditions favour the most intense physiologicalwork in the corn. The depletion of starch in the scutellumduring kilning takes place before the death of the embryo.The steeliness of malt kilned with high moisture withoutaeration is caused by gummy substances, which are accom-panied by much reducing sugar, and which result from thehydrolysis of the secondary cell walls of the endosperm. Inthe preparation of hard malt by the above method of kilning,
a decrease of the smaller starch granules and an increase ofreducing sugars take place; the endosperm of such maltcorns is strongly transformed. In mealy malt, on the otherhand, the ratio of the small starch granules to the largeones is comparatively high. The author has investigatedthe behaviour of the enzymes, particularly of " spermase "(see this Journal, 1899, 1042), on kilning in presence ofmoisture and in absence of an air current, and concludesthat under these conditions the malt diastase is devoid ofoxydasic properties, and that the oxydase (" spermase ") isreadily destroyed.—J. F. B.
Yeast, Frequent Errors in the Preparation of Zeits.Spiritusind. 1899, 22, [49], 451—453.
WITH reference to Lange's paper (this Journal, 1899,1143), Polzin remarks on the difficulty in maintaining thetemperature of acidification during the night without atten-tion if small vessels be used; he therefore prefers to uselarger vats of 330 litres capacity. In the evening he heatsthe culture to 62° C. and runs the barrels into a warmchamber, in which the exhaust steam from the pumps andother continuous machinery is discharged, and the necessarytemperature is thus maintained during the whole nightwithout attention.
The mash is saccharified with green malt at a temperatureof 64° C, cooled to 55° C, sown with some acidified mashfrom a previous preparation, allowed to ferment for 20 hoursat the lactic fermentation temperature of 55° C , andsterilised at 75° C. The acidity so obtained, corresponds to1 *9—2'0 c.c. of normal alkali, and the increase in the acidityof the main mash during fermentation is 0 • 2 c.c.
J. Krzyzanowski states that he insulates his yeast vesselsagainst radiation of heat as perfectly as possible, workingwithout a warm chamber. He uses 20 litres of spent washand 1 lb. of rye meal with 10 kilos, of malt when makingup the yeast mash. He finds that the mixture only cools4° C. during the night, and he prefers to perform theheating and cooling with a mechanical stirring worm, andthus obtains 3° of acidity. Henke writes that the necessaryquantity of water should be introduced into the vat, andthe malt should be mixed up with it before adding thepotato mash for saccharification j the heating must beeffected with a closed steam coil to avoid dilution. Themashing temperature should be adapted to the nature ofthe malt. It is comparatively easy to obtain an acidity of1-5°—2-0°, but much more difficult, one from 2-0° to 2*5°.The maintenance of the most favourable temperature of54°- C- and repeated agitation are the chief considerations ;a temperature of 60° C. is the highest permissible limit forthe evening heating.—J. F. B.
Beer Sarcina, Studies on a. F. Sch&nfeld. Woch. furItem. 1899,16, [50], 665—670.
THK ^ present investigations relate to the beer sarcinadescribed by the author in 1898 (see this Journal, 1898, 684).The following conclusions are drawn :—
The addition of lupulin to the beer or the subsequenttreatment with hops considerably impedes the virulence ofthe sarcina, but has only a slight effect on its actualmultiplication. The soft resin of the hops is a powerfulpoison against both the virulence and the multiplication ofthe organism. Beer which has suffered very much fromsarcina sickness, but which has subsequently cleared isproof against further sarcina infection. Carbonic acidunder pressure restricts the development of the sarcinaThe organism grows more quickly and powerfully in beerssuffering from gluten cloudiness than in normal beerLiquids rich in peptones are more favourable to the niulti*plication of the sarcina than liquids rich in amides: bothtypes of liquid, however, are equivalent as regards theV5 f n ? t I V1™ lence.of t h e organism is far more easilyaffected by the sarcina poisons than the actual reproductivepower.—J. F. B, r>^
Albuminoids in Beer, Importance of W. Lo6. Zeits. fiird. ges. Brauw. 22, [38], 499—502.
THE author states that Laszczinsky s method of heatWwort or beer for one hour under 1J atmos. pressure, gives amuch larger proportion of coagulable albumin tifim the
Jan. sif i9uo.] THE JOUEKAL OF THE SOCIETY OF CHEMICAL INDUSTRY. 03
ordinary methods. Further, that no peptonising influenceis exerted on the albumin in mashing; that the advisabilityof low-tcmperaturc mashing is due to the coagulum, whichis formed at boiling temperature and prevents the extractionof the soluble albuminoids, besides retarding the clarificationof the wort. Iα place of the old classification of the albu-minoids, he recommends that of Laszczinsky, viz., coagulablealbumin precipitated under the conditions cited above;albumoses, extractible by zinc sulphate; xanthine bases,precipitable by copper sulphate, sodium bisulphite, andbarium chloride ; and amides, estimated by difference-
Spirits, Continuous Rectification of Crude. W. Anders,Zeits. Spiritusind. 1899, 22, [43], 393—394.
BY the ordinary methods of rectification a sharp separationof the fine spirit from the fore and after runnings is notobtainable by dephlegmation. According to the author thisis due to the violent ebullition, which causes the particles ofvapour to have a high molecular velocity and brings abouta most intimate molecular mixture of the constituents. Butif the spirit be passed over heated surfaces in extremely thinlayers, and lie allowed to evaporate rather than to boil, alooser combination is obtained, which is readily separatedin the dephlegmator. This principle was recognised in theKilling-Oppenhehner system, and the author here describesan apparatus for continuous rectification invented by M.Strauch, of Neisse, on somewhat similar lines, which turnsout all the alcohol in the form of first-quality spirit. Thecrude spirit enters the reservoir S by the pipe z, and flowsthrough S1 and h into the dephlegmator C2, where it coolsthe light vapours and being warmed in its passage, it isthen conducted into the top of the first evaporator A^where it trickles over steam-heated surfaces and the light
vapours ascend through the column E 2 and are dephleg-mated in C The light vapours pass through Vx and arecondensed in Kl9 from which the fore runnings are drawnoff by way of V->, V-4, and V4 with a vapour-cap l4. l h espirit, freed from light constituents, passes into theethyl alcohol separator Ax where it again passes over hotsurfaces in a thin layer and the vapours are treated inthe column K b which is filled with perforated plates and anumber of slanting plates, so arranged that the ascendingvapours get through without having to come much in con-tact with the descending heavy liquors. The spirit vapoursare freed from the after runnings in the dephlegmator Cx
and are condensed in Kx and drawn off by way of r3, r4, andr5. The after-runnings pass4down the pipe n\ through thecooler Ko and are collected in the reservoir N whence theycan be pumped through a and the spirit washed out, or ifthe quantity of fusel oil is large, it can be mixed with waterand separated in the vessel X. The heating surfaces ofA and A2 are corrugated and steam enters at d{ and d2;Wx, W2, W31 and W4 are the pipes through which the coolingwater flows'. The fine spirit contains from 94*62 to 94-97per cent, of alcohol by weight and is of the best quality.
— J . F . B.
Rum, Manufacture of, at Guadeloupe. C. Pairault. Bull.de 1'Assoc, des Chim. de Sucr. et de Dist. 1899, 17, [ 3 ] ,246—255.
T H E name rum is more particularly reserved for the productof the fermentation and distillation of cane juice, whilsttafia is obtained from cane molasses, but these distinctionsare not absolute. True rum does not reach Europe*Although its manufacture at Guadeloupe is an importantone, the production, 1,800,000 litres per annum, does notsuffice for the local consumption (2,500,000 litres), thedifference being made up with molasses " tafia/.
There are two other kinds of rum made for special con*sumers, but now of no commercial importance j (1) thatprepared from boiled juice, and (2) that from the syrupdrained from sugar, produced by boiling the juice over anaked fire. This syrup has a very different flavour frommolasses or factory syrup.
True rum is made chiefly in small distilleries in thedistrict of the Basse-Terre, the amount produced in eachvarying from 150 to 600 litres per day.
The production of tafia, on the (contrary, is confined toa few large factories in the neighbourhood of Pointe-zt-Pitre. These factories manufacture sugar in considerablequantities, and distil their molasses. The factory Dar-boussier (Souques et Cie) produces no less than 40,000 to45,000 litres of tafia of 60° per week. The total productionof tafia is three million, litres, at least three fourths of thisamount being exported.
The rum factories consist of a mill of three horizontalmetallic cylinders, arranged in a triangle, and driven by awater-wheel, the power being 16 to 18 horse-power. 1,000kilos, of canes give only 600 kilos, of juice, thus leavingabout 10 per cent, of the total sugar in the bagasse. Thebagasse contains 53 per cent, of water. It is dried for useas fuel. Some distillers sprinkle it with water or hot-spentwort and subject it to a second pressing. Even then 6 percent, of the sugar is lost.
The fermentation is carried out in open, truncated woodenvats, 1 metre in diameter at the top, and of a capacity of1,200 litres. The juice has a density of 1*075, or 10° B.,which is reduced by the addition of water and spent wortto 1-045 or 1-050 (6° to 7° B.), the proportions being:wort, 800 litres; water or seconds juice, 200; spent wort200 litres. The acidity of the juice is 0*70 per litrecalculated as H2SO4, that of the spent wort being 6 to 7*5and the wort 2 grms. per litre. The juice contains about17 per cent, of fermentable sugar; the wort, 11 to 13-5 •and the spent wort, 2 to 3. The density of the spent wortis 1-008. It is probable that the spent wort plays animportant part in influencing the aroma of the distilledproduct. It is generally agreed that it makes the fermenta-tion proceed regularly, and all distillers use it.
The surrounding temperature being 25° to 28° Cspontaneous fermentation quickly sets in; in 12 hours thevat is m full work. Fermentation lasts from three to four
(34 THE JOURNAL OF THE SOCIETY OP CHEMICAL INDUSTRY [Jan. 31,1900.
days, the temperature rising to 37° or 38°, even occasionallyto 40° or 41°, without appreciably affecting the yield. Theamount of acidity increases to 5 or 6 grms. of HoSOj perlitre. The theoretical yield is 13-1 x 0-(il = 8-2 ofalcohol by volume per 100 c.c. of wort. Actual yield atSalleron 7' 1, or a loss of 1 • 1 with normal acidity. Whenthe fermentation is finished and the wort siphoned off, thedeposit of yeast is run to waste by removing a plug, andthe vat well washed with water, but not brushed out, unlessthe fermentation becomes abnormal, when the vat is brushedout and cleaned with milk of lime. Most distillers addabout 0*5 kilo, of ammonium sulphate to each vat to renderfermentation more rapid.
For distillation, the apparatus of P. Labat was formerlyin use everywhere. It consisted of a flat still holding 1,500litres, a condenser, and a refrigerator. It was simple andstrong, and gave excellent products, which, although lesspure regarded as alcohol, were more perfumed than thosegiven by the apparatus with plates. The great disadvantagewas the great consumption of fuel, and slowness in working.
The apparatus of Van Kecken, now replacing it, consists ofa cvlindrical still surmounted by a column with three plates.It exhausts the worts well. 3,000 litres containing 198 litresof alcohol gave 192 litres on distillation.
Assuming a yield per hectare (2|- acres) of 41,000 kilos,of cane, this would give 2,870 litres of pure alcohol, orabout 48 hectolitres of rum of 60°, at 40 francs perhectolitre.
The molasses used for the manufacture of tafia is 40° to41° B., and is acid in reaction. It contains 37 to 40 percent, of saccharose, 16 to 20 of reducing sugars, 4 to 4*5of ash, the rest being water and organic matter. I t is mixedwith water and spent wort in the proportions 10 : 24 : 66respectively, by volume, the density of the mixture being1*060 to 1*065. The vinasse or spent wort being oftenadded hot, the mixture is sometimes at 41° C. when ferment-ation begins. Fermentation lasts from 10 to 12 days, thevats having a capacity of 10,000 litres. The attenuation is1-020 only* Distillers reckon on a yield of 62 litres oftafia of 59° per 100 litres of molasses. The yield, calculatedfrom the amount of fermentable sugar, should be 85 litres.
Distillation is conducted in continuous apparatus with verysimple columns. The tafia is at once coloured with carameland exported in casks to Europe.—L. J . de W.
*Carbonic Acid from Fermentation ; Collection of. L. Meeus.
Zeits. Spiritusind. 1899, 22, [49], 449.GKAUAUG'S process (this Journal, 1899, 936) is beingworked on the large scale at a distillery near Eouen. Thegas is collected in a receiver, adapted to the fermentingvessel, and narrowed towards the top, and partially immersedso as to be luted in the liquid like a gasometer. The carbondioxide is pumped off through pipes to a separate building,where it is purified, liquefied and packed in suitable vessels.The distillery in question has a capacity of 300 hectolitresdaily, being equivalent to 23,000 kilos, of carbonic acid. Ifin this process the difficulty is actually surmounted ofobtaining carbon dioxide from such a source in a sufficientlypure state, an important step will have been taken.
—J. F. B.Butyric Acid Fermentation. A. Schattenfroh and K.
THE fermentation was set up by cheese, earth, water, theintestinal contents of human beings and cattle, rye andwheat meal, and leaven, by sowing small quantities insterilised milk, heating the mixture for 10—20 minutes bya current of steam and incubating in absence of air at37° C. Two species of butyric bacteria were then isolated,which the authors name Granulobacillus saccharobutyriensA. mobilis, non-liquefaciens and B. immobilis, liquefaciens.Both species produce quantities of rf-lactic acid as well asbutyric acid, the proportion of the two acids vary, and arepartly dependent on the carbohydrate employed. BacillusA, ferments milk sugar almost entirely to butyric acid,B. as a rule produces equal quantities of the two acids.Prom dextrose, saccharose, and starch, A. forms chieflybutyric acid, whilst B. always produces considerably more
lactic acid. The casein of milk is coagulated hy bothspecies, but not peptonised. The authors consider thatBotkin's " B. butyricus" has no existence.—J. F. R
Food for Milch Cows: Brewery "Settlings." [CattleFood.'] E. Kamm and E, Moller. Milch-Zeit. 1899, 28 ,97—90 ; through Zeit. Nahr. und Genussmittel, 1899, 11,860—861.
BREWERY " settlings " (Schlempe), have not hitherto beenused as cattle food. The authors have made experimentsby feeding cows on this substance giving the animals atthe same time hay, straw, beetroots, and brewers' grains.The yield and quality of the milk obtained from the cowswas up to the average, and the butter-fat prepared fromthe milk gave the following analytical results :—
Refractometer number (25° C.) 50*25Degree of acidity tfIteichert-Meissl number 2<>'3Kbitstorfer number *23l>Hiibl iodine number 33f8SInsoluble fatty acids •. • 8S*5
—\Y\ P. S.
Starch in Yeasts, Determination of 1). Crispo.Ann. Chim. anal. appl. 4 , 290.
See under XXIII*, page 77*
PATENTS.Br ewing Operations, Construction of Union Casks used in*
W. Cutler, Birmingham. Eng. Pat. 24,253, Nov. 17,1898.
THIS invention relates to a union cask for brewing purposeswhich is constructed of glass plates, held together in thedesired form by a metal framework and rendered tight bymeans cf cement. The interior of the cask being com-pletely lined with glass, no metal is exposed to the beer orother liquid. At the top and bottom of the cask, framescarrying spindles are placed, and there is also an openingto admit of the cask being cleaned.—J. L. B.
Brewers' and other Coppers and Pans Heated by DirectFire, Settings of. F. M. Maynard, Manchester. Eng.Pat. 1379, Jan. 20, 1899.
THE claims relate to the employment, above the furnacegrate, of a combustion and heat-diffusion chamber, thevertical axis of which coincides with the centres of thefurnace and pan bottom, whilst its lower part is arrangedto overhang or form a hood over the fire. Also, whilst thelower end of the chamber is expanded to form a hood overthe fire, its upper end may be expanded at a distance belowthe copper bottom, the said chamber being provided with aseries of passages and regulating devices for the admissionof air into it through ports or inlets situated around theoverhanging hood, preferably at its junction with the wallsof the furnace. Further, the employment of a double ash-pit is claimed, arranged preferably in a vertical line withthe furnace and combustion chamber, and supplied with airthrough passages leading preferably into its lower part, whilstthe upper part is enclosed or separated by a barred floor orpartition. An improved arrangement is also claimed for thepassages or pigeon holes by which heat is conveyed fromthe diffusion chamber to the flues encircling the pan orcopper, whereby the hot gases are more equally distributed.
-—J. F . B,
Beer, Alcohol, Wine, Vinegar, and the like; Impts inFermentation in the Manufacture of, and in the Prepara-tion of a, Yeast Extract for Use in the same. J. HeronLondon. Eng. P a t 24,751, Nov. 23, 1898.
THE inventor claims the preparation of yeast food bywashing out the resin and other impurities from yeast, thenallowing the purified yeast to liquefy, subsequently boilingwith hydrochloric acid, neutralising, filtering, and concen-trating He also claims the use of yeast extract prepared111 the above or any other way in the manufacture of beerwine, or the like, to stimulate and nourish the yeast cellsduring fermentation.—J. F . B.
Jan. si, i9oo#] THE JOUBNAL OF THE SOCIETY OF CHEMICAL INDUSTRY. 65
Yeast and Yeast Products, Process of Treating. R.Riickforth, Stettin, Germany. Eng. Pat. 25,101, Nov. 28,1898.
See under XVIII. A., next column.
Beer and other Beverages, Purifying, Treating, andAerating; Apparatus for. E. Scholes, Hollinwood,Lanes. Eng. Pat. 24, Jan. 2, 1899.
T H E inventor claims an apparatus by means of which theliquor can be rapidly refrigerated, aerated, and filtered, sothat the beer can be bottled without losing its carbonic acidgas or gaining any appreciable increase of temperature. Inapparatus of the indicated nature, a cylinder or receptacleis claimed, through which the beer or other beverage iscirculated, the cylinder containing a rotating refrigeratingcoil, and being also in communication with a carbonic acidgas supply to effect the rapid refrigeration and aeration ofthe liquid. Perforated cups are fixed to the rotating coilso as to facilitate the absorption of the gas.—J. F. IJ.
THE improved process claimed consists in liquefying theamylaceous material up to the point of saccharification byboiling with acid. The liquor is then neutralised andsaccharified by malt. The inventor also claims the methodof treating a mixture of powdered amylaceous material anddilute hydrochloric acid in a digester provided with a steaminjector until the whole of the amylaceous material hasbeen liquefied. The chloride'of sodium formed by neutrali-sation with sodium carbonate is useful, and the liquefiedstarch is then saccharified with a minimum expenditure ofmalt.—J. F. B.
Spent or used Hops, Treating. L. Wardle, Burton-on-Trent. Eng. Pat 539, Jan. 10, 1899.
THE claim is for mixing spent hops with yeast or extractof yeast, and utilising the product either as a cattle foodor a fertilising material.—J. L. B.
Distiller?/ Refuse [for Manure'], commonly called "PotAle" "or " Burnt Ale," Treatment of T. Storer and R.McAlley, Falkirk, Scotland. Eng. Pat. 6348, March 23,1899.
THE inventors claim a new manure produced by evaporatingto dryness pot or burnt ale, with or without the admixtureof lime.
It is remarked that the disposal of the spent wash is amatter of much annoyance to distillers, and the object ofthis invention is to evaporate it in open pans, partiallyneutralising it with lime if it be verv acid, and to obtain avaluable manure at little cost. The evaporation is preferablycarried out in a series of pans, the heat of which is regulatedso as to avoid decomposition at the higher concentrations.
—J. F. B.Non-intoxicating Beverages, Manufacture of. J. Webster,
Liverpool. Eng. Pat. 18,524, Sept. 14, 1899.THE patentee claims several recipes for making non-intoxicating " ales and stouts.,. For instance, orris root,coriander seeds, and block juice (liquorice), are mixed withwater in suitable proportions and boiled for two hours ;salt, caramel, and hops are next added, and the mixtureboiled again for two hours ; after which Demerara sugar isadded, and the whole heated to 212° F, for 5^ hours. Theliquor is then run on to coolers, allowed to ferment for24 hours at 60° F., and cleansed by adding finings andwhite of egg.—J. L. B.
0— FOODS.Jiape-seed Cakes, Volatile Mustard Oils from Various
Commercial. G. Jorgensen. Landw. Vers.-Stat. 52,269—290. Chem. Centr. 1899, 2, [16], 782. (See alsothis Journal, 1898, 1193.)
WITH regard to a judgment as to the danger of using com-mercial rape-seed cakes as fodder, the author remarks
as follows:—Those cakes which, on microscopical exami-nation, are shown to consist almost exclusively of rape seed,develop little mustard oil in contact with water, and can beused without particular caution. On the other hand, if themicroscopical examination indicates a considerable propor-tion of " Indian seeds/, (Brassica dichotoma, glauca, juncea,ramosa) and the cakes give, on further examination, largequantities (over 0-6 per cent.) of mustard oil, the thio-sinamine obtained from which contains a high percentage(over 22) of nitrogen, circumspection is needed in usingsuch cakes as cattle food.—A. S.
Brewery " Settlings " as a Food for Milch Cows. E. Rammand E. Mailer. Milch-Zeit. 1899, 28, 97.
See under XVII., page 64.
Butter fat, Chemistry of Rancidity in.—III. C. A. Brown,jun. J. Amer. Chem. Soe. 1899, 21, [11], 975.
See under XII., page 54.
Glycogen, Preparation and Determination of. A. Gautier.Comptes Kend. 129, [19], 701.
See under XXIII., page 77.
PATENTS.Yeast and Yeast Products, Process of Treating. K. Ruck-
THIS process consists of heating cleaned and dried yeast ata temperature not exceeding 85° C, with or without the useof a vacuum, until it obtains the taste characteristic of meatextracts, and may be used as food. The substance maythen be heated until quite dry, and then used in the form ofpowder; or it may be deprived of its liquid by filtrationthrough sand, charcoal, &c, the filtrate being afterwardsconcentrated and the deposit reduced to powder. For manyproducts it is necessary to remove the characteristic tasteproduced by the process, and this is effected by heating Avithalcohol or acetone or their derivatives below 60° C. for severalhours, then pressing and grinding to a fine powder ; or theproduct may be heated with water below 85° C , the waterbeing removed by subsequent pressure.—J. L. B,
Milk Casein, Modification of, and its Preparation as aFood. J. R. Hatmaker, London. From J. A. Just,Syracuse, New York, U.S.A. Eug. Pa t 1482, Jan. 21,1899.
CASEIN is dissolved in an alkaline solution containingsufficient alkali to neutralise from -|—| of the total acidity.The solution is dried in a thin film on a surface at 212°—220° F., from which the dried material is continuouslyremoved by a knife edge or brushes. The claims are forthe whole process, the drying process, casein so prepared,and the modified casein so prepared.—A. C. W.
Vegetable and Animal Albumin and Substances containingthe Same, Purifying. W. P. Thompson, London. FromG. Eichelbaum, Charlottenburg, Germany. Eng, Pat3759, Feb. 20, 1899. 6 '
THE processes claimed consist in heating the albuminousmaterial C flesh meal/ , « fish meal/ , &c.) with alcohol ormethyl alcohol and acetone under pressure, at a temperatureabove the boiling point of alcohol, and in using the samesolvents containing ammonia or sulphurous acid. A. C. W.
.)—SANITATION ; WATER PURIFICATION.
Surface Water Supplies, Protection of. J. C. Thresh,J. of State Medicine, 1899, 7, 802—805.
SURFACE water, collected on a large scale for the supply oftowns or villages, has rarely been charged with the spreadof typhoid fever. This the author attributes to one causethe storage of the water in large reservoirs holding from100 to 200 days, supply. During this storage, the water isfully exposed to the air for oxidation, and to sunlight, andthe long period of rest ensures more or less perfect sedimen-tation. Typhoid organisms introduced into such reservoirshave tittle chance of surviving and reaching the mains in
66 THE JOUENAL OF THE SOCIETY OF CHEMICAL INDUSTRY. [Jan. 31,1900.
a living condition. Nevertheless, conditions may arise inwhich the water in the mains may become infected.
To obtain full control of a gathering ground is, in thiscountry, next to impossible. Therefore, although muchgood may be done by efficient supervision of sanitaryarrangements and by draining, scavenging, &c, the possi-bility of the water becoming polluted at certain times, as,for instance, when heavy rains fall after drought, mustalways exist. It is also impossible to prevent low formsof vegetable and animal life from being carried into thereservoirs, and there multiplying, rendering the waterobjectionable in appearance and sometimes in smell.Therefore the author advocates, as precautions againstthe spread of disease by surface water, (1) the utmostpossible control of the watershed or collecting area; (2)very ample storage ; (3) sand filtration. Where the waterhas a plumbo-solvent action, the filtration should be througha mixture of sand and soft limestone.—L. A.
Crude Sewage, Bacterial Treatment of J. of StateMedicine, 1899, 7, 747.
T H E experiments of Drs. Clowes and Houston at Crossnessprove that such bacteria as B. enteritides spoi*ogenes andthe B. coli pass through the beds in but sli^htlv diminishednumbers, and hence, doubtless the B. typhosus wouldsurvive, and infect any stream into which the effluentmight be allowed to flow.
Gas coke of the size of walnuts seems the best adaptedfor use in the bacterial beds, and apparently no extrapurification is gained by increasing the depth of cokebeyond 6 feet. The experiments were made with screenedsewage, and the beds have been able to dispose of all thesuspended nuitter without becoming clogged. The effluentis not always clear, but by a single treatment the dissolvedoxidisable and putrescent matters are reduced over 50 percent., and the fluid remains free from objectionable odour.When worked properly, about one million gallons of sewageper day can he treated upon a bed 1 acre in area. Theexperiments made with secondary beds show that a furtherpurification takes place. The effluent produced by chemicaltreatment of the Crossness sewage is speedily fatal to fishplaced therein ; but in the first effluent from the coke-beds,not only gold-fish, but roach, dace, and perch, have livedfor months. From the bacteriological point of view, Dr.Houston does not regard the results as being so satisfactory,but he adds: — " In the attempt to treat sewage on bio-logical lines, it is to he noted that the solution of thesuspended matter, and even the partial destruction ofputrescible matters by microbial agencies afford sufficientground for justifying, the process, at all events as a pre-liminary measure. Whether this preliminary treatment isto be supplemented by further treatment, either by passagethrough coke beds, or by land irrigation, or by any othermethod, is a matter largely dependent on circumstances.'.
The reminder is given that the experiments at Crossnessare concerned with aerobic treatment only. The sewagehas not been, prior to the treatment, exposed to conditionsfavourable to the growth of anaerobic organisms. Thelatter, undoubtedly, are capable of digesting or dissolvingthe suspended (organic) matters in sewage, and it may yetprove that they are more efficient for this purpose thanthose bacteria which can only flourish in the presence ofoxygen. Much better results have been obtained, from thechemical point of view, by submitting sewage to the actionof both classes of organisms.—L. A.
Towns' Refuse, Destruction of tvitfi Special Reference tothe " EcoTiometer." K. U. Hodgson. J. of State Medicine,1899, 7, 725—741.
ALTHOUGH the practice of burning towns, refuse has beenin operation for many years, it is only during recent years thatthe utilisation of the heat so generated has become a prac-tical question. The earlier types of destructor were quiteuseless for the production of power. The principle of amodern destructor consists in the production and mainten-ance, in the cells and combustion chambers, of a sufficientlyhigh temperature to completely consume the refuse andevolved vapours, without the use of any extraneous fueland in such destructors the heat may be fully utilised and
made to evaporate fiom 1 lb. to 2 lb. of water per pound ofrefuse consumed.
To suppose that power generated by a refuse destructorcannot be depended upon for electric lighting is a fallacy.Whilst five years ago 80 lb. was regarded as the maximumsteam pressure obtainable by burning refuse alone, plantsare now building or in operation for over double that pres-sure, and also evaporating double the weight of water perpound of refuse. Towns, therefore, requiring steam-driver*electric-lighting plant needing more power than their avail-able refuse can give, should at any rate utilise all the powerthus obtainable, and the deficiency alone should be made*up by burning coal. At the Darvven Eefuse-destructor andElectricity Works, where steam at 200 lb. pressure isproduced by burning refuse, the grate-area of the cellis 90 sq. ft., and the grate, which is very wide, has fourcharging doors, the space below being divided by wallsforming four ashpits, each fitted with independent steam-jetblowers. Thus, any section of the grate can be charged orcleaned whilst the remainder is at full work. The gasespass into the combustion chamber and thence through and'around a 30 ft. x 8 ft. Lancashire boiler, finally passing:away through a regenerator formed of cast-iron pipes into*the chimney. The air drawn from between the regeneratorpipes to supply the furnace has a temperature of 300° F .
Tables are given which show the results obtained withvarious destructors.
The " Econometer" is a gas-weighing balance, whichshows automatically and constantly the percentage ofcarbon dioxide in the gases passing up the chimney, andtherefore, indicates any waste of heat caused by allowing,too much air to pass through the furnace. The gases,,drawn from the flue pass through the apparatus, and arereturned to the chimney or main flue at a point higher up,the current being maintained by an aspirator. A wood-wool filter first strains out the coarser particles of soot, acotton-wool filter collects the finer particles, and a calciumchloride tube dries the gas, which, thus purified and cooled,,passes into the gas-weighing globe. The gases leaving the-globe are taken away by a tube into the interior of thebalance case. The globe is balanced by weights, so that whenfilled with air, the indicator points to zero on the scale-When gases containing carbon dioxide are drawn throughthe globe it descends, and the indicator travels along thescale until it reaches a point which shows the percentage ofcarbon dioxide present. When coal is being burnt, thevolume of air actually used bears to the theoretical amountrequired the ratio «' • t where K is the percentage of carbon
dioxide in the gases (Bunte). The losses corresponding toall percentages of CO2 from 2 to 15 are given in a table.*
•—L. A .PATENTS.
Purifying Water and other Liquids, Apparatus for.II. Desruraaux, Paris. Eng. Pat. 22,520, Oct. 26, 1898.
THESE improvements relate to apparatus for purifyino-water, &c. of the kind described in Eng. Pat. 7006of 1889, and are for the purpose (1) of providing improvedmeans for regulating the supply of water to be purified -(2) of automatically stopping the apparatus when workingwith variable delivery; (3) of facilitating the movement ofthe hollow rotary shaft of the saturator; (4) of facilitatingthe cleansing of the filter ; (5) of regulating the distributionof the reagents; and (6) of preventing mud from beinoearned into the decantor or treating chamber by the ^water.—L. A.
Filtering Apparatus, [Water], C. G. E. Salzbero>er »n^C. Kappesser, both of Westphalia, Germany p™ £ •2019, Jan. 28, 1899. 7 ' ^ P a t -
Two or more chambers, filled with filteringmounted on a hollow shaft, with which they commnn'through perforated plates or sieves, the shaft T ! ?connected to the discharge pipe for the filtered water Tfcfapparatus is immersed in the water to be filtered β-n**!water passes inwards through the lower filtering chamWor chambers to he discharge pipe. The water is p r w Z Sfrom entering the upper chamber or chambers of ftapparatus by means of removable slides. When it •
Jau. 3\, 1900.] THE JOURNAL OF THE SOCIETY OF CHEMICAL INDUSTRY. 67
desired to recharge the lower chambers with fresh filteringmaterial, the slides are removed, and the chambers arerotated on the shaft, so as to bring the upper chambers intothe lower or operative position, and the lower chambersinto the upper position, where they can be convenientlyrecharged. Means are provided for opening and closingone end of the shaft, and for locking the chambers in theposition to which they are adjusted. In a modification thechambers are mounted on a hollow cylinder, which isprovided with covers, operated by eccentrics, and adaptedto control the admission of the water to the chambers.
—R. A.Water - purifying Apparatus, L. Hirt, Grevenbroich,
Prussia. Eng. Pat. 18,129, Sept. 7, 1899.THE apparatus consists of a series of chambers arrangedafter the fashion of a filter-press, comprising at one end aheating chamber into which the water is admitted and inwhich it is raised in temperature by exhaust or live steam,in the middle a precipitation chamber which the hot waternext enters and in which it is mixed with suitable chemicals,and at the other end a filter press by which the suspendedprecipitate is removed. In being heated, the water eitherflows between hollow plates through which exhaust steamis led ; or it flows through a pipe into which a jet of livesteam is injected. By the latter method, the solids pre-cipitated by heat, which would incrust the plates of theheater, are said to be kept in suspension by the free circula-tion of the water.—L. A.
Sterilising Water or other Liquids, Apparatus for.L. Gathmann, Washington, Columbia, U.S.A. Kng, Pat.21,452, Oct. 27, 1899.
A CLOSED chamber containing, insulated iron electrodes isinserted in the water main in such a manner that all thewater flowing along the main must flow through thechamber and past the electrodes. The water is in thismanner " subjected to the action of an electric current ofa character such as to destroy the germs or minute forms ofanimal life therein."—L. A.
Precipitated Sewage Sludge, Carbonising and Obtaining ofProducts from. W. It. Ilutton, jun., Whiteinch, Lanark.Eng. Pat. 21,921, Nov. 2, 1899.
THE sludge is carbonised in " retorts, gas producers, orthe like, at a temperature varying from 1,000° to 1,400° F.,so as to obtain char or coke as a residual product.',
—L. A.Precipitated Sewage Sludge, Utilisation of W. K. Hut-
ton, jun., Whiteinch, Lanark. Eng. Pat. 23,562, Nov. 9,1898.
THE sludge is destructively distilled in retorts, producingchar or coke and volatile products.—L. A.
Purifying Waste and Impure Waters, particularly suchWaters as contain Greasy Matters; Method of andMeans for. J. Delattre, Dorigniers-Flers (Nord),France. Eng. Pat. 555, Jan. 10, 1899.
THE water to be treated is first pumped up to a suitableelevation, then mixed with excess of sulphuric acid andallowed to flow through settling tanks, which retain theprecipitated fatty and other matters. The effluent, clarifiedby passing through a filter, is neutralised with milk of lime,and continues to flow through a second series of tanks, inwhich a further deposit is retained. The neutral or slightlyalkaline effluent is discharged into the river. The greasydeposit from the acid treatment is extracted by a volatilesolvent and the fat is recovered. The inventor claims thegeneral combination and arrangement of plant for carryingout the above process, which is illustrated and described inthe specification.—L. A.
( C.) —DISINFECT ANTS.Formaldehyde, Disinfection of Dwellings with. R. von
Walther and A. Schlossmann. Miinchener medicin.Wochensch. 1899, 46, 1535, 15G2; through Chem. Zeit.Rep. 1899, 374.
WHEN using formaldehyde vapour as a disinfectant, it isimportant simultaneously to vaporise water, so that the
saturation of the air may be increased. Lingner's appa-ratus is said to be useful for this purpose, and with its aid,employing steam as well as the formaldehyde, rooms canbe completely sterilised, even if they contain such materialsas garden mould mixed with albumin. The use of glycerinis not recommended; it simply reduces the necessaryamount of formalin.—F. H. L.
XIX-PAPEK, PASTEBOAKD, Etc.Rosin Sizing. C. Dreher. Papier-Zeit. 1899, 24,
[101], 3998.THE author's process consists in the preparation of rosinsoaps, rich in free rosin, by the help of phenols. ^ He statesthat crude carbolic acid is miscible with rosin in all pro-portions. The addition of carbolic acid to rosin causes aconsiderable lowering of the melting point; for instance, arosin which melts at 120° C. in the pure state has its meltingpoint lowered to 95° C. by the addition of 10 per cent.ofcarbolic acid. Consequently the molten condition, in whichthe rosin is most easily saponifiable, can be readily obtainedunder water in open boilers. The presence of carbolic acidnot only assists the saponification of the rosin, but enables thesoap to hold more free rosin in suspension, when dissolvedin water, than without the phenol. Proportions of 10 and20 per cent, of carbolic acid on the rosin impart an odourto the paper, but with 2 per cent, a perfectly odourlesspaper is obtained. This small quantity does not give the-maximum advantages described above. A size can beprepared by this method in a very short time, it is said,which contains 40 per cent, of free rosin. It forms aperfectly smooth emulsion, and does not leave the slightestodour on the paper treated with it.—J. F. B.
PATENT.Pulp and other Paper-makers' Materials, Method and
Apparatus for Mixing or othenvise Treating. J .Almond and S. F. Andrews, Bath. Eng. Pat. 24,600,Nov. 22, 1898.
TIIE claim is for an archimedean screw, working verticallyin a tank containing the materials.—L. A.
X X - P I N E CHEMICALS, ALKALOIDS,ESSENCES AND EXTEACTS.
Simple Methods of Preparing Sulphur, Chlorine, andBromine Compounds of the Cerium Metals. W. Muth-mann and L. Stiitzel. Ber. 32, [17], 3413—3419.
1. Sulphides, Ce.S^ LCL2SZ, Nd2S3, Pr3S3. — DidierVmethod of heating the oxides in a stream of H2S does notyield a product free from oxide, and the action is very slow.The authors used the pure anhydrous sulphates, heatingthem to dull redness for a considerable time in a stream ofdry H2S. The colour-change was soon apparent; ceriagave finally a brown-black to black powder, lanthana apure yellow, neodymia an olive-green, and praseodymium achocolate-coloured powder. The conversion was practicallycomplete, and analyses showed that the sulphides were verypure; no unchanged sulphate remained. The sulphidesare fairly stable m the atmosphere at the ordinary tempera^ture, the stability being greater the higher the heat usedin their preparation. They are slowly decomposed withevolution of ILS on boiling with water, La2S3 being mostreadily decomposed. Dilute acids dissolve them to clearsolutions, with liberation of H2S. Their ignition tempera-ture is _ comparatively low in dry air-below a red heat-Oe2b3 is even pyrophoric if finely enough divided Theproduct of combustion in all cases is a mixture ofsulphate and oxide. Ce2S3, on boiling with KOH, alwaysgives the yellow eerie hydroxide, not a greenish oxysulphideas stated by Mosander ; nor could the authors ever obtainMosanders crystalline cerium sulphide, but always theamorphous variety. Specific gravity determinations gave
ftJ^TSSr^ 5'02; La2S*4*9,08; N^2.m Chlorides, CeCl3, LaCl3> frc.-These are readily
obtained m the anhydrous form by heating the sulphides in
p 2
68 THE JOURNAL OF THE SOCIETY OF OHEMIOAL INDUSTRY. [Jan. 31,
dry HC1. The sulphates were converted into sulphides, asdescribed above ; the apparatus was allowed to cool some-what ; the H2S was driven out by a stream of CO2 ; thenpure, thoroughly dried HC1 was passed through, and theheat was increased to a point not exceeding dull redness.The reaction began very soon, and finally the colours of theproducts were:—cerium and lanthanum chlorides, purewhite; neodymium chloride, a fine rose-colour; praseo-dymium chloride, green. Any sulphur liberated by de-composition of H2S in the tube was driven out by passingCOj through the heated tube. The yields of chlorides werepractically quantitative, analyses showing that the productswere very pure. The chlorides are very hygroscopic; theydissolve in water, with a hissing sound, to a clear solution.They are also soluble in alcohol. They can be volatilisedwith difficulty, and are comparatively readily fusible.
3. Cerium Bromide, CeBr%.—This was obtained in apure, anhydrous state in the same way as the chloride, byheating Ce2S3 in a stream of hydrobromic acid. It is awhite, crystalline, hygroscopic powder, dissolving in waterto a clear solution.—H. 13.
THE author finds that very dilute aqueous solutions ofdiazo compounds are gently acted upon by hydrofluoricacid, so that in this way the manufacture of organic fluorinecompounds becomes possible. Thus, 10 kilos, of aniline,32*5 kilos, of hydrochloric acid, and 20 litres of water arediazotised with 7*53 kilos, of sodium nitrite. The solution,along with 20 kilos, of hydrofluoric acid, is conveyed into ajacketed pan, connected with a condenser and a tube lead-ing into two consecutive receivers, cooled by ice. The panis gently heated until the evolution of nitrogen commences ;towards the end of the reaction the steam is turned on fully.When no more nitrogen is evolved, the mixture is neutra-lised ; the oil formed is separated, distilled with steam, andfinally fractionated. The fluorobenzene is a limpid oil ofstrongly aromatic odour, and boils at 85° C.
In a similar way, fluoropseudocumene is prepared frompseudocumidine (meltingpoint, 24°; boiling point, 172°), anddifluorodiphenyl from benzidine (melting point, 87°).
Some of the aromatic fluorinated hydrocarbons are liquid,some are solid. The fluorine is so firmly attached in thenucleus that in most cases metallic sodium is alone able toremove it. Whilst chlorine, bromine, and iodine may bereplaced by the sulphonic group by means of concentratedsulphuric acid, the fluorine cannot be substituted in thismanner.
The presence of fluorine increases the volatility of ahydrocarbon and also the capability of diffusion through ananimal membrane. The solid fluorine compounds sublimeeasily. They are not decomposed in the organism. Nitricacid may replace the fluorine by a nitro group. Fluorinatedhydrocarbons are easily soluble in fatty oils.
The physiological effect of the fluorine compounds is notantiseptic, but aseptic, micro-organisms not getting killedby them, but only prevented from multiplication. Suchfluorine compounds, when properly purified, form valuabletherapeutic agents.
Experiments with fluoroform have demonstrated that itmust be absolutely free from impurities, even from air.For this purpose, the author has devised a method anddesigned an apparatus by which such pure fluoroform maybe obtained from iodoform and silver fluoride.—S. K.
Hydrocarbons, Unsaturated, New Mode of Preparation ofL. Tschngaeff. Ber. 1899, 32, [17], 3332—3335.
T H E method in question has for its object the transfor-mation of an alcohol into the corresponding unsaturatedhydrocarbon and depends upon the decomposition, whichcertain xanthates undergo, when subjected to destructivedistillation. By distilling under ordinary or slightlydiminished pressure, xauthic ethers of the general formula—CnHsm-i O-CS.SR; R denoting any alcohol radicle (thereaction apparently proceeding in the smoothest mannerwhen R = C H 3 \ decomposition usually ensues and thismainly in accordance with the equation—
C*H2 M_I O.CS.SR = CnH2m_a + CSO + R.SH,
although a secondary reaction also appears to go on inpart, according to the equation—
CBH2w._i O.CS.SR = CnH2m_2 + CS2 + E.OH.
Both reactions give rise to the formation of an unsaturatedhydrocarbon of the formula CftH2»t-2> which is readilypurified by fractional distillation, finally over metallicsodium. The decomposition is effected with great easeand at a comparatively low temperature. The yieldsare for the most part satisfactory. To illustrate theadvantages which the new method possesses, the authorgives as an example the transformation of menthol intomenthene. For this purpose menthol was converted intomenthyl-xanthie acid and its methyl-ether subjected todestructive distillation, the chief products of the reactionbeing menthene and methyl-mercaptan. Menthene ob-tained in this way differs from all previous preparationsin its optical activity, giving higher and practically con-stant values. Two preparations obtained at different timesgave [a]D = +114-77° and +116*06°, whilst menthenesprepared by other means (from /-menthol), gave numbersranging from 0° to + 60°.—D. B.
Glycerin, The Speed and Limits of Esterification of, byPhosphoric Acid. H. Imbert and G. Belugou. Bull.Soc. Chim. 21 , 935.
See under XXIV., page 80.
Eucalyptus, Three Neiv Species of. R. T. Baker. Proc.Linn. Soe. of N.S.W. 1899, Part 2, June 28, 292 300.See also this Journal; 1890, 737, 827.
E. Smithii.—The kino gives a turbid solution in cold waterand contains eudesmin but not aromadendrin. The yieldof essential oil is high, 1-354 per cent., it consists almostentirely of eucalyptol and dextropinene, phellandrene isabsent. The oil has a low specific gravity, but contains 70per cent, of eucalyptol.
E. Dawsonii.—" Slaty gum." The kino is similar tothat of E. Smithii. The yield of oil is only 0-172 per cent.its specific gravity is 0-9414 at 15° C , its chief constituentis a sesquiterpene ; phellandrene is also present. It containsno oucalyptol.
E. Camphora.—" Sallow" or " Swamp Gum." Theyield of oil is 0-398 percent.; it contains eudesmol (seefollowing abstract), pinene and eucalyptol. No phellandrenewas detected. The sp. gr. is 0*9167 at 15° C. A. C. W.
Eucalyptus Oil, The Crystalline Camphor of {Eudesmol)and the Natural Formation of Eucalyptol. H. G. Smith'J. and Proc. Roy. Soc. N.S.W. 33 } 86—107. See alsothis Journal, 1898, 180, 868; 1899, 66, 167.
THE crystalline camphor (eudesmol) found in the essentialoil of E. piperita in small quantity has now been isolated inlarger amounts from the oils of other species. The oil ofE.goniocalyx is very rich in eucalyptol, it also containseudesmol and dextropinene. The crude oil of E. camphoragives on redistillation 18 per cent, boiling between 280° and290° C. ; the distillate solidifies on cooling. In all caseswhere eudesmol has been found, it is accompanied bveucalyptol ; it has never been found in oils free fromeucalyptol or containing only traces. See also this Journal1899, 1049.—A. C. W. Journal,
Poplar Buds, Essential Oil of F . Fichter and EBer. 1899, 32, [16], 3183-3185.
TH*: oil, as obtained from Schimmel, was purified bvfractionation under 1 2 - 1 4 mm. pressure. The small firstfraction possesses the pleasant smell of the oil in J n l !trated form, the second and principal fraction 132° iiv?n(2630-269° C. under ordinary pressure) had thTsp £D i = 0-8926, and rotation in 2 dcm. tube aD = + ,0° 4 Jat 22° C. The third fraction, distilling at from i7i»«» •200° C , solidified to a buttery mass t o
The second fraction had the molecular weight of asesquiterpene, it yielded a mtrosochloride, nitrolpiperidinenitrolbenzylamine, mtrosate, and nitrosite identical with t h 'corresponding compounds obtained by Chapman f7om the
Jan. si, 1900.] THE JOUENAL OP THE SOCIETY OP OHEMIOAL INDUSTRY. 69
humulene from hop oil (this Journal, 1893, 783 ; 1895, 63),hut in much smaller quantity. This fraction appears tohe a mixture of humulene Avith an unknown and activesesquiterpene. The third fraction is a mixture of C24H50
and higher homologues. The quantity of this stearopteneis ahout 0*5 per cent.—A. C. W.
JBergamoty The Development of Essence of. E. Charabot.Comptes Eend. 129, [19], 728—731.
T H E author has examined comparatively the green andripe fruits, with the following results:—Density of theessence practically the same; rotatory-power, much greaterin the case of the ripe fruit. During ripening, the free acidsslightly diminish, the linalyl acetate increases, whilst thetotal linalool diminishes. The terpenes increase, hut theproportion of limonene to dipentene remains constant, whilstthe hergapten diminishes. Thus the linalool seems to beformed first, and then the acetic acid, which, acting on thelinalool, acetvlates one part and dehydrates another.
—J. T. D.
Digitalis, The Colouring Matter of. A. and A. Trillat.Comptes Kend. 129, [22], 889—890.
THE residue from the preparation of digitalin fromDigitalis lutea was evaporated to a syrup, extracted bybenzene, the benzene evaporated, the oil extracted from theresidue by petroleum spirit, and the solid residue crystal-lised from amyl alcohol, and afterwards from ordinaryalcohol of 9(J per cent. Fine silky yellow needles werethus obtained, melting at 217° C, and with the formulaC16H1o04. The substance is insoluble in water, mineralacids, or petroleum spirit, soluble in ethyl or amyl alcoholor chloroform. Alkalis dissolve it, giving a fine redsolution. It yields no reducing sugar, and is not affectedby acetic acid and phenylhydrazine. It seems to constitutethe colouring matter of the plant, but is apparently notderived from chlorophyll, and is peculiar to this one speciesof Digitalis.—J. T. D.
Strychnine and Methylene Iodide, Reaction between. V. F.Trowbridge. Arch. Pharm. 1899, 237, 617; throughChem.Zeit. Rep. 1899, 371.
HEATED for an hour in a sealed tube in presence of methylicalcohol, or agitated for several days with a chloroformicsolution of the alkaloid, strychnine and methylene iodidereact to form a white crystalline compound—
P TT Yfj piT T\~<2\ *-*-h22 2 2 • v>JLloloj
melts at 212°. On digesting the aqueous solutionAvith freshly precipitated silver chloride, the correspondingchlorine derivative is obtained in the form of white needles,very soluble in water, from which double salts containinggold, mercury, or platinum can be prepared. The analogousbromide may be obtained from the chloride by shaking itswarm aqueous solution with silver oxide and faintly acidifyingthe filtrate with hydrobromic acid. It yields white needle-shaped crystals.—F. H. L.
Strychnine and Iodoform or Chloroform, Compounds of.P. F. Trowbridge. Arch. Pharm. 1899, 237, 622 ; throughChem. Zeit. Rep. 1899, 371.
LEXTRAIT has already obtained the compound—
o c
from the alcoholic solutions of its constituents ; the samebody is produced when strychnine and iodoform are mixedin molecular proportions. On boiling it with alcohol, how-ever, a more stable compound, 2C2lH22;N2O2. CHI3, separatesfrom the filtrate in dark reddish-brown plates. At ordinarytemperatures chloroform does not combine with strychnine*;heated in a sealed tube to 150° for 10 hours, crystals of
KJXOOO . HC1. CHC13
are formed; but the substance is not permanent, andquickly loses part of its chloroform.—F. H. L.
Bismuth, Sulphates of. B. H. Adie. Proc. Chem. Soc.1899,15, [215], 226.
T H E author has investigated the conditions of formationand limits of existence of the sulphates of bismuth, and hasfound that from sulphuric acid of any strength betweenthose represented by H2SO4, 6H2O and H2SO4, 12H2O, abasic bismuth sulphate having the formula 5Bi2O3, 11SO3,17H.,0 crystallises out ; if between H2SO4, 3H2O andand"H2SO4, 5H2O, the sulphate may be represented asBioO,, 4SO3, 7H2O, and if the strength be between H3SO4,HoO 'and H4SO4, 2H2O, the salt obtained has the compositionBf2O3, 4SO3, 3H2O. From sulphuric acid itself, the sulphatewhich crystallises out at temperatures above 170° has theformula Bi2O3,4SO3, H2O ; if below 170°, Bi2O3,4SO3,10H2O.
This temperature 170° is that at which the acid sulphatesare decomposed when heated in an air-bath, the normalbismuth sulphate, Bi2O3, 3SO3 being formed.
Cinchona. J . M. Vargas-Vergaru.
Seepage 11.
Ether, Detection of Aldehyde in. H. Blaser. Pharm.Centr. H. 40, 607.
See under XXIII., page 73.
Ethyl Nitrite, Determination of K. C. Cowley andJ. P. Catford. Pharm. J . 1899, 63, [1534], 471.
See under XXIII., page 77.
Lemon Oil, Examination of J . Walther. Pharm. Centr.40, 621.
See under XXIII., page 78.
Formaldehyde in the Free State and in its Compounds,Method for the Detection and Estimation of. G. H. A.Clowes and B. Tollens. Ber. 1899, 32, [15], 2841.
See under XXIII., page 77.
Salt-forming Alkaloids, A Simple Alkalimetric Method forthe Estimation of, with Phenolphthaleln. H. M. Gordin.Ber. 1899, 32, [15], 2871.
See under XXIII., page 78.
PATENTS.
Aromatic Oxyaldehydes, Manufacture of. T. R. ShillitoLondon. From J. R. Geigy and Co., Basle, Switzerland.Eng. Pat. 27,236, Dec. 24, 1898.
See under IV., page 41.
Perfumes and Flavourings from Essences, Extraction of.H. Sauvinet, Malakoff, France. Eng. Pat. 2204, Jan. 31.1899.
THE process claimed, consists in absorbing the essence in aporous material (cotton-wool, sponge, pumice, &3.), whichwill reduce it to a state of very line division, extracting theabsorbing material by dilute alcohol or other solvent*, andfiltering. The product is soluble in water.—A. C. W. '
Ionone into the two Varieties, a- and β-lonone, Process forSeparating. J . C. W. F. Tiemann, Berlin, GermanvEng. Pat. 1944, Jan. 27, 1899.
THE process consists in boiling ionone with sodium bi-sulphite solution, or with sodium sulphite solution towhich is added acetic acid or excess of ammonium sulphateuntil a clear solution is obtained. The feebly alkalinesolution is then extracted by ether to remove impuritiesand β-ionone removed by a strong current of steam. Thensodium carbonate is added, and the α-ionone distilled overwith steam, or caustic alkali is added, the liquor rapidlycooled after a short time and extracted with ether, or afteradding caustic alkali and cooling, the liquid is neutralisedand the α-ionone obtained by steam distillation. If theionone contain only very small quantities of the $ varietywhich seldom happens, the solution obtained by boilimrwith bisulphite may be concentrated until the hydrosulphonic acid salts of α-ionone crystallise out on cooling whenthe mother-liquor is subjected to the above process ofseparation.—A. C. W.
70 THE JOUENAL OF THE SOCIETY OF CHEMICAL INDUSTRY. [Jan.3i,i9oo.
Sweetening Liquids, Production of. P. Porchere, Lyons,France. Eng. Pat. 7190, April 5, 1899.
THE claims are for solutions of anhydrobenzoic o-sul-phamide or p-phenetolcarbainide or their salts in diluteglycerin, water, alcohol, glucose, or sugar syrup, and thecombinations of these solutions with cane sugar, glucose,essences, &c—A. C. W.
Peroxide of Hydrogen and other Peroxides, Process ofPreparing. E. Edwards, London. From T. Drescher,Gorlitz, Germany. Eng. Pat. 21,333, Dec. 9, 1899.
BARIUM peroxide is subjected to grinding action so as to finelycomminute it whilst being acted upon by sulphuric or otheracid for the production of hydrogen peroxide. The processmay " be used in the preparation of other peroxides madeout of peroxide of barium, or other peroxides made bymeans of acids."—E. S.
XXI.-PHOTOGEAPHY.a Silver-Germ" Theory of the Latent Photographic Image.
J. M. Eder. Phot. Corr. 1899, 36, 650; through Chem.Zeit. Rep. 1899, 376.
THE author still maintains his opinion that the " silver-germ "hypothesis is incredible (see this Journal, 1899,516 and785). The action which mny occur during developmentbetween the metallic silver already reduced (chemically), andthe unaltered silver bromide of the film is quite insignificantin comparison with the effect of light on the plate. This is jshown in spectrum photography; for the negative obtainedfrom a concave grating bears perfectly sharp lines, whichdevelop up to proper density without spreading laterally toanything like the same extent.
He also protests against the use of the expression- " silver-germ " to denote the substance composing the latent
image, when the hitter is regarded as a sub-brornide.—F. H. L.
Ferrous Oxalate Developer, Action of Thiosulphate upon.J. Sterry. Phot. Ocntralbl. 1899, 5, 387 ; through Chem.Zeit. ReV 1899, 376.
IT is already well known that the activity of an ordinaryferrous oxalate developer is greatly increased by the additionof traces of a hypo/' [whilst an excess is first useless, andafterwards prejudicial]. The author has investigated the prac-tical bearings of this property of thiosulphate, determiningthe speed of the developer when applied to slow plates, andwhen containing various proportions of the reagent. Hisresults are as follows :—
Proportion of Thiosulphate.
1111
0100,00010,0001,000100
1:10
Relative Speed.
13'15'
2iriY0"
1Ti00
'8'0
—F. H. L.Iron Developer y A Stable. G. Hauberrisser. Phot.
THE author recommends the addition of Rocholle salt to theusual mixed ferrous oxalate developer, with the object ofkeeping the iron in solution. The developer is prepared asfollows :—To five parts of an aqueous 1 : 3 solution of ferroussulphate, slightly acidified with sulphuric acid, are added1 i-i- parts of an aqueous 1 : 5 solution of Rochelle salt;the mixture is boiled and poured whilst hot into 17* partsof an aqueous 1:3 solution of neutral potassium oxalate.To every 100 c.c. of this solution may be added, as required,5_10 drops of 1:10 solution of potassium bromide. Ifstored in well-corked bottles, filled to the neck, the solutionremains clear and preserves its developing powers unim-paired for a long time. It can, however, be regeneratedwhen necessary by placing in the sunlight, which exercises•a reducing action upon it according to the equation:—
not so'well suited to under-exposed plates as the organicdevelopers, but is to be preferred in most other cases.
y — H. H. 13. S.Hydrogen Peroxide and Potassium Ferro- and Ferri-
cyanides, Action of Light on Solutions of W, A,Kistjakowsky. Chem. Zeit. 1899, [86], 931.
WHEN air is passed through a solution of potassium ferro-eyanide, exposed to the light of the electric arc, it becomesalkaline to phenolphthalein. The addition of hydrogenperoxide accelerates the change. In diffused daylight theabove change does not occur. An aqueous solution of purehydrogen peroxide (1 to 3 per cent.) containing a littlepotassium ferroeyanide (0*01 to 0*005 normal), decom-poses very slowly in the dark, but much more rapidly insunlight or in the light of the arc. When the ferri- and ferro-cyanides and caustic potash are present in a determinedratio, and the intensity of light is maintained constant,the rate of decomposition of the hydrogen peroxide may beexpressed by a logarithmic formula. When a solutionof hydrogen peroxide containing ferri- and ferrocyanidesof potassium, is exposed to light for 5 or 10 seconds, thedecomposition proceeds in the dark at three times itsformer rate. The influence of light is not due to a rise oftemperature.—T. E.
Colour Photography ; The Joly Process. J . W. Hinchley.See page 5.
Sensitising Paper and other Surfaces ; New Process for.11. C. Schupphaus.
See page 16.
PATENTS.Photographic Printing, Impts. in. A. F . Hargreaves,
Eoslin, Midlothian. Eng. Pat. 25,043, ISTov. 28, 1898." A FEKRO-pitussiATE blueprint" prepared on cotton or othersuitable fabric in the usual way, is well washed to removeall unchanged chemicals, and is afterwards subjected to theaction of a dye bath consisting of a solution of any or allof the following materials :—madder, alizarin, purpurin orlogwood; the temperature of the bath is preferablygradually raised in 30 or 40 minutes from ]00°F. to theboiling temperature, the liquor being well agitated mean-while. After washing and treating with a boiling soapsolution, the prints are again washed, dried, pressed, and ifdesired, starched and mounted. By this process the bluecolour of the print is changed owing to the deposition of apurple, black or grey lake, the iron present acting as amordant.—T. H. P.
Sensitised Continuous Films for Photographic and Cine-matographic Purposes. J . T. Sandell, London.Pat. G20, Jan. 10, 1899.
A SUITABLK surface is coated with sensitised emulsion,either in a single layer sufficiently thick to give a film strongenough to be used without any support, or in severalsuperposed layers of graduated degrees of sensitiveness.To give the film the necessary hardness to render it self-supporting, a hardening agent such as alum or formaldehydeis mixed with the emulsion. When dry, the film of emulsionis stripped from the surface to which it was applied.
—T. H. P.
THE exclusion of light from photographic films arranged ina roll or « cartridge " is generally effected bv means of anenveloping roll of black paper, the colouring matter ofwhich is liable to have an injurious effect on the film eithprwhen in the « cartridge » or when immersed in the develop-ing or fixing solution. ^ In this patent such action is obviated
Hkely to injurious affect the i ^ ^ S r i ^ S 5 Shim under ordinary conditions of storage, use, develoDmontor fixmg The protecting end portion! of the film Slight-excluding portion are made integral with the °mreceiving portion.—T» H. P ,
Jan.si, woo.] THE JOUBNAL OF THE SOCIETY OF CHEMICAL INDUSTRY* 71
Photographic Positives, Production of. J . E. Thornton,Altrincham, and C. E. S. Kothwell, Manchester. Eng.Pat. 887, Jan. 14, 1899f
PHOTOGRAPHIC pictures are said to be produced in a moredirect and rapid manner and with the use of shorterexposures than the usual method affords, A film ofgelatino -bromide emulsion is supported by a black or-coloured backing of paper, celluloid or other flexiblematerial. After short exposure, the film is developed with amon-staining developer, and is then fixed and washed in theusual way. The picture is then whitened by immersionin a mercuric chloride solution. After washing and dryingthis picture remains as a light deposit on a black or colouredbackground.—T. H. P.
XXII—EXPLOSIVES, MATCHES, Etc.Phosphorus, Lower Oxides of A, Michaelis and
M. Pitsch. Annalen, 3lO, [1],45—74.T H E authors have examined a number of so-called loweroxides of phosphorus, but find that only one exists, havingthe formula P4O, which they term phosphorus suboxide.They have prepared it in two ways, either by dissolvingordinary phosphorus in aqueous alcoholic soda andprecipitating the dark red solution with dilute acid, or elseby removing water by means of acetic anhydride fromJiypophosphorous acid. Phosphorus suboxide forms abright orange red powder of specific gravity 1*9123 at-6° C. It can when dry be heated in the air to a tolerablyhigh temperature without inflaming, but if moist it takesfire spontaneously after heating for some hours to00° C. Chlorine converts the dry compound into phos-phorus oxychloridc and pentachloride, whilst the moist oxideis oxidised by halogens and by sodium hypochlorite to[phosphoric acid, although iodine only acts very slowly.Sulphuric acid is reduced by the oxide to sulphurettedhydrogen, whilst concentrated nitric acid inflames it andhydrochloric acid is without action. Aqueous alcoholicpotash or soda lye dissolves the suboxide to a dark redsolution from which it is precipitated by acids includingcarbonic acid. The red solution on standing or warminggives off hydrogen and hydrogen phosphide leavingsodium hypophosphite in solution.—T. A. L.
Matches, A Non-Phosphorus Tipping-paste for. II. Gans.Zeits. f. angew. Chem. 1899, [45], 1082.
ACCORDING to his German Pat. 105,061, the author adds to afeebly acid or neutral solution of sodium thiosulphate halfthe equivalent quantity of cupric chloride, and somebarium chloride. He thus obtains a voluminous yellowprecipitate, which is unaffected by the air, according to theequations :—CuClo + 2 Na2S2O3 -f BaCl2 = 4]NTaCl +CuI3aS4Or), Double salts and barium salts of otherpolythionic acids are doubtless also produced in smallquantities. Other oxidizing agents, such as ferric chloride,may be used in. place of cupric chloride, and similarpolythionates of other bases obtained. A practicabletipping-paste is produced from 10 to IS parts of the abovebarium-copper salt and 9 to 10*5 parts of gypsum, 3*7 to3*8 parts of sulphur, 3*7 to 5*1 parts of iron pyrites, 11 to12 parts of gelatin, and 57*5 to 59*0 parts of potassiumchlorate. This paste is said readily to ignite paraffin, evenwhen rubbed merely on the coat sleeve or a smooth surface,and to be proof against moisture. Its temperature ofignition is said to be 90° to 100°.—J. A. B.
PATENTS.Explosives. J . E. Evans-Jackson, London. From XL Alvisi,
Borne. Eng. Pat. 25,833, Dec. 17, 1898.T H E author claims that when ammonium perchlorate isadded to explosive substances, which may or may notrequire further oxygen to burn them, or is substituted forother oxidising salts, the following results obtain, namely(1) there is an increase in propulsive power; (2) anincrease in breaking power; (3) an increase in the ratioBreakingj)o^ J n Q r d e r t o b t a i n ^ m a x i m u m effect
Propulsive powerfrom ammonium perchlorate, the mixtures should be pre-
ferably ignited with detonators containing that substance.It is pointed out that ammonium perchlorate decomposesin three ways, namely:—
f i ^ "NTJ-T O1O — "NTH" f 1 4- 5 O
(2*.) NH4C1O4 = 2 H42O + CI + N + O2.
(3.) 2 NH4C1O4 = 2 HC1 + 3 H2O + N2 + 50 .
In substituting this salt therefore, for other oxidisingagents, these decompositions must be remembered. ^ Amongthe examples of explosives given, the following areselected:—
(1.) As detonators for filling capsules: Fulminate ofmercury, 90 or 83 or 80 parts by weight; Perchlorate ofammonium, 10 or 17 or 20 parts by weight.
(2.) As explosives : Nitroglycerin, 75, 80, or 60 partsby weight; Perchlorate of ammonium, 25, 20, or 40 parts.
(3.) As a gelatin gum : Nitroglycerin, 75 parts byweight; Soluble cotton, 5 parts; Cellulose (sawdust),5 parts; Ammonium perchlorate, 15 parts.—C. M.
Match, A New or Improved. W. P. Jones, St. Martins,and t l . M. Bates, Clapham. Eng. Pat. 26,332, Dec. 13,1898.
A NON-PHOSPHORUS match composed of chlorate of potash,3 to 4 parts; antimony sulphide, | to | par t ; leadthiosulphate, 1 part (or thiosulphate of other heavy metal);black oxide of manganese, -g- to £ part ; potassiumbichromate, ^ to £ part; powdered glass, red prussiate ofpotash and the usual agglutinating substances, as founddesirable.—G. W. McD.
Nitrating Cotton and other Organic Substances ;Apparatus for. T. C. Henchman, Essex. Eng. Pat.2645, Feb. 6, 1899.
A NITRATING apparatus consisting of a feeding table, a drumrevolving in an acid tank, a specially constructed chainpassing under the drum, rotating rolls to remove thenitrated substance, and squeezing rolls to remove excess ofacid.—G- W. McD.
Matches, Ignition Compositions for. C. R. Andersson andA. O. Anderssons Kabriks Aktiebolag, WenersborgSweden. Eng. Pat. 1698, Jan. 24, 1899.
THE composition of the ignition paste is given as follows :—Chromate of potash, 40 '5 parts; powdered glass, 19 #0;sulphur, 7*0; bichromate of potash, 7*0; oxide of zinc,4-5 ; silicate of magnesia, 4 ' 5 ; resin, 3*0; amorphousphosphorus, 3• 5; glue, 10*0; chromate of lead, 0*7; andtragacanth, 0*3 part. A solution for the preparation ofthe matches is also described consisting of : Gum benzoin,20 parts; turpentine, 5 ; and alcohol, 75 parts.
A SAFETY match consisting of a wooden stem tipped withan ignitable composition at both ends.—G. W. McD.
Friction Matches, Composition for Wax Tapers for*J, Craveri, Buenos Ayres. Eng. Pat. 22,147, ISTov 6*1899. * '
THK composition of the material forming the taper is givenas follows :—-White ceresin, 40 parts; purified colophony15 parts; calcium sulphate, 32 parts ; zinc oxide, 7 parts •and potassium nitrate, 6 parts.—G. W. McD. '
XXIIL-ANALYTICAL CHEMISTRY,APPARATUS, ETC.
PATENTS.Mercurial Air-Pumps. H. S. Maxim, 18, Queen's Gate
Place, London. Eng. Pat. 17,177, Aug. 9, 1898.THE flow of mercury in air-pumps of the " Geissler " and" Sprengel" types is regulated by means of a float, whichcloses the inlet when the mercury in the head rises above acertain level. In the improved pump claimed, the floatcontains glass beads or other particles of a suitable material
72 THE JOURNAL OF THE SOCIETY OF CHEMICAL INDUSTRY [Jan. si, woo.
through which the mercury flows from the inlet nozzle, andis thereby comminuted. The inlet nozzle passes through ahollow stopper containing a hygroscopic material, a mercuryor other suitable seal being employed to form a hermeticjoint between the stopper and head. The fall tubes haveenlarged upper ends, which open into the vacuum chamberat a point above that where the mercury enters thechamber.—K. A.
Lamps, Blowpipe. P. and J. Heinz. Pforzheim, Ger-many. Eng. Pat. 18,819, Sept. 18, 1899.
THE claim is for a blowpipe lamp automatically regulatedby the air pressure in the blowpipe, " wherein the valveregulating. the gas supply is actuated by a piston whichis moved so as to open the valve by the air pressure sup-plied by the blow-pipe/, or by " an electro-magnet whichis excited by the current of an electric circuit that is closedby means of the air pressure of the blowpipe.,,—C. S.
Apparatus for the Generation of Gases;] A ConvenientLaboratory. N. J. Lane.
See page 14,
INORGANIC CHEMISTRY.—QUALITATIVE.
Perezol: A New Indicator for Alkalimetry. Duyk.Annales de Chim. Analyt. 4, [11], 372—374.
THE indicator perezol is an alcoholic solution of pipitzahoicacid (or " Perezone ") (5:1000), which occurs to the extentof 5 per cent, in the rhizomes of Pcrezia adnata, a commonMexican plant. The acid is extracted from the coarselypowdered rhizomes by means of toluene or benzene ; onevaporating the solution at a temperature of 50° CM thecompound separates out in orange yellow crystals, which arepurified by recrystallisation, and dissolved in alcohol in theproportion indicated. Jt'erezol is an extremely sensitiveindicator for alkalis. One drop gives on dilution withdistilled water an opalescent liquid, which shows a sharpand immediate rose-mauve colour in the presence of thefaintest trace of alkali. Distilled water after it has beenboiled in a glass vessel gives with this indicator, adistinct alkaline reaction from the trace of alkali dis-solved from the glass. Saliva also gives an alkalinereaction with perezol. Drinking water, from the presenceof alkaline-earthy carbonates, reacts in a similar manner.The reaction towards alkaloids is very sensitive, so that theindicator is specially valuable in alkaloidal determinations..Perezol, sensitized with alkali, is almost equally delicate as areagent for free acid ; not only mineral acids but carbonicacid, and organic acids are indicated by it. Boric acid alonedoes not react with perezol, but does so in the presence ofglycerin. Salts of the mineral acids and of ammonium areneutral towards it, but carbonates, bicarbonates, boratesand acetates react as alkalis. It is more sensitive to alkalithan to acid.—J. O. B.
Gold, Iodometric Determination of F. A. Gooch andF. H. Morley. Ainer. J. Science, SILLIMAX, 8, [4],261—266. Chera. Centr. 1899, 2, [18], 847.
PETERSON (this Journal, 1899, 177) has stated, that in thedetermination of small quantities of gold by titration withsodium thiosulphate, after treatment with potassium iodidesolution, the amount of thiosulphate required is 1], timesgreater than that necessary for the conversion intotetrathionate in the usual May. The author has proved,experimentally, that this statement is incorrect, and thatthe thiosulphate reacts in the usual manner upon the iodineset free by the action of the potassium iodide upon goldchloride.—A. S.
Chromium in Steel, Determination of R. W. Mahon.J . Anier. Chem. Soc. 1899, 21, [H]> 1057—1060.
THE following method embodies various modificationsadopted by the author for this determination:—Three grms.of the sample are dissolved in 50 c.c, of concentrated
hydrochloric acid, and the solution is evaporated to a moistcake. Fifty c.c. of concentrated nitric acid are added, andthe liquid boiled until the nitrous fumes evolved have nearlyceased. When somewhat cooler, it is then treated with4 grins, of potassium chlorate, and again boiled until thevolume is reduced to about 30 c.c. After diluting the solu-tion to 300 c.c, 15 c.c. of ammonium hydroxide (sp. gr.0-90) are introduced, the liquid thoroughly mixed^ andwhen cold, filtered through a ribbed double paper which iswashed with cold water. The filtrate and washings arediluted to about 450 c.c. and titrated with standard solutionsof ferrous ammonium sulphate and potassium permanganate.
In order to avoid reduction of the chromic acid by thepaper, it is essential that the solution should be dilute andcold. It is also necessary to avoid having too much freenitric acid. The results quoted, show that this method willeffect an accurate determination of the chromium in steeland in solutions containing chromium.—C. A. M.
Sulphur in Pig Iro?i, Determination of. M. J . Moore*J. Amer. Chem. Soc. 1899, 21, [11 J, 972—975.
IN most steel and iron works it is customary to pour themolten metal into water to obtain what is known as a "shotsample/, to pulverize this sample in a »steel mortar, and todetermine the silicon and sulphur in the powder after it hasbeen passed through a sieve. Having had occasion to com-pare the composition of samples taken from the cupolas bythe shot method with that of drilled samples from themixer, the author found that apparently the latter containedthe greater percentage of sulphur, whereas the reverse shouldhave been the case. In order to determine the cause of thediscrepancy, comparative determinations were made, bothby the volumetric and gravimetric methods, on samplestaken from the mixer byr the shot method, and those caughtin a sand-mould from the mixer-ladle, and drilled. From-the results of these it appeared that in neither case did thevolumetric method give the whole of the sulphur, and thatthe error was greater in shot samples than in drilledsamples.
The mean results from five samples of steel were:—Sulphur in steel, 0*1; sulphur found in shot samples frommixer; volumetric, 0*060; gravimetric, 0*096 per cent.Sulphur in sand samples, volumetric, 0*084 ; gravimetric,.0*097 per cent.
The gravimetric method used was that given in Blair^s" Analysis of Iron and Steel."
In the author's opinion the difference betweeu the volu-metric results yielded by the two samples is sufficient tocondemn the practice of taking shot samples.
From recent experiments he finds that the error betweenthe gravimetric and volumetric results is not very noticeablewith iron containing less sulphur than a No. 2 grade.
—C. A. M.
Double Phosphates of Ammonmm as Precipitants ofBeryllium, Zinc and Cadmium, in Analysis. M. Austin.Ainer. J. Science, Silliman, 8, [4], 206—216. ChemCentr. 1899, 2, [16], 791.
THE author states that it is impossible to accurately deter-mine beryllium as pyrophosphate, by ignition of the doubleammonium phosphate, precipitated from beryllium solutionsby " microcosmic salt" or by ammonium phosphate andammonium chloride. On the other hand, in presence of10 grms. of ammonium chloride, if the liquid be allowed tostand for an hour, and of 20 grms. if the filtration becarried out immediately after cooling, zinc ammoniumphosphate can be obtained of proper composition yieldingthe pyrophosphate on ignition. This method may there"fore be recommended for the determination of zincCadmium may be determined as pyrophosphate if the prelcipitate produced by microcosmic salt in almost neutral-solution, containing ammonium chloride in the pronortionof 10 grms per 100 c.c, be allowed to stand I Z ^ Zbefore filtration. By this method, a beautiful c rys taZemass of cadmium ammonium phosphate of the requiredcomposition separates from the solution. It is importantthat the reagents added, contain no free acid, and ^ lof ammonia and ammonium salt. A. S.
Jan. si, 1900.] THE JOURNAL OF THE SOCIETY OF OHEMIOAL INDUSTRY. 73
Copper in Cyanide Solutions, Estimation of. J. E. Clennell.
See page 14.
Bismuth from Lead, Separation of J. Clark.
See page 26.
Copper, Analysis of J. Clark.
See page 27.
ORGANIC CHEMISTRY.—QUALITATIVE.
Nitrogen in Organic Substances containing Sulphur,Detection of E. Tauber. Ber. 1899, 32, [16], 3150—3154.I N testing organic substances containing sulphur for nitro-gen, O. Jacobsen has recommended that the substance beheated with excess of iron powder before heating withpotassium. This is not only unnecessary but objectionable,because, in presence of iron, atmospheric nitrogen is takenup forming more or less cyanide according to the intensityand duration of the heating. When considerable excess ofpotassium is employed, reliable results are obtained withoutiron, even when a relatively large amount of sulphur is pre-sent. About 0*02 grm. of the substance is warmed verygently with 0 • 2 grm. of potassium until they are well mixed;the temperature is then raised sufficiently to soften the glasstube, and the heating continued for about two minutes.After dissolving the mass in water, ferric chloride is added.
By heating sodium carbonate or hydroxide with charcoaland iron in a current of nitrogen, the author has succeededin converting from 10 to 25 per cent, of the alkali employedinto sodium cyanide, at temperatures at which in the absenceof iron no nitrogen is taken up. Magnesium, tungsten,chromium, nickel, and copper, were tried in place of iron,but had very little or no effect.
The process with iron was patented bv V. Adler in 1880.—T. E.
Cotton-seed Oil, BecckVs and HalpheiVs Tests for.P. iST. Raikow and N. Tscherweniwanow. Chem. Zeit.1899, 23, [9V], 1025—1028.
FROM the results of their experiments the authors concludethat in Becchi's test the relative amount of silver nitratepresent has a considerable influence on the degree of dis-coloration, whether or no the solution contain colza oil ornitric acid. Thus, in the case of olive oil and walnut oil, adark coloration could be obtained, which varied in intensitywith the proportion of silver nitrate employed.
They also find that the results of the test for cotton-seedoil may be widely different according to whether nitric acidbe present or absent. They consider that of the differentmodifications of the test which they have tried, that of theItalian Scientific Commission is the most reliable. Accordingto this modification, the silver nitrate solution must contain0*04 per cent, of free nitric acid. With more, the reagentis not sufficiently sensitive, whilst with less, olive oil willgive a reaction.
Halphen's reaction (this Journal, 1897, 1045) was foundto be much more reliable than Becchrs test, no colorationbeing obtained under varying conditions with linseed, olive,walnut, poppy, or earthnut oils. The test is, in the author'sopinion, best made in accordance with Halphen's directions,but the heating may also be carried out in an ordinary water-bath, whilst the colour is obtained, though much more slowly,on exposing the mixture to the direct heat of the sun. Theuse of amyl alcohol, as prescribed by Halphen, is advan-tageous, but not essential. Its action, however, appears tobe more than a mere dilution of the liquid or retention ofthe carbon bisulphide in contact with the oil. Althoughcarbon bisulphide by itself may under certain conditionsgive a slight rose coloration with cotton-seed oil, the simul-taneous action of carbon bisulphide and sulphur is requiredto obtain the characteristic reaction. The presence of morethan 1 per cent, of sulphur is stated to be superfluousand to weaken the sensitiveness of the test, when only tracesof cotton-seed oil are present. The smallest quantity ofthat oil which the authors could detect hy this test was0*5 per cent. As in the case of Becchi's test, the sensitive-ness of cotton-seed oil towards Halphen's reagents was
destroyed by heating it with superheated steam or at atemperature of 220° C—C. A. M.
Ether. Detection of Aldehyde in. H. Blaser. Pharm. Centr.E . 40 , 607. Chem. Centr. 1899, 2, [18], 848.
IN the preparation of the Magenta-sulphurous acid reagent(1 :100) for the detection of aldehyde in ether, the Magentais not completely decolorised even by large quantities ofSO2. The use of large quantities of sulphurous acid may,also, have a disturbing influence on the reaction. Theauthor, therefore, recommends the employment of a solu-tion of Magenta (1 : 100,000) which has been completelydecolorised by exposure to sunlight.—A. S.
Azo- and Hydrazone Compounds differentiated by Bromine.H. E. Armstrong. Proc. Chem. Soc. 15, 1899, 243.
ALTHOUGH the constitution of the " oxyazo " compoundshas been the subject of numerous investigations, apparentlychemists are not yet in agreement as to their formulae ;indeed, only recently, Hantzschin Germany, and MacPhersonin America, have arrived at diametrically opposite conclu-sions. The difficulty arises from the fact that parahydroxy-azobenzene—the parent of all "oxyazo " compounds—andquinonephenylhydrazone are unquestionably isodynamic.Methods such as Hantzsch and Farmer have adopted must,
i therefore, be regarded as in principle the only suitable onesfor the determination of structure in such cases, and extremecare must be taken in interpreting interactions.
A number of observations made in the author's laboratoryby Messrs. Panisset, Seligmann, and Isherwood are ofinterest as bearing on the problem.
The stability of diazobenzene in presence of bromine wasestablished by Griess in his earliest investigation. Diazo-benzeneparasulphonate is also untouched by bromine, andaction only takes place gradually as it becomes hydrolysed.Azobenzeue is only very slowly and imperfectly acted onby bromine. Nitrogen, in fact, by no means tends topromote substitution, unless associated with hydrogen.
If oxyazobenzene were parahydroxyazobenzene, onewould expect it to be readily brominated in the ortho-positionrelatively to the hydroxyl; but, as a matter of fact, it yieldsa product convertible into parabromaniline and phenol onreduction, and which is easily prepared from these, a resultonly compatible with the view that towards bromine itbehaves as a hvdrazone.
This view is confirmed by the fact that when the ethylatedcompound is brominated, a substance is formed whichIsherwood finds to be identical with that produced oncoupling orthobromophenol with diazobenzene and thenethylating. It is noteworthy that the bromine is removedfrom this compound with exceptional facility, both whendissolved in acetone, and when left in contact with sulphurousacid.
The behaviour of bromine in excess towards the quin-hydrazones is characteristic. Quinonebromophenylhydrazoneis resolved by it into bromodiazobenzene and tribromophenol,and ordinary Tropecolin into diazobenzenesulphonate andtribromophenol. So complete is the change in this lattercase, that if, after the tribromophenol has been filtered off,phenol be added to the solution, and then alkali, an amountof Tropreolin can be recovered almost equal to that originallytaken.
ORGANIC CHEMISTRY.—QUANTITATIVE.
Marine Animal Oils, Analysis of H. Bull. Chem Zeit1899, 23, [93], 996.
IT is possible to effect a fractional distillation of the mixedfatty acids of these oils by heating them at about 200° C , andpassing a strong current of superheated steam through themfirst at about 200° C , and afterwards at 180°, 160°, 140°, 120°^and 100° C. The various fractions obtained at the differenttemperatures collect in the distillates in the form of colour-less^ to light-yellow liquids, each of which consists of acids ofsimilar molecular weight. Owing to the tendency of theunsaturated fatty acids to become oxidised, and to the factthat the brown oxidised acids are not volatile with super-heated steam, the author prefers to effect a preliminaryseparation by a method based on the difference in solubility
THE JOUENAL OF THE SOCIETY OF OHEMIOAL INDUSTEY. [Jan. 31.1900.
of salts of the acids. The oil is saponified with absolutealcoholic potassium hydroxide, and the potassium saltswhich separate out on cooling are pressed, recrystallised fromabsolute alcohol, and again pressed. The united mother-liquors are concentrated to a smaller volume, cooled and thedeposit collected as before, this process being repeated untilno more solid potassium salt can be obtained. The fattyacids left in the mother-liquor are liberated and saponifiedwith absolute alcoholic sodium hydroxide, and the insolublesodium salts separated in the same way as the potassiumsalts. The alcohol from these second mother-liquors isremoved by evaporation, and the residue treated withanhydrous ether so long as anything dissolves. Thealcohols (cholesterin, &c.) which pass into solution togetherwith the sodium salts of the most unsaturated acids canbe separated by treating the ethereal extract with water,which removes the latter. By recrystallising the residueleft from the treatment with ether from absolute alcohol, anadditional small amount of a solid sodium salt can beobtained, and finally the fatty acids are recovered from thealcoholic filtrate from this.
As an example, the author gives the following resultsobtained from 1 kilo- of white cod-liver oil;—
Patty Acids.
A.—"With potassium salts insolublein alcohol.
E.—With sodium salts insoluble inalcohol.
C,—With sodium salts soluble inether.
IX—With sodium salts insoluble inether.
1Weight.
Grms.33 ro
375-0
120*0
69-0
AcidValue.
194-2
190*0
167'0
169-0
IodineValue.
67*5
135*6
322*4
347*0
The fatty acids A contained nearly the whole of thesaturated acids, together with acids of the oleic acid series.13 consisted of acids of the oleic and linoleic series, and C,in the main, of acids of the series C»H2^-8O2 and
on—in^ o n i n Q?In order to illustrate the method of fractional distillation
with superheated steam, the author gives the subjoinedresults obtained with fraction A :—
Temperature. Weight Acid Value.
100140120100
Grms.83*395' 5
115*714-2
182-0200*0209*0212*0
Iodine Value.
102-662*440'033*0
Saturated fatty acids were present in all the fractions,stearic acid being the principal acid in the first, a mixtureof stearic and palmitic acids in the second, and of palmiticacid and its lower homologues in the third and fourth.
In almost all the oils examined, the author found erucicacid, C22H40O.2, and a new acid of the formula C20H38O2which melted at about 20° C. In liver oil there was alsofound a new acid of the oleic series containing 21 carbonatoms. It melted at 24*5° C, had an acid value of 171*6,and yielded a lead salt readily soluble in ether.
Two highly unsaturated fatty acids were found in herringoil with the formula C^K^O2 and C24H40O2 respectively.Both remained liquid at —20° C. Their respective acidvalues were 179 and 154-9, and their iodine values 344*5and 279. All the highly unsaturated fatty acids separatedby the author had a high specific gravity (about 0-95).
—C. A. if.Acetyl Value in Fat Analysis, Meaning of. J. Lew-
kowitsch. Analyst, 1899, 24, [285], 319—330.IN this paper the author supplements his former communi-cation on this subject (this Journal, 1897, 503). From anumber of experiments he has found that three washingsare sufficient for the acetylated product, prolonged washingcausing slight dissociation, with the result that the acetyl
value will be too low. In determining the value, it is prefer-able to use 5 grms. of the acetylated product, since with thisquantity, 1 c.c. of decinormal potassium hydroxide corre-sponds to about 1 unit in the acetyl value. Every pre-caution must be taken to avoid the introduction of carbondioxide in the distilled water used in either of the methods,and the water used for generating steam should bethoroughly boiled before the steam is passed into thedistilling flask. In the filtration process the separationof the insoluble fatty acids may be facilitated by theaddition of a slight excess of mineral acid, for which anallowance is made in the subsequent titration of the solubleacids.
It is shown in a series of tables that concordant resultsare obtained by both processes in the case of oils whichcontain only a small proportion of volatile acids.
Oils, such as cocoa-nut and palm-nut oils, which containa large amount of acids intermediate between soluble andinsoluble acids, are best examined by the distillation pro-cess, in which the fatty acids have a better chance of beingthoroughly agitated with hot water. At least 600—700 c.c.of the distillate (or filtrate) should also be collected, toinsure that the total quantity of volatile acids is obtained.
From the fact that castor oil, which consists principally ofthe^glycerides of hydroxylated fatty acids, has the highestacetyl value (150), whilst the triglyceride of ricinoleicacid has a theoretical acetyl value of 159*1, this value hashitherto been regarded as a measure of hydroxylated fattyacids.
The author, however, shows that the acetyl value maybe due to other causes than the presence of hydroxylatedfatty acids.
Thus, the presence of an alcohol would also give rise toan acetyl value, which, in this case, would be identical withthe saponification value of the acetate. Since fats or fattyoils rarely contain more than 1 per cent, of cholesterin orphytosterin, the influence of these substances on the acetylvalue will be within the limits of experimental error in themethod, but where considerable quantities of free alcoholsare present, the case is otherwise. This point is illustratedby the figures given in Table L, obtained with a number ofwaxes.
With reference to these results the author states thatwhilst, in his opinion, it is certain that in the case ofcarnauba wax, beeswax, and wool-wax, the true acetylvalue indicates the presence of free alcohols, furtherresearch is required to prove whether this also holds goodfor the other waxes in the table. The figures given in thelast column show that, with the exception of carnaiiba wax,the difference between the saponification values of theoriginal and acetylated substance affords a rough checkon the correctness of the direct determination of the acetylvalue. This approximate correspondence was also observedin the case of ordinary oils and fats, with the exception ofcastor oil, which may be regarded as analogous to earnaubawax.
Since blown and boiled oils have high acetyl values ithas been generally assumed that they contained hvdroxvacids, and the author has therefore examined numeroussamples prepared on a commercial scale and in the laboratory. Some of his results are given in Table I I .
The « oxidised acids » given in the fourth column weredetermined by Fahnon's method, based on their i n s o l u Sin petroleum spirit, a method which the author has fouiSto be valueless m the case of castor oil fattv arid* TTfurther points out that his objections to this m e t Wsubstantiated by the attempts to calculate the amountthe hypothet.cal hydroxy acids from the Cvalue, on the assumption that these a Vl iweight of 300 (the molecular ^ t ^ JCH(OH)O) Theseg ( ecular ^ t ^ JC18H35(OH)O2). These calculated result'multiplying the true acetyl value by f tcolumn IX., and show a great dev2L« *yielded by Fahrion 's metnod ( I V 0 ^note that the difference in the s a iX.) cannot be used as a checkcase of blown and boiled oils
m
a ° e t y l value in
ff? r t h y o£C H o l u n m
i
Jan, si, woo.] THE JOURNAL OF THE SOCIETY OF CHEMICAL INDUSTRY- 75
The specimen of acids from the oxidised linseed oil wasfreed from all substances soluble in petroleum spirit, andthe acetyl value on multiplication by 0*55 should havegiven the theoretical 100 per cent., instead of 71*6 percent., assuming that they consisted of hydroxy acids only.The author therefore concluded that lactonic substances werepresent, the differeuce between the saponification value andthe acid value (199 — 168 = 31) being regarded as a measureof their amount.
In the case of the commercial blown oils, in which thereis an approximate correspondence between the true acetylvalue and the percentage of oxidised acids, the author con-siders that the acetyl value may safely be regarded as ameasure of oxidised acids. But in all the other oils thecalculated oxidised acids are much higher than those actuallyfound, and in the want of definite knowledge as to thenature of the substances causing the high acetyl valuein these cases, the author proposes to describe them us" unknown acids."
The presence of mono- or diglycerides in a fat wouldalso cause an acetyl value. The author has shown in aformer paper (this Journal 1898,1107) that such compoundsdo occur in partially hydrolysed triglycerides, and in anumber of experiments which are given in detail he hasobtained indications of the presence of knrer glycerides innaturally hydrolysed fats.
The uncertainty introduced into the acetyl value by theprobable presence of mono- and diglycerides may heeliminated by determining the acetyl value of the fattyacids as well as of the original fats. If the two values beidentical, one AVOUM infer that only triglycerides werepresent j but if mono- or diglycerides were present thesoccnd value should be considerably lower, provided thatno oxidation occurred in the preparation of the fattvacids. J
The acetyl value might also furnish a measure of therancidity in fats, indicating not only the dissociation of thetriglycerides, but in addition the amount of oxidation Inillustration of this point the author gives (Table I I lS theresults obtained with fats in the fresh state, and 'iftwexposure to the atmosphere.
The results given in the Column XV. show that exposedor rancia tats have a. higher acetyl value than the freshiats. In the case of cacao-butter and curcas oil thiscannot be due to the presence of lower glycerides. but theauthor considers that further work is required to determinef infimtrkKr 4Vir\ T«TS%*U-U ~C X"U . ^__i i . «-vi m i n e
indication of
The final conclusion arrived at is, that inasmuch as th<?acetyl value may be due to a, hy droxy-acids; 6, free alcohols •c oxidised fatty acids ; d, « unknown acids" e, mono- anddiglycende3 5 and f9 rancidity; it cannot be redded as a
76 THE JOURNAL OF THE SOCIETY OF OHEMIOAL INDUSTEY. [Jan. si, woo.
constant until it is possible to chemically differentiatehydroxy acids, oxidised fatty acids, and " unknown acids "and to determine to what extent each of these contributestowards the formation of the value.—C. A. M.
INSTEAD of estimating tannin and the like, and basicdyestuffs by means of comparative dyeings, the authorproposes to make use of the formation of lakes by pre-cipitating the dyestuff on a metallic tannate, since theselakes are practically insoluble in water. The methodsuggested is described in the following example:—Weighedquantities of Safranine T (9*6786 grms.), tannin (11*8322grms.), and antimony oxalate (10 grms.)*are each dissolvedin water. Each of the solutions made up to 1 litre.50 c.c. of the tannin and antimony solutions are mixedand well shaken, and then 50 c.c. of the Safranine solutionare added. After shaking for 15 mins. the mixture isfiltered and the precipitate washed until the wash watersare almost colourless, the filtrate being made up to1 litre. The strength of the solution made by diluting100 c.c. of this filtrate to 1 litre is compared with theshade produced in 1 litre of water by running in sufficientof the original Safranine solution diluted 10 times. Jnthe example quoted, 20-6 c.c. were required, correspond-ing to 0'199378 grm. of Safranine in excess. The 50 c.c.of the original Safranine solution contained 0*48393 grm.of Safranine, hence the difference 0*284552 grm. corre-sponds to the 0-591616 grm. of tannin used. The amountof dilution to be employed depends upon the particularcolour under examination, yellow dyestuffs for examplerequiring to be compared in stronger solutions.—T. A. L.
Beetroot, Estimation of Sugar in. J. Weisber<*. Bull.de l , Assoc, des Chim. de Sucr. et de Dist. 1S99,17 [~3l237—238. '
THE author refers to an extractor invented by F. Poupe, ofPrague, for facilitating the extraction of sugar in testing
XIII.
TrueAcetylValue.
XV.
Difference • Difference
X.-VJII. XIII.-VI.
7*1
7*94144*810'454*41
10-78'9
8*8
124/47#0
10!76-4
- 0*5
+ 9'3+ 2'444- 6'If)4- 6-18
beetroots, but, whilst ad-mitting its superiority tothe older extractors ofSoxhlet and Scheibler, headheres to the opinionthat the only practicalmethod for the control ofthe sugar content of beet-root chips is hot aqueousdigestion carried out withproper attention to sam-pling,, quantity of basicacetate of lead added,temperature of the bathrtime of heating, &c. Thistemperature should not bethe boiling point, as re-cently recommended byZamaron, but 75° to 80° C*at the maximum. Theresults obtained by theextractor fully confirm theaccuracy of those obtainedby hot aqueous digestion,
—L. J. de W.
Starchy New Method forthe Rapid Determina-tion of D. Crispo.Ann. Chim. anal. appl. 4,289—290.
THE author makes use ofthe property of causticpotash of dissolving starchto a clear, stable liquid.3-391 grms, of the starchare made into a paste withwater, washed into a
Jan. 81. woo.] THE JOUENAL OP THE SOCIETY OF CHEMICAL USTDUSTEY.
200 c.c. flask, 50 c.c. of 6 per cent, potash added, withagitation, water added till the flask is f full, the latter heingplaced for 1 hour, with frequent shaking, on the hoilingwater hath. After cooling, the flask is filled up to themark, the liquid filtered until sufficiently clear, and polarisedin a 200 ni.m. tube. The polarhnetric reading in degrees,Ventzke multiplied by six, indicate the percentage ofanhydrous starch.
On examining commercial products by this method, theresults obtained were :—Wheaten starch: 81 ' 3—80• 7—81*9 per cent, of starch, 0*3 per cent of ash, 0*2 per cent,of nitrogenous substances, and 17*9 per cent, of water.Maize starch: 85*45 per cent, of starch, 0*31 per cent, ofash, 0*38 per cent, of nitrogenous substances, and 14*42per cent, of water, llice starch: 85*05 per cent, of starch,0*75 per cent, of ash, 0*50 per cent, of nitrogenous sub-stances, and 14*56 per cent, of water.
The applicability of the method to food-stuffs has yet tobe ascertained, for in these cases, the lcevo-rotatory productsof the action of potash on the nitrogenous substances willhave to be taken into consideration.—A. S.
Starch in Yeasts, Determination of. D. Crispo.Ann. Chim. anal. appl. 1899, 4, 290—291.
THE author's method (see preceding abstract) may be usedfor the determination of starch in yeast. The yeast is firstground up with water, to ascertain whether it depositsimmediately in lumps, in which case it is allowed to standfor some days, until soft, brown, and pasty. 50 grms. ofthe yeast are made into a paste with water ; if necessary,pressed through silk gauze, then suspended in about 2 litresof water, thoroughly agitated and allowed to settle ; after10—20 mins. the liquid poured off, and the washing repeated4—5 times until the liquid is almost clear. The deposit isfinally washed into a graduated flask, so that 1—2 grms. ofstarch are present in 100 c.c. For each grm. of starch,1 grm. of potash is added in solution, the mixture wellshaken, the flask filled with water till f full and placed for1 hour in a boiling water-bath, whereby the thick liquidrapidly becomes thin and yellow. The flask is filled up tothe mark, and the liquid filtered and polarised in a 100 or200 mm, tube. In the latter case, the scale divisions(Ventzke) read off and multiplied by 0*10173 indicate theanhydrous starch per 100 c.c, of liquid. The amount of"moist starch' , is calculated by assuming it to contain18 per cent, of -water; in other words the percentage ofanhydrous starch is multiplied by the factor 1,22. Itwas found by experiment that of the starch present, on theaverage 11 per cent, is lost by the washing, and this mustbe allowed for.
In nine experiments with mixtures of starch and yeast ofknown composition, three gave excellent results, and of theothers, one gave 0*8 per cent, too low, and the remainderup to 0'7 per cent, too high.—A. S.
Glycogen, Preparation and Determination of. A. Gautier.Comptes Rend. 129, [19], 701—705.
THE liver or muscle is coarsely divided, and boiled for 15minutes in one and a half times its weight of water; it isthen pulped, and the pulp boiled in the same water for 30or 40 minutes. The mass is then strained through a cloth,and the solid exhausted with fresh water till the washingsare no longer coloured by iodine-water. The liquid is thenevaporated to half its bulk, about a tenth of it trituratedio a thin paste with mercuric acetate (20 to 25 grms. perlitre of liquid to be treated) and a little potassium acetate,and the paste added to the bulk of the fluid, with constantagitation. A filtered sample must show no further pre-cipitate with additional mercuric acetate. The whole isleft at 18° to 20° C. for 12 hours with frequent shaking,and filtered. The solid is washed with 1 per cent, mercuricacetate solution, and then retains no glycogen. The solutionis now acidified with acetic acid, and poured into an equal.volume of 85 per cent, alcohol, the precipitate washed with33 per cent, alcohol acidulated with acetic acid, redissolvedm water at 70°—80° C, filtered, acidulated with 5 per cent,acetic acid, and 2 per 1000 of common salt added to it; itis boiled, cooled, neutralised, re-precipitated by alcohol,
filtered, and the precipitate washed with alcohol and ether-alcohol and dried. The product of pure glycogen, onlycontaining from \\ to 4 per cent, of water removable at110°—120° C.
Glycogen only appears to dissolve in water; it can beseparated from the "solution" by filtration throughasbestos.—J. T. D.
Formaldehyde in the Free State and in its Compounds;Method for the Detection and Estimation of. G. H. A.Clowes and B. Tollens. Ber. 1899, 32, [_15]> 2841—2848.
THERE are many methods for the estimation of freeformaldehyde, but no process has yet been introducedby which combined formaldehyde, i.e., methylene unitedto two oxygen atoms, could be quickly determined quanti-tatively. Tollens and his collaborators have recently prepareda number of methylene derivatives of the polyvalent acidsof the sugar group (Annalen, 289, 20; 292, 3 1 ; 299*316). It was desirable to devise a method by which thesemethylene groups could be directly determined.
A solutionTcontaining 0-0206 grm. of formaldehyde in1 c.c. was employed. To 2—5 c c. of this solution a filteredsolution of 0*30—0*35 grm. of phloroglucinol in 15 c.c. ofwater and 15 c.c. of strong hydrochloric acid was added;a yellowish-white flocculeut precipitate being immediatelyformed. The mixture was warmed for two hours at 70°—80°C, and on the following day filtered through a Gooch crucible.The precipitate was washed with 60 c.c. of water, dried forfour hours in the water bath, and weighed. Slightly less thanthe theoretical quantity of the phloroglucide was obtained,calculated according to the equation C6H6O:i + CELO =C-HGO3 + H2O. By using stronger hydrochloric acid andwarming for a longer period, quantities in excess of thetheoretical were obtained. The phloroglucide retains asmall quantity of water, about 4- mol., which is lost at110° O.; it is also somewhat soluble in the acid employed.The errors partially compensate one another, the resultingerror being so small that the method would be quite sufficientto determine whether a compound contained 1 or 2 mols.of formaldehyde. Most methylene compounds examinedgave a quantitative precipitation of the phloroglucide whenmixed with 5 c.c. of water and then with a solution of aslight excess of phloroglucinol in 15 c.c. of strong hydro-chloric acid and 15 c.c. of water and warmed for 2 hourson the water-bath at 70°—80° C. Some compoundsexamined, required the use of stronger acid. The filtratefrom the above process must be treated with a little strongsulphuric acid; if further precipitation occurs, the experi-ment must be repeated, using a solution of phloroglucinolin 10 c.c. of water and 10 c.c. of fcstrong sulphuric acid, oreven in 10 c.c. of water and 20 c.c. of acid. The reactionis then successful, secondary reactions do not occur to asufficient extent to interfere with the accuracy of theprocess.
All the substances examined gave results which left nodoubt as to the number of methylene groups present. Thecompounds which are most readily formed were mosteasily decomposed. The methylene derivatives of themonobasic acids are more stable than those of the alcohols,the compounds of acids containing more than one carboxylgroup require the use of very concentrated acid to effecttheir decomposition.—A. C. W.
Ethyl Nitrite, Determination of. R, C. Cowley andJ. P. Catford. Pharm. J. 1899, 63, [1534], 471—472.
Yon the^ determination of the percentage of ethyl nitritein the official spirit and solution, the authors recommenda colorimetric method based on the reaction betweennitrous acid and metaphenylene diamine, resulting in theformation of Bismarck Brown. A standard solution ofsodium nitrite is prepared containing 95 mgrms. of thecommercial (98 per cent.) salt per litre. The colourstandards are obtained by adding 1, 2, and 3 c.c. of thenitrite solution to successive portions of water eachcontaining about 10 drops of dilute sulphuric acid (1 in 3)and 10 drops of a solution of metaphenylene diamine(1 in 200), and finally making each up to 40 c.c. Thesecolour standards correspond to 1, 2, and 3 per cent, of
78 THE JOUENAL OF THE SOCIETY OF CHEMICAL INDUSTRY. [Jan. 3if woo.
ethyl nitrite, and may be kept for constant reference, asthe authors could detect no perceptible change in themafter exposure to daylight for many Aveeks. |
The sample to be tested is diluted to contain 1 grm. in100 c.c, and 1 c.c. of the diluted liquid is immediatelytreated with the test solutions, made up to 40 c.c, allowedto stand for 1 hour for the full development of the colour, ;and then compared with the standards. If necessary the j
samples should be further diluted in order to match thecolour standards
Standard.
Xo. 39
>y —
„ 1
Per Cent.
Dilution of Sample in c.c. to match Standards.
40GO
120
3'0
».
112
2*8
• •50
100
1• •4080
2-0
• •
70
l'7o
• •• •60
1*5
• •
40
1*0
The water used should have been recently distilled orboiled, and the sulphuric acid should be free from nitrouscompounds.— A. S.
T H E author communicates a method for the determinationof the aldehvdic constituents of lemon oil by means of thereaction between those bodies and hydroxylamine, resultingin the formation of oxinies. 10 or 15 grrns. of a 5 percent, (by weight) solution of hydroxylamine hydrochloridein 80 per cent, alcohol are made up to 250 c.c, and thehydroxylamine determined in 25—50 c.c. of this dilutesolution by titration with -1- normal XaOH in the usualmanner, using first Methyl Orange and then phenolphthalemas indicators.
A similar weight of the strong solution of hydroxylaminehydrochloride is mixed with a known weight of the sampleof lemon oil, and the mixture diluted with absolute alcoholfree from aldehyde until a clear solution is obtained. From0*5 to 1 grm. of sodium bicarbonate is added, the solutiontransferred to a 150 c.c. flask, and heated for 45 inins.on the water-bath under a reflux condenser. The solutionis cooled, washed into a 250 c.c. flask with distilled water, thecondenser also being thoroughly rinsed, the aqueous layercompletely shaken out, and made up to 250 c.c.; 25 c.care measured off, dilute hydrochloric acid added in presence-of Methyl Orange until a faint rose colour is produced, andthen -j-1- normal NaOTI to complete neutrality. Phenol-phthalein is next added and titration continued in the usualmanner with the T
J- XaOH. The number of c.c. of NaOlIrequired after the addition of the phenolphthalein, multipliedby ten and substracted from the number of c.c. used inthe titration of the hydroxylamine solution alone, indicatethe amount of hydroxylamine consumed by the aldehyde.This amount multiplied by 0'0152 or 0*0154 gives thequantity of citral or citronellal in the weight of lemon oiltaken. Using this method, the author found that naturallemon oil contains approximately 5 per cent, of citral.
—A. S.
Salt-forming Alkaloids, A Simple Alhalhnetric Method forthe Estimation of with Phenolphthalehu H. M. Gordin.Ber. 1899, 32, [15], 2871—2876.
T H E principle of the present methods in use for thealkaliraetric estimation of alkaloids, is the solution of thebase in standard acid and titration of excess by standardalkali* With many alkaloids the final reaction is veryuncertain, and when the solution is coloured by smallamounts of foreign bodies, as is often the case, the methodbecomes quite useless.
When the alkaloid periodides are precipitated fromaqueous solutions in the presence of acid by a solution ofiodine in potassium iodide, an equivalent of the acid isprecipitated with the alkaloid, (The general formula ofa periodide is (Alk. H I ) m I n ) . Similarly, if the acidsolution is precipitated by Mayer's reagent, the generalformula of the double salt formed, is (Alk. H I ) m (Hgl«)n.Thus, if an alkaloid be dissolved in excess of standardacid and precipitated by neutral Wagner's or Mayer's
reagent, titration of the excess of acid in the filtrate willat once give the acid neutralised by the alkaloid* Theend reaction is sharp, since only traces of alkaloid arepresent. That reagent should be used which causes mostcomplete precipitation; to decide which to employ, addeach reagent to the filtrate from the precipitate producedby the other. If both give an equally complete precipita-tion, Mayer's reagent is to be preferred, because itsprecipitates settle more quickly.
It is convenient to employ - ^ N" acid and alkali; theseshould be made exactly equivalent, phenolphthalem beingthe indicator. The acid is best standardised against apure alkaloid. About 0*2 grm. of pure anhydrousmorphine is dissolved in 30 c.c. of acid in a 100-cc.flask ; then the iodine solution (10 grms. of I and 15 grins,of KI in 1 litre) is added a little at a time, with continualshaking, until no further precipitation occurs and the liquidappears dark red. The volume is made up to 100 c.cand the flask well shaken until the precipitate settles,leaving a completely clear liquid. This is filtered, 50 c.c.are decolorised by a few drops of 10 per cent, thiosulphate,and the excess of acid titrated. The acid is thusstandardised in terms of morphine; its equivalency toother alkaloids can then be calculated. The results quotedare quite satisfactory. Berberine cannot be estimated bythis method ; the acid present appears to take no part inthe precipitation of this alkaloid; a solution of freeberberine may even be completely precipitated by con-centrated potassium iodide solution without any additionof acid. In solutions of colchicine, precipitation by meansof the alkaloid reagents only occurs in the presence of anexcess of acid so great as to be unsuited to an accurateestimation; this alkaloid may be readily estimated byhydrolysis with standard potash and titration of the excessof alkali.—A. C. \V.
LIQUID sulphur dioxide dissolves the most diverse bodies,organic and inorganic; the solutions are often coloured,though both solvent and dissolved substance are colourless.Reactions between dissolved substances take place so readilythat a condition of electrolytic dissociation is indicated.This is confirmed by measurements of electrolytic con-ductivity ; the solutions of simple salts examined, conductwell and often better than the aqueous solutions. Thedegree of dissociation, as indicated by the conductivitymeasurements, may be confirmed by the boiling-pointmethod. Most unexpected results were here obtained, whichshow that a comprehensive examination of the solutions inthis solvent is required, to decide whether it acts chemicallyupon the dissolved substance and whether polymeric ions donot exist in the solutions.
The following compounds are readily soluble in liquidsulphur dioxide. .Salts :—KI (yellow), Nal (yellow), NH I(yellow), KbI (yellow), S(CH3)3T (yellow), NYCHAJ(yellow), X(C 2 H 6 ) 4 I (yellow), KBr, NH 4CNS, NH,(CH,f6lNH,(CH3)2C1, NH(CH3)SC1, N(CH3)4CJ, N(CH,)*Br, FeCL(yellowish-brown), cobalt sulphocyanide (blue). Hydro-carbons :— Benzene, toluene, triphenylmethane, diphenyl(yellow), fluorene (yellow), phenanthrene (yellow), naph-thalene (yellow), nitrobenzene (greenish), limonene (yellow)pinene (yellow). Less soluble are anthracene (yellow)*β-dibromonaphthalene (yellow) ; ligrom and iodoform arealmost insoluble. Alcohols (readily soluble) : All fattyalcohols from methyl to capryl alcohol, benzyl alcoholmenthol, borneol, o-cresol (yellow), β-naphthol (yellow,),
Jan. 31,1900,] THE JOURNAL OF THE SOCIETY OF CHEMICAL INDUSTRY. 79
(blood-red), β-naphthylamine (orange), phenyl - j8 - naph-thylamine (blood-red), benzidine (orange), chrysaniline(orange), carbazol (yellow), quinoline and pyridine (yellow),acetanilide, formamide (yellow), acetnaphthalide (^yellow)*The solutions are colourless unless the contrary is stated.
Reactions.—Solutions of potassium iodide and trimethyl-aminonium chloride give a precipitate of insoluble potassiumchloride. Solutions of potassium iodide and α-bromisobutyricacid precipitate the insoluble potassium α-bromisobutyrate.Addition of a solution of ammonium sulphocyanide to adilute solution of anhydrous ferric chloride produces adeep blood-red coloration. Solutions of ferric chloride andsalicylic acid give a violet-brown coloration different tothat observed in aqueous solution.
Electrolytic Conductivity of Salts.—The conductivities ofsolutions of the following salts in liquid sulphur dioxidewere determined at 0° C. for different concentrations :—KI, Nal, X H J , KbI, S(CH 3) 3I, N(C 3H 3) 4T, N(C 2 H 5 ) 4 I,KBr, KCNS, NH 4CNS. For comparison, the conductivitiesof eight of these salts at 0° C. in aqueous solution werealso measured. The conclusions to be drawn from thesemeasurements are : 1. The salts show throughout so con-siderable a conductivity in sulphur dioxide solution thatthis must be regarded as a good ionising medium. 2.Certain salts (S(CH 3) 3I, N(CH3)4T> N(C 2 H 5 ) 4 I) possessa greater conductivity than in aqueous solution at the sameconcentration. 3. Analogously constituted salts show differ-ent increases of molecular conductivity with increasingdilution. 4. In aqueous solution the iodides of potassium,rubidium, and ammonium have almost the same conductivityat equal concentrations, but in sulphur dioxide solution theammonium salt has a considerably lower conductivity thanthe other two. 5. In aqueous solution the conductivitydecreases with increasing complexity of the (positive) ions ;in sulphur dioxide solutions the reverse is the case. 6.The rate of increase of conductivity for increasing dilutionis very different in the two solvents; hence the degree ofdissociation at the same concentration must be different.7- The velocity of the ions is also different in the twomedia.
Franklin and Krause have examined liquid ammonia asa solvent. See this Journal, 1899, 180, and Arner. Chem.Journ. 20, 848.—A. C. W.
X-Rays, The Chemical Action of. P. Villard. ComptesRend. 129, [22], 882—883.
AVHKS* a Crookes tube has been in action for some time,it acquires a violet tint over the portion of the surfaceexposed to the cathode rays. By surrounding the anodeof a focus tube with a wide tube of either lead-glass orordinary glass, the author found that the lead-glassblackened rapidly when the tube was in action, throughreduction of the lead ; but when it was previously linedwith a thin coating of aluminium, which is opaque tocathode rays, but transparent to X-rays, there was nolonger blackening, the glass acquiring the violet tint men-tioned above. This effect, which seems to be due to oxidation,is therefore clearly due to the X-rays.—J. T. 1).
Liquid Mixtures of Constant Boiling Point, A Contributionto the Study of Garnett Kyland. Amer. Chem. J . 1899,22, [5], 384-396.
TITE author has examined a series of 80 mixtures of pairsof liquids mutually soluble in all proportions, and twomixtures the components of which have limited mutualsolubilities ; of the former class, 45 of the mixtures werefound to distil at a constant temperature at or below theboiling point of the more volatile constituent, two at aconstant temperature above the boiling point of the lessvolatile constituent, whilst in one case the constant dis-tilling temperature was situate between the boiling pointsof the constituents, and with three of the mixtures theresults were uncertain.
The conclusions arrived at are :—1. The large proportion of constant boiling mixtures
found, show that this phenomenon is more common thanhitherto supposed, and in fractional distillation shouldalways be guarded against.
2. The changes in the composition of the distillates,corresponding to the changes in pressure and temperatureof the distillation, indicate that the two mixtures investigated(benzene with either methyl or ethyl alcohol) are not truechemical compounds, and that any approximation tomolecular proportions must be regarded as accidental.
3. Mixtures of liquids partially soluble in each other, distilat a constant temperature, but as long as there are two layersof liquid in the distilling vessel there is a deviation fromthe law for mutually insoluble liquids which distil in theratio of the products of their respective vapour densitiesand vapour tensions at the temperature of distillation.
4. With mixtures of liquids soluble in all proportions,the results in general indicate that the above law (see 3)is more or less modified by the mutual influence of thecomponent liquids. In those cases examined, the largestdeviation was found with a mixture of propyl alcohol and
under 762 mm. pressure;7 6 ° 7 7 °benzene,which distils at 76the proportion of alcohol to benzene in the distillate is16-5 : 83'5, the theoretical ratio at 80° being 28*5:71 e 5.For carbon bisulphide and acetone, boiling at 38 • 5°—39*5°(766 mm.), the ratio found is 74 : 26, the theoretical valuebeing 66:34 (at 40°) ; whilst a mixture of carbonbisulphide and ethyl bromide, boiling at 37°—38° (770 mm.),gives a ratio 32:68, the theoretical number for 37*5°being 35 : 65.—T. H. P.
eSalt Solutions, Action of Magnesium on. D. Tommasi.
Bull. Soc. Chim. 1899, 21, 885—887. (See also G.Lemoine, Comptes Rend. 1899, 129, 291.)
Potassium Chloride.—When a solution of potassiumchloride is treated with magnesium, hydrogen is evolvedand the liquid becomes alkaline. The chloride is notdecomposed, but favours the oxidation of the magnesium tomagnesium hydrate by the water.
Ammonium Chloride.—In ammonium chloride solutionf
magnesium is violently attacked, with evolution of hydrogenand formation of the double chloride of ammonium andmagnesium.
and
Calcium, sodium, and lithium chlorides behave likepotassium chloride.
Magnesium chloride, as also the chlorides of copper,cadmium, lead, and iron (ferric), give hydroxychlorides, andin some cases magnesium chloride.
Ferric chloride is not reduced.Barium and strontium chlorides are hardly acted upon.Cobalt and chromic chlorides give magnesium chloride ar
hydrate of cobalt or chromium.Copper chloride is not reduced to the metal; lead only
partially, but gold and platinum are Avholly reduced.Cupric sulphate at 0° C. is reduced, and gives only
cuprous hydrate; at higher temperatures, hydrogen isevolved, and, besides cuprous hydrate, the basic sulphate,metallic copper, and magnesium sulphate are formed. '
Zinc, ferrous and manganous sulphates give thecorresponding hydrates, hydrogen and magnesiumsulphate.—J. MeC.
Rhamninose : A Saccharose from Xanthorhamnin C andG. Tanret. Comptes liend. 129, [19], 725—728.'
BY fermenting at 45°-70° C. an aqueous solution ofxanthorhamnin with the ferment discovered in Persianseeds by Liebermann and Hermann and by Marshall Wardand Dunlop (whiclrthe authors propose to call rhamninase^a saccharose is obtained having the composition C H Owhich becomes hydrolysed under the influence of dilute adds 'forming two molecules of rhamnose and one of galactoseRhamninose is soluble in water and in alcohol, slightly so inglacial acetic acid, insoluble in acetone or acetic ether I thas a sweetish taste, is laevo-rotatory ( [ a ] D = — 4i<>\* , l n
crystallisable, and melts with decomposition at 140° C Tthas one-third of the reducing power of an equal weight ofglucose, is unacted on by most of the usual ferments, andgives no insoluble hydrazone or osazone with phenvlhvdrazine. Sodium amalgam reduces it to rhamninite C H( [«] D = - 57°), which with dilute sulphuric acid hydrolv*rhairinose and dulsite (C,sH^O,a + 2H«O — 9P TT
80 THE JOURNAL OP THE SOCIETY OF CHEMICAL INDUSTBY. [Jan. a.
C6H14O6) ; but whilst the yield of rhamnose is the theoretical,that of dulcite is only about half of that shown by theequation. The oxidation of rhamninose by nitric acid yieldsmucic and galactonic acids, that by bromine water arhamninotrionic acid, C18H3.2O13, lsevo-rotatory, monobasic,hydrolysed by dilute sulphuric acid into rhamnose andgalactonic acid (ClsH,o015 + 2H2O = 2C6H,o05 + Ct)HrO7).
—J. T. b.
Methylene Sulphate. M. Delepine. Comptes Rend. 129,[21], 831—833.
BY acting on formaldehyde with fuming sulphuric acid,-white crystals of methylene sulphate are obtained: CHX)+ HoSoO- = SOo.OXHo + H.SO4. This substance~isstable at the ordinary temperature, nearly insoluble in allthe usual neutral solvents, save acetone ; melts with decom-position about 155: C., and, if maintained at this temperature,it breaks up into sulphur dioxide and trioxide, carbonmonoxide, water, and formaldehyde. It is hydrolysed at60° —70° C , by water or alkalis, yielding sulphuric acid andformaldehyde. Alcohols, at the same temperature, producesulphuric acid and the formal and alkylsulphuric acidcorresponding to the alcohol used. The author has preparedin this way dibenzylic formal, CH2 (OC7H7)2, and severalsalts of benzylsulphuric acid- The higher homologues offormaldehyde behave quite otherwise with fuming sulphuricacid.—J. f. D.
Glycerin, The Speed and Limits of Esterificatioii of byPhosphoric Acid. H. Imbert, and G. Belugou. Bull.Soc. Chim. 21, 935 — 939.
THE speed of esterification, and the limit of the amount ofglycerophosphoric acid formed by the reaction of molecularproportions of phosphoric acid and glycerin, depend on thestate of hydration of the acid (the reaction being hinderedby the presence of water), and on the temperature (boththe velocity of reaction and the ultimate amount of glvcero-phosphoric acid formed being much greater at 105 C. thanat 50° C. or 15" C ) , The yield of glycerophosphoric acid,however, depends also on the time; it very soon reachesa maximum, then diminishes to a minimum, and increasesagain more slowly to a maximum limit. For molecularproportions at 105° C , the percentage of the total acidesterified is 22*74 immediately after mixture, 4 '78 after1 hour, 12*40, 43'12, and 42*87 after 4, 45, and 75 hoursrespectively. Prunier and Portes, process, then, for pre-paring glycerophosphoric acid by heating to 110° C. for sixdays, a mixture of syrupy phosphoric acid and commercialglycerin gives a good yield, since the high temperaturedehydrates the mixture, and the long time allows themaximum limit to be reached.—J. T. D.
Double Iodides of Mercury and Ammonium or Potassium,Dissociation of, by Water. M. Francois. ComptesBend. 129, [23], 959—962.
W H E N a small quantity of water is poured upon thesedouble salts, dissociation occurs, mercuric iodide beingdeposited ; but the action ceases when a certain limitingproportion of alkali iodide to double salt in the solutionis reached. Further addition of water does not change thisas long as any of the double salt remains undissolved.Moreover, the action is reversible, the same limit beingreached when strong solutions of alkali iodide are left incontact with excess of mercuric iodide for forty-eighthours. If a large excess of water be added, however, com-plete dissociation occurs, mercuric iodide being deposited,and the supernatant liquid then consists simply of a solutionof mercuric iodide in the alkali iodide.—J. T. D.
Styrolene : Transformation into Metastyrolene under theInfluence of Light. G. Lemoine. Comptes Rend. 129,
,719—722
exothermic action, which takes place equally, though moreslowly, in the dark.—J. T. D.
EDUCATIONAL.
Ascough Scholarship. Chem. and Druggist, Jan. 6, 1900.
T H E daughters of the late Mr. Jesse Ascough, of The Grange,Handsworth, have offered the University of Birmingham adonation of 1,000/. to found a scholarship in chemistry atthe University, to be called the Ascough Scholarship.
THE author has investigated the rate of polymerisation ofstyrolene when layers of different thicknesses were exposedto sunlight, and has compared this with the rate at differedtemperatures in the dark- He concludes that sunlight has<no specific action on styrolene, b t m«rety accelerates an
LEXICON DER KOHLENSTOFF-VERBINDUNGEN. Von M. M.BICHTER. Zweite Auflage der " Tabellen der Kohlenstoff-verbindungen nuch deren empirisclier Zusammensetzunggeordnet." Achtzehnte bis 27te Lieferung. Verlag vonLeopold Voss, Hamburg and Leipsic. 1899, PriceM. 1.80 per Number (Lieferung). Williams and Nor-gate, 14, Henrietta Street, Co vent Garden, London.H. Le Soudier, Paris. G. E. Stechert, New York.
SEE this Journal, 1899, 1162. Lieferungen 18 to 27 ofthis Lexicon may now be had.
A N INTRODUCTION TO ANALYTICAL CHEMISTRY. By Prof.G. G. HENDERSON, D . S C , M.A., and Mr. A. PARKER.B.Sc, the Glasgow and West of Scotland TechnicalCollege. Blackie and Son, Limited, 50, Old Bailey,London, E.C.; also Glasgow and Dublin. 1899. Price55.
SMALL 8VO volume, containing preface, table of contents,introduction, and 210 pages of subject-matter, an appendixon " Chemical Equations," Appendix I I . (Atomic Weights),tabular diagram of Spectra, and the alphabetical index.The pages contain a few illustrations. The subject is sotreated as to combine elementary qualitative and quantita-tive analysis, adding also a concisely described method ofpreparation of a well-known salt, when a metal is con-sidered. Acidimetry and alkalimetry and the principlesof general volumetric analysis are described.
OPTICAL ACTIVITY AND CHEMICAL COMPOSITION. By Dr*H. LANDOLT, Professor of Chemistry in the Universityof Berlin. Translated, with the author's permission, byJohn McCrae, Ph.D. Whittaker and Co., 2, White HartStreet, Paternoster Square, London. 1899. Price 4.9. 6d,66, Fifth Avenue, New York.
CONTAINS preface, title and contents, and subject-matterfilling 153 pages, concluding with an alphabetical index.This little work forms what is practical!}' the sixth chapterof the first volume of Graham-Otto's <c Lehrbuch derChemie.', The contents are classified as follows :—I. GeneralPrinciples of Optical Activity. I I . Connection between theRotatory Power and the Chemical Composition of CarbonCompounds. III . Connection between degree of Rotationand Chemical Constitution.
LES SUCRES ET LEURS PRINCIPATJX DERIVES. Par L.MAQUENNE, Professeur au Museum d'Histoire Naturelle.Georges Carre et C. Naud, Editeurs, 3, rue Racine 3*Paris. 1900. Price 16 fr.
THIS work, on "The Sugars and their Principal Derivatives,"is an 8vo volume, with preface, 1,010 pages of subject-matter, table of contents, and the alphabetical index ofsubjects. The subject-matter is divided and classified into
^ ^— — — i r . - ^ . „. Tetrites. iii. Pentites.iv. Hexites. v. Alcohols of Higher Atomicity A 6. vi.Cyclic Polyalcohols. PART III . Keducing Sugars, chap. i.Generalities, ii. Trioses and Tetroses. iii. Pentoses, iv.Hexoses. PART IV. Hydrolysable Sugars. PART V. Acidsderived from Sugars. PART VI. Various Compounds,chap. i. Osozones. ii. Saccharines, iii. Osamines. *
Jan. 31, woo.] THE JOURNAL OF THE SOCIETY OF CHEMICAL INDUSTRY. 81
LUBRICATION AND LUBRICANTS : A TREATISE ON THETHEORY AND PRACTICE OF LUBRICATION, AND ON THENATURE, PROPERTIES, AND TESTING OF LUBRICANTS.By LEONARD ARCHBUTT (Chemist to the Midland Rail-way Co.) and R. MOUNTFORD DEELEY (Inspector ofMotors and Boilers, Midland Railway Locomotive De-partment). Charles Griffin and Co., Ltd., Exeter Street,Strand, London. 1900. Price 21s.
LARGE 8VO volume, containing preface, table of contents,list of tables employed in the text, and subject-matterfilling 427 pages, followed by an alphabetical indexof subject-matter. The text is illustrated with 123 woodengravings, and upwards of 96 tables are given. Thesubject-matter is classified in chapters, devoted as follows :—I. Friction of Solids. II. Liquid Friction, or Viscosity,and Plastic Friction. III. Superficial Tension. IV. Theoryof Lubrication. V. Lubricants : their Sources, Preparation,and Chief Properties. VI. Physical Properties andMethods of Examination of Lubricants. VII. ChemicalProperties and Methods of Examination of Lubricants.VIII. Systematic Testing of Lubricants by Physical andChemical Methods. IX. Mechanical Testing of Lubri-cants. X. Design and Lubrication of Bearings. XLLubrication of Machinerv.
Cratit Report*OFFICIAL NOTICES.
T H E EXPORT OF EXPLOSIVES.
The following Proclamation is published in the Gazetteof January 12th:—
B Y THE QUEEX.—A PROCLAMATION.
Victoria, R,Whereas by " The Customs and Inland Revenue Act,
1879," Section 8, certain goods may, by Proclamation orOrder in Council, be prohibited either to be exported orcarried coastwise : And whereas We, bv and with the adviceof Our Privy Council, deem it expedient and necessary toprohibit the goods hereinafter mentioned to be exported orcarried coastwise ; We, by and with the advice aforesaid, doherebv order and direct that from and after the date hereof,the following goods, being articles which We have judged-capable of being converted into or made useful in increasingihe quantity of Military Stores, that is to say :—Picric acid(Trinitro-phenol), Trinitro-cresol, Carbolic acid (Phenol),Cresylic acid (Cresol), shall be, and the same are hereby,prohibited either to be exported from the United Kingdomor carried coastwise-
Given at Our Court, at Osborne House, Isle of Wight,this eleventh day of January, in the year of ourLord one thousand nine hundred,-and in the sixty-third year of Our Reign.
G O D save the QUEEX.
COAL PRODUCTS AND THE WAR.
Bd. of Trade J., Dec. 30, 1899.
The following notice has been issued by the ForeignOffice :—" Information has been received that agents fromthe Boer Government are endeavouring to purchase some ofthe residual products of gasworks. All manufacturers arewarned to be cautious as to accepting such offers topurchase coming from any new or unknown quarter, as itmay amount to the offence of trading with the enemy/ ,
TARIFF CHANGES AND CUSTOMSREGULATIONS.
DUTY ON ALKALOIDS.
Bd. of Trade J., Jan. 4, 1900,The Board of Trade have received, through the Foreign
Office, a copy of a Spanish Koyal Order of the 6th ultimo,determining the duties chargeable upon alkaloids, asfollows :—
1. Alkaloids and their salts imported in a pure conditionand contained in capsuks are dutiable under section 104 of
the Customs Tariff—" Minimum Tariff "—duty, 30 pesetasper kilo.
2. Alkaloids mixed with other substances and formingpharmaceutical products, are dutiable either under section118 of the Customs Tariff as " pills, capsules, medicinaljujubes, and the like,5, or under section 119 as "pharma-ceutical products, not specified—" Minimum Tariff "—duty,2 pesetas per kilo, and 1 peseta per kilo, respectively.
SPAIX : TARIFF EEVISION.
Bd. of Trade J., Jan. 11, 1900.The classification of petroleum, &c, is now as follows :—
Articles.Rate ofDuty.
Petroleum and mineral oils which on dis-tillation at 300° C. leave more than 80 percent, of residum Per 100 kilos,
DoM do., from 20 per cent, to 80 per cent,inclusive - . . »
Do., do., less than 20 per cent „Naphtha, mineral lubricating oils, vaseline,
and mixtures of these articles with animalor vegetable oils or fats „
Benzine, gasoline, and the like Per kilo.
Peseta 3
30'00
25-0037*00
50*0000-75
The following alterations have been made in theclassification of certain kinds of glassware :—
Glass and crystal in sheets for windows* •. . Per 100 kilos. 35*00Do., for cupboards and glass for mirrors, . . . „ j 45'00Glass and crystal, coated with mercury,
silver, or platinum Per kilo. 1*00
In the class of metals, the only alterations of importanceappear to be that wrought-iron tubes, of all kinds, includinggalvanised and those coated with sheet brass, are nowdutiable at the rate of 24 pesetas per kilo., and that newheadings have been formed for nickel, cobalt, and aluminiumin lumps, bars, sheets, and wire (duty 25 pesetas per 100kilos.). Manufactured articles of the same metals pay2 pesetas per kilo. Articles nickel-plated or coated with cobaltnow pay 1,25 pesetas per kilo., and gilt or silvered wares1 *75 pesetas per kilo.
In Class ILL (chemicals, drugs, &c.) there are severalalterations. Vegetable products not specially mentionedare now dutiable at the rate of 25 pesetas per 100 kilos.,if used exclusively in medicine, and at the rate of 15 pesetasif not so used. The duty on varnishes has been increasedto 30 pesetas per 100 kilos., on starch to 25 pesetas, onmineral and vegetable wax to 40 pesetas if in lumps, and to55 pesetas if manufactured; on perfumery the duty hasalso been raised to 2*50 pesetas per kilov
The following new headings appear amongst others inthe group of chemicals :—
Articles. Rate ofDuty.
Acetic and pyroligneous acid Per kilo.Citric and tartaric acid, citrate of calcium,
tar t ra te of potassium, &c 9>Phenol and naphthalene 9fCarbide of calcium ffChlorate and chromates of potash and
soda, &c, MSealing wax of all kinds nSulphate of potash and ammonia, nitrate of
soda, calcium phosphate, Stassfurt saltsand Thomas slag Per 100 kilos.
Peseta.0-50
0*400*60
0'250'20
0'10
UNITED STATES,
Customs Decisions.Bd. of Trade J., Jan. 4, 1900-
Fulminate of Mercury—Canadian Duties and InternalRevenue Tax not Elements of Dutiable Value.--As Canadian
82 THE JOURNAL OF THE SOCIETY OF CHEMICAL INDUSTRY. [Jan. 31, 2000..
duties and internal revenue tax are not exacted in Canada onnitric acid, mercury, and alcohol imported from the UnitedStates and consumed in the manufacture in bonded ware-house in that country of fulminate of mercury, such dutyand tax are not elements of the dutiable value of the articleon importation from Canada into the United States.
IMPORT DUTY ON ACIDS IN BRAZIL.
Bd. of Trade J., Jan. 4, 1900.
TariffNo.
Articles.
Old Rate. New Rate.
R-itesDuty. ' of I Duty.
{ j Duty. •
Ratesof
Duty.
178 Acids— ; Reis.! Hydrochloric or mil- ji riatic—; Pure kilo. 150
Impure! „ ; 50Sulphuric, oil of i
vitriol— ;Pure „ 150Impure . , . . „ 50
PerCent.
2525
2525
Reis.
12030
32030
PerCent,
PROHIBITION OF IMPORTATION OF CALCIUM CARBIDEINTO SJERVIA.
Bd. of Trade J.y Jan. 13, 1900.The Board of Trade have received notice through the
Foreign Office to the effect that the importation of calciumcarbide into Servia has been prohibited, on the ground thatthis preparation is utilised for the manufacture of gas, andthat its sale is, consequently, an infringement of theGovernment's petroleum monopoly.
EXTRACTS FROM DIPLOMATIC AND
CONSULAR REPORTS.
AUCTION OF QUININE IN BATAVIA, JAVA.
Bd. of Trade J., Jan. 4, 1900.The United States Consul at Batavia reports that the
efforts which have been made in Batavia to sell the productof the Java plantations independently of the trust in Europe,have been crowned with success, and the first public auctionin Java of sulphate of quinine will take place about the endof January or February next.
The following will" be sold: (1) about 5,000 to 6,000kilos, of sulphate of quinine, satisfying the requirements ofedition 2 of the Pharmacopea Neerlandica ; (2) about 1,000kilos, satisfying the requirements of the PharmacopeaNeerlandica, edition 3. The lots will be as follows : (a)cases of 25 tins, containing each 1 kilo, net, making 25kilos, net; (6) lots of 2 enses of 4 tins of 2*835 kilos, each,making a total of 22*68 kilos.
RUBBER INDUSTRY IN LAGOS.
Bd. of Trade J., Jan. i8, 1900.
The rubber industry in Lagos will, it is feared, havelittle, if any, importance for some few years. The reportrecently issued by the Colonial Office says that this is dueto the reckless way in which the sap has been collected.In many instances the trees have been cut down, and inother cases the incisions have been made so very deep thatthey have caused the death of the trees. The formation ofplantations of the Kickxia Africana is the only way toresuscitate the rubber trade, and one European "firm hasalready taken up the matter. The natives also havepromised to do their best to conserve the few remainingtrees, and, under the direction of the Superintendent ofWoods and Forests, nurseries of the various rubber-yielding plants have been established in different parts ofthe Colony and Protectorate. In this way there are, it maybe, reasonable grounds for hope that the export of' rubberwill resume its former dimensions within the next sevenyears.
CIDER MANUFACTORIES IN GERMANY.
Bd. of Trade J.y Jan. 18, 1900.The Belgian Consul at Cherbourg writes that for
years large cider factories have been founded in Germany-on the model of those which have been working inNormandy for the last 20 years. The German ciderfactories buy large quantities of cider apples, and manytruck loads are imported into Germany.
As Germany is a country where beer is the chief beverage^and where the consumption of cider is relatively small, itis concluded that most of the cider made in Germany isintended for export.
It is to be noted, says the Belgian Consul, that the manu-facture of cider is a very remunerative industry, and itmust indeed be so, since the German factories pay theirway in spite of the considerable cost of carriage of applesby rail.
MINERAL EXPORTS OF NEW CALEDONIA.
Foreign Office Misc. Series, No. 520, Jan. 1900.The following table shows the quantities of minerals
The following manures are used in Sou(h Australia :—Phosphate of Lime.—Under severe cereal cropping, phos-
phoric acid is most likely to become deficient, hence about90 per cent, of the manures used in the colony containphosphates. The form most commonly and profitably usedis mineral superphosphate, which is sold guaranteed tocontain between 35 and 38 per cent, soluble phosphate oflime, and costs about 41. 17s. 6d. per long ton (2,240 lb.).This manure is chiefly drilled in with the seed, at the rate ofbetween 80 and 112 lb. to the acre.
Bone superphosphate or vitriolised hone costs about51. 15s. per long ton. I t is not, however, used largely forcereal crops, as the land does not in the majority of casesrequire nitrogen. The results generally are not as good aswhen mineral superphosphate is used, unless the soil is-deficient in nitrogen.
Basic slag or Thomas phosphate contains 25 to 40 percent, of phosphate of lime, and is sold for 3/. 10s. per longton. The value depends largely on its fine state of division^80 to 90 per cent, should pass through a sieve of 10,000meshes to the square inch. This fertiliser has not crivensuch general satisfaction as mineral superphosphate. <jwin<*to the light rainfall, South Australian soils are usually fullysupplied with lime, but are deficient in moisture. On someclays poor in lime, peaty and light sandy soils, it has paidwell, but in general it is a profitable manure only for specialland. • * J r
Bone dust or meal is seldom used for manure, as theaction of the phosphates is too slow and not suited to alight rainfall.
Nitrogenous manures do not claim much importance inthis colony, on account of the regular practice of fallowing
f j r «s tarsal s-JSsupply of nitrogen will be sufficient for some years to
Jan.3i, 1900] THE JOURNAL OF THE SOCIETY OF CHEMICAL INDUSTRY. 83
crops are required. The general potash manures employedare kainit, wood ashes, and muriate of potash.
In place of broadcasting the fertilisers, the system ofsimultaneously drilling-in manure and seed is used. Thispractice will probably revolutionise the wheat-growingindustry, for less than half the amount of fertiliser isrequired per acre in the combined process, and, again, mostof it is at once available as a plant food. Practically allthe drills are made in the United States or Canada.—J. L. B.
GENERAL TRADE NOTES.
A COMMITTEE ON PATENTS.
Chem. and Druggist, Jan. 20, 1900.Mr. Ritchie, President of the Board of Trade, has ap-
pointed a Departmental Committee " to consider varioussuggestions which have been made for developing thebenefits afforded by the Pateut Office to inventors, andreport.,. The Committee consists of Mr. F. J. S. Hopwood(Chairman); Mr. Ed. Carpmael, President of the CharteredInstitute of Patent Agents; Mr. C. V. Dalton, C.B., Comp-troller-General of Patents; Mr. J. A. Kempe, Deputy-Chairman of the Board of Customs ; and Mr. S. E. SpringKice, C.B., of Her Majesty's Treasury. Mr. Arthur Neeves,of the Board of Trade, is secretary of the Committee.
GERMAN CHEMICAL TRADE.
Chem. and Druggist, Dec. 30, 1899.The Association for the Protection of German Chemical
Industrial Interests recently held its twenty-second annualmeeting at Strasburg, at which the Secretary submitted areport reviewing the chemical industry in Germany duringthe past year, and this has now been published. The infor-mation given deals with matters almost 12 months old. Itwould seem as if the year 1898 had been a favourable onefor the German chemical trade. In the compilation of hisfigures he has used the returns of 103 companies whichexisted in 1898. These companies worked with an aggre-gate paid up capital of 287,103,100 m., on which theydistributed in dividends the sum of 36,428,325 m., corre-sponding to an average dividend of 12*69 per cent. Incomparison with the preceding year this is only a slightadvance, which is explained by the fact that the prices ofthe raw materials in almost every instance were considerablyhigher, without it being possible to advance values of themanufactured products in the same proportion. Theaverage dividend of the German chemical joint stock workssince 1889 has been as follows.—
Toar. Per Cent. Year. Per Cent,
33891890189118921893
10*5812*8111*2911*9213 "18
1894189518961897189S
12*7112 3012-1112*69
The number of fully-occupied people employed inchemical factories increased from 131,000 to 136,704, or4*25 per cent.; wages advanced simultaneously from 120*9to 129-6 million marks, or 7*2 per cent.—which figuresmay be taken as fair evidence of the activity in the Germanchemical industry.
Turning to individual products, the report states that theconsumption of soda and potash increased considerably inGermany, but that the exportation fell off by 7,000 tons.Values also fell slightly, while the cost of production in-creased. The demand for sulphuric and hydrochloric acidsduring 1898 was so active that the factories could scarcelymeet the demand, but the use of hydrochloric acid in theproduction of chloride of lime is gradually decreasingowing to the electrolytic method of production. As regardschloride of lime itself, the extremely low prices wereadvanced about 20 per cent, on account of the increasedconsumption. The saltpetre industry continued at a lowebb, owing partly to the introduction of smokeless gun-powder and the keen competition. In pharmaceuticalproducts, fine chemicals, essential oils, &c, there was a
good demand throughout the year at slightly increasedprices on the average. Acetic acid met a satisfactorydemand, at, however, ruinously low prices; while morebusiness was done in oxalic acid. In tartaric acid theFrench and Italian competition has again been strong,but the demand for the German-made article remainedconstant
THE RUSSIAN CHEMICAL INDUSTRY.
Comtn. Intelligence, Jan. 6, 1900,The chemical industry of Russia is at present compara-
tively undeveloped, but the importation of foreign chemicalsis gradually decreasing. Though there is a very largequantity of pyrites in Russia, the import of foreign pyritesis by no means diminishing despite the high duty, and themanufacture of sulphuric acid from them is increasing sorapidly that in 1897 the quantity of this acid imported hadfallen to 10,000 poods- Imports of nitric and hydrochloricacid in the same year were valued nt 42,000 roubles, whereasin 1890 they amounted to 1,226,000 roubles. The enormousdeposits of Glauber salts at Karabougaz Bay, on theCaspian, as well as those in the province of Astrakhan arenow to be seriously worked by a large French company.The consumption of soda in Russia amounts on an average to5,000,000 poods a year, and as there was only one companymanufacturing it on a large scale, the importation of it wasmaintained until the present year, when new works wereopened in Slaviansk.
INCREASING OUTPUT OF RUSSIAN PETROLEUM.
Comm. Intelligence, Jan. 13, 1900.
The output of naphtha in Baku is gradually increasing.The output for a period of nine months was, in 1895, 284million poods; in 1896,288 millions; in 1897, 311 millions;in 1898, 359 millions, and in 1899, 395 millions. From thisit will be seen that the export of Russian oil is graduallyincreasing, while the export of American oil has fallen off.The rise in prices of oil has resulted, too, in more rationalworking, the greater portion of the naphtha being nowrefined into oil, whereas hitherto most of the naphtha wassold in the crude state, mixed with the residues, for fuel.The railway tariff for the transport of naphtha, which wastemporarily reduced to 12 copecks per pood, will be, accord-ing to an official communication, a?aiu increased fromJanuary 15, 1900, but only to 16 copecks per pood, and not19, as it was previously.
OLIVE-OIL INDUSTRY IN PORTUGAL.
Comm. Intelligence, Dec. 30, 1899.
This industry is far from satisfactory, and all thosedesirous of consuming good oil are obliged to import fromFrance or Italy. The exportation is of no importance,although this country produces an abundant quantity ofolives. These are wasted through want of good oil-refinin^machinery—such as exists, for instance, in the South ofFrance and Italy. This matter ought to he taken up andenquired into hy those seeking to advantageously emplovcapital. *
A REVIEW OF MEXICAN IMPORT TRADE,
Comm. Intelligence, Jan. 13, 1900.
Ale and Beer.
Several breweries are in operation ; some make a verygood class of beer, which is more adapted and suitable forthe use of the people and climate than that of foreignmanufacture. A small quantity of Tennant's stout andginger ale is imported from Great Britain. All the breweriesare companies, and stocks are principally held by Germans'Mexicans, and Spaniards. J w i iuans ,
Bricks (Fire).
Sometimes there is a demand for good Scotch bricks butthe consumption is small and principally in the m ^districts, for repairs on boiler/and "as ay f aroacS'™fcupels. Generally when any new boilers L ordered thebricks for setting them are imported with thl\!VBabcock and Wilifok have office Z s p U l Ige* here
C 2
rnHE JOUBKAL OF THE SOCIETY OF CHEMICAL INDUSTEY. [Jan. 31, icoo.
Cement.This article is manufactured in the country. Two factories
are in operation. One of them bought the patent right froman English Company to manufacture Portland cement inthis country.
Although a good deal is manufactured, it is not first class.A great deal is imported from Great Britain, and some fromGermany. Peter's cement is the best known.
Chemicals.
This class of goods is handled by Germans and French,and several factories are in operation in the manufacture ofacids, &c, although the principal chemicals and drugs areimported from Europe. A large business is done in causticsoda for the manufacture of soap, which is extensively usedall over the country.
Crucibles.A great many of these are used in the mining districts,
and on the railways. Ten or 15 years ago the Morgancrucible was the only one known, but now a great manyFrench and American (Dixon's) are used; and the Morgancrucible is losing ground.
RUBBER TREKS.
Chem. and Druggist, Dec. 30, 1899.The Department of Agriculture has recently issued some
valuable information on the subject of rubber trees.Experiments in India with certain species were not success-ful, owing to the fact that the trees did not develop thecharacteristic lacteal ducts. In the light of the work ofthe Department's experts this was due to error in selectingthe variety. Unless care be taken in this direction, failurewill result in securing rubber, even though the trees mayapparently grow well. There are four varieties of rubbertrees, which must be utilised according to the soil andclimate of the place of cultivation.
(1.) Castilloa elastica grows well and produces rubberin places where the climate is hot, humid, and the soildrained.
(2.) Hevea brasiliensis, if the climate be hot, humid, andthe soil swampy or covered with water.
(3.) Manihot Gtaziovii, the Ceara plaut, if the climateis hot and the soil dry, sandy, or stony.
(4.) Sapium biglandulosum, in temperate or cold climates,such as Florida, Louisiana, &c.
The last variety is especially suitable for growing oncoffee plantations.
BLUE COMPOUND FOR COPPER SULPHATE.
Chem. and Druggist, Jan. 6, 1900.
At a recent meeting of the Council of the Royal Agri-cultural Society of England, Dr. Voelcker stated thatwarnings had been given from time to time in the reportsof the Chemical Committee to purchasers of "blue vitriol "(copper sulphate) for wheat - dressing, potato - spraying,charlock-eradication, and other purposes, that they shouldbe careful to see that what was supplied to them was thegenuine material, and not a mixture of copper sulphate andcrystallised ferrous sulphate ("green vitriol") in varyingproportions—a mixture sometimes sold as "agriculturalsulphate of copper."
In his annual report to the Council Dr. Yoelcker refersto this matter at considerable length, and mentions casesthat have come under his notice in which he found 20 percent, and 30 per cent., and even as much as 90 per cent, ofadmixture of ferrous sulphate, while in one instance alreadyreported the so-called " blue vitriol" consisted entirely of"green vitriol " coloured with Prussian blue so as to makeit look like copper sulphate.
ATTAR OF ROSE STILLS IN TURKEY.
Bd. of Trade J., Jan. 13, 1900.
The Turkish Minister of Agriculture proposes to facilitatethe acquisition by persons engaging in the attar of rosesindustry of the necessary apparatus (stills, &c.) of thelatest kinds, as these are greatly needed in Turkey, and itis said that he will make the necessary provisions for the
purchase and sale, on credit or hire, of stills to personsneeding them. These stills cost about 25 to 30 Turkishpounds each.
T H E PAPER SCARCITY.
Comm. Intelligence, Jan. 13, 1900.
Paper and Pulp has been making enquiries concerningthe enormous demand for news paper owing to the war andthe serious dearth of supplies. The reasons for the presentstate of affairs are alleged to be : —
1. The difficulty of getting wood pulp, which is scarce anddear.
2. The price of coal, which has gone up terribly.3. The enormous increase in demand and stoppage of
supplies of paper from America.Most of the great London dailies are using from 20 to 100
per cent, more paper now than they were two months ago.Messrs. Edward Lloyd, Ltd., said they were unable to takeany fresh orders for paper. The mills controlled by thiscompany are working night and day, and extra steamershave been chartered to bring all the available supply of pulpto the mills.
Similar reports are to hand from the provinces and abroad.The American Paper Trade Journal says that Americanpapermakers are no longer seeking foreign markets forproducts which are now inadequate to the home demand,and England is cut off from this source of supply. On theother hand, America finds in England an eager competitionfor such raw materials as she desires to bring, over from theother side, and which are needed to relieve the scarcity inthe States.
CHINESE LE\THKK.
Com?n. Intelligence, Jan. 13, 1900.
The process by which Chinese leather acquires its peculiarcharacteristics is described by the Boston Journal of Com-merce as follows :—The skins are put into tubs containingwater, saltpetre, and salt, and after 30 days are taken out,the hair is shaved off, aud the skins well washed in springwater; each hide is then cut into three pieces and wellsteamed, which is done by passing them several times back-ward and forward over a steaming oven. Further, eachpiece is stretched out separately over a flat board andsecured with nails, so as to dry gradually and thoroughly inthe sun. The smoke of the oven makes the leather black,and if it is desired to have it of a yellow appearance it isrubbed over with water in which the fruit of the so-calledwongchee tree has been soaked.
PROCESS FOR KEFIXING IXDIGO.
Chem. and Druggist, Dec. 30, 1899.
From Yokohama we learn that Prof. Nagai is said tohave completed a new process for refiuiug indigo. l ie ha?*been carrying on a series of experiments at Tokushima, andcomparative tests are now being made of the dye in» materialprepared according to his methods and that procured fromIndia. The Xagai indigo is to he called Awa XacniiSevian. n
THE WORLD'S SUGAR PRODUCTION.
Comm. Intelligence, Jan. 13, 3 900.Two-thirds of the world's sugar is now produced from
beets. Prior to 1871-72, the world's production of beet-sugar has never reached 1,000,000 tons; in the presentcrop year it is, according to latest estimates, 5,510 000 ton*while the cane-sugar crop, which in 1871-72 was 1,599,000tons, is in the present year 2,904,000 tons. Thus cane-sugar production has scarcely doubled during the periodunder consideration, while that from beets has more thanquintupled. In the meantime the price has fallen morethan one-half, the average cost in foreign countries of all
l X h Z ^ 7 m t ° t h e U n i t e d S ta tes in ««» fiscal yearpound g C* ^ P ° U n d j a U d i n 1 8 9 9 2-39 c. per
No development of the world's production of
tobt
had reached
Jan. si, woo.] THE JOURNAL OF THE SOOIETT OF OHEMIOAL INDUSTRY. 85
1900, 5,510,000 tons. In 1854-55 beet-sugar formed 13per cent, of the world's total sugar crop, and in 1899-1900it formed 66 per cent.
The following table shows the world's production of beet-and cane-sugar respectively, and the grand total in certainyears, from 1872 to 1899; also the average price of sugarin foreign markets. The figures relating to production arethe crop years ; those of price, fiscal years. The statementsof quantity in each case are in thousands of tons :—
World's Production of Beet- and Cane-Sugar, and Average' Price per Pound, 1871-1899.
Eng. and Mining J.y Jan. 6, 1900.Deducting certain duplications, such as lead used in
making white lead, coal used for coke, &c, which amountedto 121,206,968 dols. in 1899, against 87,530,840 dols. in1898, it appears that the grand total of mineral productionin the United States in 1899 was 891,424,082 dols., ascompared with 709,816,750 dols. in 1898.
Metallic Products.
Aluminium.—The high price of copper and the suitabilityof aluminium for conductors has given the sole produceran opportunity to supplant copper to some extent inelectric power work. The consumption for minor uses isalso increasing. The output of 1899 was 6,500,000 lb., asagainst 5,200,000 lb. in 1898.
Cobalt Oxide.—The sole producer of this substance in1899 increased its output to 10,200 lb., from 9,640 lb, in1898.
Copper.—High prices for the metal have stimulatedmining, but the total output of copper for the year fromdomestic ore was, after making allowance for that recoveredin the by-product copper sulphate, 592,672,637 lb., showinga gain of only about 11 per cent, over the 1898 figures,535,900,232 lb., the normal increase of production beingabout 10 per cent.
Copper Sulphate.—The production in 1899 was approxi-mately 67,089,499 lb., including 26,239,499 lb. recovered asa by-product in the electrolytic refining of copper. The1898 production was 55,119,361 lb., including 28,068,501 lb.recovered as by-product.
Lead.—The total production of lead in the United vStates,including that produced from foreign ores and bullion, was291,038 short tons in 1899, compared with 317,684 shorttons in 1898. The amount produced from domestic ores inthe two years was respectively 213,003 short tons and228,475 short tons. The production was distributed asfollows, the 1898 output being in brackets : antimonial lead,7,174 short tons [9,643] ; soft lead, 48,480 short tons[50,468]; desilverised lead, 235,384 short tons [257,573].The labour troubles in the Coeur d'Alene District, in BritishColumbia, and in Colorada, greatly curtailed the output.
Nickel.—Figures so far received show a production of61,179,689 oz. in the United States for 1899, an increase of2,416,562 oz. over in 1898. All this, as well as the cobaltoxide produced in this country, came from the Mine LaMotte, in Missouri. The total production by refiners in theUnited States from both Canadian and domestic ores,including the nickel turned out as nickel oxide, was8,052,047 lb. in 1899, compared with 7,138,929 lb. in 1898.
Quicksilver. — The production of quicksilver fromCalifornia mines in 1899 was 28,713 flasks. There was a
small output in Texas ; the Oregon mines produced nothing.The total output in 1898 was 30,493 flasks.
Silver.—Figures so far received show a production ofabout 63,000,000 oz. in the United States for 1899, anincrease of about 4,000,000 oz. over 1898. There was, asusual, a large production from imported ore and bullion,most of which came from Mexico.
Zinc and Zinc Ore.—The production of the variousrefineries and smelters in this country in 1899 was 135,796short tons. High prices for the metal stimulated the output,the 1898 figures being 114,104 short tons. Exports of zincore more than doubled, being 27,526 short tons in 1899 and11,782 short tons in 1898.
Zinc, White.—The production of zinc white in 1899shows a decrease as compared with 1898, the figures for thetwo years being 31,663 short tons and 32,747 short tons,respectively.
Non-Metallic Products.
Asbestos.—The total production of asbestos in 1899 was912 short tons, almost all of which came from the mines ofthe Sail Mountain Asbestos Company in Georgia, the 1898output of which was 885 tons.
Barytes.—The production of barytes in 1899 shows aslight gain, the output being 30,296 short tons, comparedwith 28,247 short tons in 1898. Most of the increase camefrom the Missouri deposits, although the Virginia mineswere as busy as usual.
Bauxite.—Most of the bauxite mined in 1899 came fromthe deposits in Georgia and Alabama, the output of theMissouri mines being small. The total production was35,842 long tons in 1899, compared with 26,791 long tons in1898.
Bromine.—The production of bromine in 1899, includingthat produced as bromide of potassium, was 460,000 lb.,the production showing a slight decrease from the 486,978 lb,produced in 1898.
Carborundum. — The sole producer of this substance,used as an abrasive, and also in steel making, increased itsoutput to 1,632,407 lb. in 1899, from 1,594,152 lb. in 1898.
Cement.—Owing to great activity in all building enter-prises, the production of both Portland and hydrauliccements during the past year was very heavy, themost marked increase in the output of the natural rockcements coming from the Indiana-Kentucky region. Thetotal output for 1899 was 10,048,447 bbls. of 300 lb. eachcompared with 8,161,078 bbls. in 1898. The production ofPortland cement also shows a great gain, the increase beingmost marked in Michigan, New Jersey, and Ohio, the NewYork works showing an actual decrease. Several producersof slag cement have come into the market, and at least oneis known to be meeting with success. The total productionof Portland cement in 1899 was 5,146,064 bbls. of 400 lb.each, compared with 3,584,586 bbls. in 1898.
Coal and Coke.—The United States now leads the world,in coal production. The total output of the mines in 1899*including anthracite used locally, was 56,697,525 short tonsof anthracite and 187,843,750 short tons of bituminousmaking a grand total of 244,581,275 short tons, comparedwith 218,106,519 short tons in 1898. The production ofcoke in 1899 also gained heavily, being 19,344,883 shorttons, against 15,897,797 short tons in 1898.
Copperas.—The output for 1899 was 13,895 short tons ascompared with 11,285 short tons in 1898.
Fluorspar.—Production has doubled during the 3 ear,chiefly owing to the activity of the mines in Kentucky'The output was 24,170 short tons, as against 12,145 shorttons in 1898.
Fullers' Earth.—The total production of fullers' earth in1899 was estimated at 14,463 short tons, the greater part ofwhich came from Florida. The production declined some-what, the output in 1898 having been 15,553 tons. Newmines are being opened on the Pacific coast, near Bakers-field, California, by the California Fullers , Earth Companywhich promise well. The chief use of the article is byrefiners of petroleum and cotton-seed oil.
Garnet—Owing to the competition of other substancesas abrasives, the output of garnet shows a decline. Most ofit continues to come from the Adirondacks. The 1899'
86 THE JOURNAL OF THE SOCIETY OF CHEMICAL INDUSTRY. [Jan.8i.uoo.
output was 2,295 tons, compared with 2,882 short tons in1898.
Grahamite.—Thevv were 3,013 short tons of grahamitemined in 1899, nearly all of which came from Utah. The1893 production was 2,675 short tons.
Graphite. — The production of crystalline graphite in1899 was 3,248,383 lb., as against 1*647,679^ lb. in 1898.The great bulk of the output came from mines in New YorkState. The Philadelphia Graphite Company, however,greatly increased the output of its mines in ChesterCounty, Pennsylvania, and a new Pennsylvania producer,the Standard Graphite Company began work. There^ wasa production of 2,631 short tons of amorphous graphite inthe year, compared with 1,200 tons in 1898, most of theincrease coming from the mines of the Philadelphia GraphiteCompany. The production of artificial graphite at theworks at Niagara Falls has made great progress, and theoutput in 1899 was 378,410 lb., as compared with 185,647 lb.in 1898.
Limestone Flux.—The production of limestone for fluxvaries according to the activity of the blast furnaces of thecountry. The 1899 production was 6,224,151 long tons, asagainst 5,275,819 long tons in 1898-
Phosphate Rock.—The output of phosphate rock shows adecided gain, though there is not the wonderful increaseshown by 1898 figures as compared with 1897. The outputin 1899 was 1,738,3^2 long tons, compared with 1,257,645long tons in 1893. The increase is most marked in theTennessee fields.
Pyrites.—The output of the American pyrites minesshows an actual falling off during the year. The greatbulk of the ore mined continues to come from Virginia.The production in 1899 was 176,208 long tons, compared-with 191,160 long tons in 1898.
Petroleum.—The total output of crude petroleum in 1S99was 54,048,100 bbls. The price per barrel rose decidedlyduring the year, greatly increasing the activity of drillerswithout proportionate results. The 1898 output was51,774,465 bbls.
Salt.—There was a decided increase in the output of saltfor 1899, the amount being 19,025,794 bbls., in comparisonwith 18,756,394 bbls. in 1898.
Soda.—The domestic production of soda, including sodaash, caustic soda, and other products, reduced to a commonbasis of 58 per cent, soda ash, in 1899 was 363,000 tons,compared with 340,622 metric tons in 1898. This increasehas come chiefly from the Solvay Process Works, theelectrolytic process works showing, if anything, a decrease.
Sulphur.—The production of sulphur fell off more thanone-half, chiefly owing to the competition of Japanesesulphur, which can be laid down cheaper than the Nevadaproduct in the San Francisco market. The production inLouisiana is almost stopped. The output for the year was1,337 long tons, compared with 2,726 long tons in 1898.
Talc—There was mined in 1899 59,470 short tons offibrous talc, as against 54,807 short tons in 1898, the totalproduction in both years coming from mines in New YorkState,
T H E U.S. ALKALI AND CHLORINK INDUSTRIES IN 1899.
Eng. and Mining J., Jan. 6, 19C0.
J. 2?. Watson and A. T. Weightman.Considerable activity has been shown during 1899. These
industries have generally improved since 1898. Englishammonia soda has partially recovered from the depressionexperienced during the two preceding years, having createdother markets to take up the quantities displaced owinc todomestic manufacture in and increased taiiff upon impoita-tion into the United States. Prices were well maintained inEngland, but cutting was experienced in the earlier monthsof the present year in the United States. Mutual arrange-ments were arrived at in regard to domestic trade, butincreased competition due to the Columbia Chemical Com-pany beginning to erect works at Barberton, O., will probablydisturb the market for next year. Ruling prices have been60 c. to 70 c. contract and 80 c. to 90 c. market.
Leblanc soda is still decreasing in demand. Shipmentsto the United States have not been very extensiveruling slightly higher than ammonia soda.
Bicarbonate of soda has ruled generally active; pricesbeing on the decline. The increased production due towork's being erected at Laramie, Wyoming, increased facili-ties for production at the Pennsylvania Salt Company'sWorks, the utilisation of carbon dioxide from large breweriesin Milwaukee, and close competition, will cause furtherdecline.
Crystal carbonate in the States is manufactured by onlyone works, but the demand is increasing arid others are likelyto undertake this manufacture. There has been less demandshown for sal soda, particularly for foreign manufacturers,but the general market has remained fairly active. Pricesruling: Casks, at from 50 c. to 60 c. and kegs, 60 c. to 7uc.In several large towns works have been established in thepast year where sal soda is manufactured from soda ash,notably Chicago, New York, Milwaukee and PittsburghThey are able to meet the demand in their own localitiesand make a profit, due to difference in freight between sodaash and sal soda, no freight being paid in carrying thewrater of crystallisation. Profits are small. A furtherdemand has been created in the increased use for bicarbonateof soda by the manufacturers of carbonated waters, whilemonohydrate of soda shows a slightly increased demand,due to fresh markets being opened up.
Domestic makers of caustic soda by the electrolyticprocess have still to expect the increasing demand forsoda ash, and the consequent displacement of caustic, aslarge soap makers continue to put in plants for the manu-facture of caustic from ammonia soda ash.
With the prevailing prices and contracts made for sodaash in bulk, caustic from the electrolytic process will haveto be sold in very close competition. The increasingdemand for heavy chemicals is dependent to a large extenton the increasing prosperity of the population, and directlydependent on the advancement of civilisation. Comparisonshave been made on the quantities of soda products per headof population in various countries, for instance, Canada, 4 ;United States, 5 | ; England, 7.
The demand for bleach in the United States has beenextremely active, notwithstanding the increased tariff oftwo years ago, and the increase in domestic manufacture.The problem of the future is to what extent chlorine canbe utilised in the various manufactures.
The increasing quantities of sulphite and wood pulp forpaper manufacturers means a proportionate decrease ofmanufacturing paper from rags, esparto, straw, jute, &c,since the former process does not require so much chlorine'to bleach the pulp as the latter. Textile industries are,however, creating somewhat increased demand in thisdirection.
Greater activity has been shown in the United States,England, France, and Germany in the manufacture ofelectrolytic chlorine. English works by the older processesstill continue to keep active, notwithstanding the onslaughtof the various electrolytic processes; greater economies^inthe manufacture of hydrochloric acid and bleach have beenbrought about, and managerial and brokerage expenses cutdown. Improvements in the machinery have^been extremelyinfrequent. The future existence o'f Leblanc works isdependent entirely on the by-products and the higher <rradeheavy chemicals. & to
Great things are expected in the immediate future in theelectrolytic processes of manufacture in the alk-ili tradeIt is generally acknowledged that these processes* will'notaffect the alkali so much as the chlorine industry, and thatthey will be ultimately regarded as chlorine processes,producing caustic soda as a by-product, the soda marketbeing still largely maintained by the ammonia-soda processand the natural soda. 1
The introduction of these processes will, however, causethe centres of manufacture to shift from localities wherecoal is cheap to localities where water po™er can beObtainedeasily, consistent of course with a P g O o d supplv of rawmaterial and reasonable transportation facilities N o L u b tgreat cutting of prices will result before he electronicTT ^ ^ ^ to 4 TGbTbTreason of l ^ ^ ^ <"** to ov4-prbut by reason of the enormous amount of capital investedin the older processes they will die hard, and the
Jan. si, woo.] THE JOURNAL OF THE SOCIETY OF OHEMIOAL INDUSTRY. 87
processes Avill have to deal with keen competition at the•early stages of their introduction. Ammonia soda cannot'easily be displaced for the manufacture of soda ash by:an electrolytic method, and bicarbonate of soda is in the^ame situation. The only fields that seem likely to haveany tendency toward displacing soda ash by the ammonia-soda process are the natural soda fields and springs in theWestern States.
Wyoming and Kansas show great advantages which willhe taken advantage of as the population and transportationfacilities increase. Soda ash can be manufactured from•salt by the ammonia soda process at a cost of 9 dols. a ton.The Western fields, with fuel equal to the Central andEastern fields, can produce soda ash at a cost of not over7 dols. a ton.
Bicarbonate of soda is already reaching the Middle-Western markets from these States, and is coming in direct^competition with Middle-Eastern manufacturers. Theirinexhaustible supply shows that these States will have to*be reckoned with. The extreme Western market andPacific Coast shipments will be well taken care of by manu-facturers along the Coast line of California, particularlynear Los Angeles. One ot the features whbh the Cali-fornian manufacturers have to contend with is the fuelsupply, the distance to coal being great. The Chinese andJapanese markets are on the steady increase, but are chiefly•supplied from England.
SULPIIATE OP AMMONIA IN 1899.
Bradbury and Hirsch, Liverpool.The average price for the year has been III. 5s. 9 |J . per
ton f.o.b. Hull, against 9l 9s. 1\d. per ton in 1898, and7/. 186*. 4f</. per Ion in 1897. The year's working hastherefore been highly prosperous. The average prices ofnitrate of soda at Liverpool were—11. 19s. Id. per ton in1899, 11. l\s. 3d. per ton in 1898, and 1L 15s. 5c/. per tonin 1897.
This prosperity is due in the first place to the policy ofmakers, adopted in 1897 and since persisted in, in disposingof their output as it has become available ; in the next placeto the absence of any important increase in production,and to the remarkable increase in Spanish and Colonialconsumption. The importance of this increased consump-tion will only be appreciated when the further markedshrinkage in demand from all nitrate of soda consumingcountries, the United States excepted, is taken into account.Nitrate of soda has been much the cheaper article per unit,and it has been used in place of sulphate of ammonia whereit could be substituted to advantage.
The last review tabulated the exports to the principalnitrate of soda consuming countries for three years; thefollowing statement gives the figure over a longer period,and adds similar particulars of shipments to the otherimporting countries :—
Sulphate of Ammonia daring 1899.— Shipments.
To France„ Germany and Belgium
To Spain ,„ Italy„ Canaries «
To Holland„ Java„ British Guhuui„ West Indies7, Mauritius
To United States„ other countries
Total Exports.,
1899. 1898, 1897.
Tons.10,0 1933,622
Tons.15,96642,232
43,671 58,198
38,2754,7152,994
31,4823,:*<M>2,453
Tons,5>3,11655,187
78,303
27,1853,8312,518
45,98 i 37,241
1896. 1895.
Tons.12,76543.386
Tons.7,345
40,277
1894.
Tons.8,796
41,470
56,152 47,623 50,266
20,9824,1462,532
22,1532,6911,914
17,403758
1,294
33,554 27,660 26.788 19,455
8,444,13,643
5,2274,7652,620
10.1958,2-56,2984,9302,701
9.8186,8374,9174,0232,<»28
34,699 32,389 27,653
8,2157,802
4,6614,447
8,86-14,607
140,371 136,936 152.981
8,2756,8264,2993,046
7,1485,9056,2212,3691,665
29 433 23,311
9,8202,960
11,6412,335
11,4996,2015,3253,6881,173
27,886
4,2651,466
126,025 111,700 103,338
France, Germany, and Belgium are pre-eminently nitrate•of soda consuming countries. There has been some increasein German production, but the total output there is stillestimated at about 10u,000 tons. Estimated French pro-duction in 1899 is 36,000 tons, or 1,000 tons more than that in1898, and 12,000 tons less than that in 1896. Any increasein production on the Continent, therefore, does not accountfor the extraordinary shrinkage in shipments to France,Germany, and Belgium. The figures^ for the six years1894—1899 correspond so strikingly with the cheapness ordearness of sulphate of ammonia in relation to nitrate ofsoda for the corresponding years, that no other conclusionis possible than that relative prices have been the determiningfactors with consumers.
Where nitiate of soda does not compete —in Spain, Italy,and the Canaries—consumption is determined by otherconsiderations than that of price, and it will be observedthat the shipments to Spain show marked progress on anadvancing market. The remark applies also to sugar-growing colonies, as will be seen from the figures. Exportsto Holland are classed with colonial shipments because alarge portion is re-exported to Dutch colonies, and probablythe great increase in direct exports to Java in 1899 accountspartly for the shrinkage in shipments to Holland.
Demand for the United States is always an uncertainquantity, and one which it is impossible to forecast. Thelarger demand in 1899 has been partly occasioned by thelarge sales of American ammoniates to France at relativelyhigh prices, but seeing that probably not more than half ofthe American consumption is taken for agricultural purposesit is evident that agricultural exigencies do not altogetherdetermine the total requirements. Production in the UnitedStates in 1899 is not estimated at more than 12,000 to15,000 tons, whilst imports have been 8,200 tons—say22,000 tons altogether. If half of this has been taken forchemical and refrigerating purposes, there has only beensome 11,000 tons available for agriculture—an insigniacantquantity when the possibilities of the country are consideredand compared with the United States consumptiou of nitrateof soda in 1899, which has been about 160,000 tons.
Production in the United Kingdom during 1899, from allsources, we estimate at 202,000 tons, viz. :—
r< i Tons.Gasworks 133,000Ironworks l8>m
Shaleworks 37>30()
Coke and carbonising works ] 3 QQQ
T o t a l 202,000
THE JOURNAL OF THE SOCIETY OF CHEMICAL INDUSTRY. [Jan. 31, woo.
Of this production we estimate that—Tons.
England contributed 12S,2OOScotland „ 71,000
Ireland „ 2,800
The production during the previous five years was :—
1898. 1896. 1895. 1894.
GasworksIronworksShaleworksCoke and carbon
ising works.Total
Tons.130,000
17,70037,30011,500
Tons.133,000
18,00037,00010,000
Tons. ! Tons.127,50016,5003S,0009,000
119,60014,60038,3007,000
Tons.113,50010,00033,0003,500
190,500 198,000 191,000 179,500 160,000
Production in 1898 from gasworks, for the first timesince records have been kept, showed a decline on thepreceding year. Notwithstanding electric lighting and theuse of water-gas and other illuminants in recent vears,production of sulphate of ammonia from gasworkscontinued to increase up to 1898, though in varying ratios,from year to year, and, having regard to the condition oftrade in 1898, the shrinkage in output of sulphate ofammonia is somewhat puzzling. Last year, particularattention was called to the fact, that whereas the ratio ofincrease in production of sulphate of ammonia from gas-works was 6 per cent, in 1896 as compared with 1895, the
ratio in 1897 as compared with 1896 was only 4 per cent.The extended use of other illuminants was probably themain cause of the shrinkage, but the comparative immunityfrom fogs in the winter months might also be a contributingfactor.
The rapid expansion in output from all sources ex-perienced between 1893 and 1897 has entirely disappeared;and although the proceeds from sulphate of ammonia arean important item in the revenues of producers, the rate ofoutput is determined by considerations quite apart from themarket price of sulphate of ammonia.
There has been a further falling off in home consumptionin 1899, owing to advanced prices over the spring monthsand to the smaller requirements of manure manufacturersfor compounds, the tendency being still for foreign buyersto make their own mixtures.
Exports show an increase of 3,500 tons, as compared withthose for 1898.
The year's working therefore shows :—Tons,
Stock brought forward from 1898 4,000Production in 1S99 202,001)
Available supply 206,000"
Exports in 1S99 110,500Home consumption in 1899 58,500Stock carried forward to 1900 7,000
200,000
NITRATE OF SODA.
Shipments, Consumption, Stocks, and Prices, for Three Years. W. Montgomery and Co. 30/A December 1$99
Shipments for six months ending 31st December.Do, for year ending 31st December (Afloat lor Europe on 31st DecemberStocks in United Kingdom ports :—
1897. 1898. 1809.
LiverpoolLondon*.Out ports
Tons.6,0001,800
13,200
Tons.4,5002,4009,100
Tons.0,0001,800
22,200
Stocks in Continental ports on 31st DecemberConsumption in United Kingdom for six months ending 31st December
Do. in Continent for six months ending 31st DecemberDo. in United Kingdom for VI months ending 31st DecemberDo. in Continent „ „ „Do. in United States „ „ „Do. in other Countries „ „ „Do. in the World „ „ „
Visible supply on 31st December
Price on 31st December p e r
Y
1897.
Tons.700,000
1,060,000394,000
21,000
224,00032,500
238,500108,500867,500110,00014,000
1,100,000630,000
Is. Gtf.
1898.
16,000
110,00032,000234,000132,0001)00,000142,00012,000
1,186,000703,000
1890.
Tons.819,000
1,260,000571,000
Tons.806,000
1,360,000494,000
30,000
20G,0( O34,000
270,000123,000
1,017,000160,00030,001)
1,330,000730,000
7.9.
BOARD OF TRADE RETURNS.
SUMMARY OF IMPORTS.
I Year ending 31st December.Articles.
1898. 1899.
MetalsChemicals and dyestuffsOilsHaw materials for non-textile in-
dustries.Total value of all imports . . . .
£21,852,3815,484,4208/356,405
52,226,006
£28,263,843
5,768,8909,688,760
56,666,589
470,378,583 485,075,514
SUMMARY OP EXPORTS.
Articles.
Metals (other than machinery)..Chemicals and medicinesMiscellaneous articles
Total value of all exports
.—_
Year ending 31st December.
1898.
£
32,746,7908,339,215
33,322,975
233,359,210
1S99.
£
40,312,4438,855,523
35,016,514
201,660,617
Jan. 31,1900.] THE JOUENAL OF THE SOCIETY OF CHEMICAL INDUSTRY. 89
IMPORTS OF METALS TOR YEAK ENDING 31ST DECEMBER.
Quantities. Yalue.
Articles,
Copper :—Ore TonsRegulus „Unwrought „
I r o n : —Pig and puddled „Ore „Bolt, bar, &c. . . . „
Steel, unwrought.. „Lead, pig and sheet „Pyrites „Quicksilver Lb.Silver ore Yalue £Tin Cwt.Zinc TonsOther articles . . . Value £
patent• The dates given are the dates of the Official Journals in
which acceptances of the Complete Specifications are advertised.Complete Specifications thus advertised as accepted are open toinspection at the Patent Office immediately, and to oppositionwithin two months of the said dates.
/ . •" . / - _, > / - > >. , VV'vy
I.—PLANT, APPARATUS, AND MACHINERY.
APPLICATIONS.
25,094, A. J. Boult.—From the Societe Anonyme deProduits Chimiques de Droogenbosch, Belgium. Improvedmethod of rendering iron vessels resistent to acids. CompleteSpecification. Dec. 18.
25,109. J. E. Thornton and C. F. S. Eothwell. Improve-ments in coolers, condensers, radiators, geysers, and thelike apparatus. Dec. 19.
25,229. J . J . Meldrum, T. F. Meldrum, and J. W.Meldrum. Improvements in or connected with supplyingair to furnaces and in steam jet blowing or forcing apparatustherefor and other purposes. Dec. 20.
25,235. W. Brown. Improvements in or connected withfurnaces. Dec. 20.
25,640. G. N. Vis. Improved vacuum evaporating appa-ratus for separating salt from solution especially frombrine. Dec. 28.
1900.
51. M. E. Douane. Improvements in refrigerating appa-ratus working with volatile liquid. Jan 1.
205. C. A. Matthey. Improvements in and connectedwith centrifugal separators. Jan. 3.
369. II. Renno. Improvements in compressers for usewith refrigerating machines. Complete Specification.Jan. 6.
370. EL Renno. Improvements in refrigerators, con-densers, and the like. Complete Specification^ Jan.V
451. F. Pinther. Improvements relating to apparatusfor regulating the supply of air to furnaces. Jan. 8.
534. E. G. Behrend. Improvements in cooling orrefrigerating apparatus. Jan. 9.
542. A. C. Calkins. Improvements in compressing ap-paratus for making cupels or the like. Filed Jan. 9. Com-plete Specification. Date applied for July 13, 1899, beingdate of application in United States.
649. J . Laidlaw and R. A. Robertson. Improvements incentrifugal apparatus. Jan. 11.
701. J . Grouvelle and H. Arquembourg. Improvementsin the manufacture of coolers or condensers. CompleteSpecification. Jan. 11.
769. O. H. Bryant and G. T. Augspurg. An improvedmachine or apparatus for compressing gas. Jan. 12
COMPLETE SPECIFICATIONS ACCEPTED.*
1898.21,300. E. Shaw. Apparatus for cooking, concentrating,
and evaporating liquids. Jan. 17.
1899.
470. J. H. Cooper and J. W. Cooper. A continuouskiln. Jan. 17.
3,552. B. J. B. Mills.—From La Societe Anonyme desFontaines a Gaz, France. Gas furnace. Jan. 17.
4767. J . Harvey.— From R. Harvey, United States.Evaporators. Jan. 10.
i 16,161. J. Armstrong. Reverbeiatory furnace. Jan. 10.20,956. A. J. Boult.—From The Park and Lacy Com-
pany, United States. Machines for compressing air andother compressible fluids. Dec. 29.
22,438. W. M. Miller. Evaporating, boiling, and dryingappliances. Dec. 30.
23,158. J. McNeil and C. McNeil. See Class XVI.
IL—FUEL, GAS, AND LIGHT.APPLICATIONS.
25,138. D. M. Dorman. Improvements in acetylene gasgenerators. Dec. 19.
25,171. J . H. Abercrombie and R. B. Symington. Im-provements in machines and apparatus for manufacturingincandescent lighting mantles. Complete Specification.Dec. 19.
23,271. F . Baker.—From C. Martin, Victoria. Newmethod and means of illumination. Dec. 20.
25,374. H. J. Robus. Improvements in apparatus foruse in the manufacture of coal gas. Complete Specification.Dec. 21.
25,503. G. H. Quelch and J. O. Kent. Improvementsin the preparation of masses containing carbide of calciumfor use in the generation of acetylene gas. Dec. 23.
25,707. F. McNamee. Improvements in preparing peatfibre, peat dust, peat fuel, and the like. Dec. 30.
1900.56. H. M. V. Etten and H. Greenfield. Improvements
in the manufacture of artificial fuel. Complete Specification.Jan. 1.
179. E. Mayrisch. Improvements in connection withgas purifying appparatus. Complete Specification. Jan. 3.
194. E. W.Lancaster. Improvements in and connected"with apparatus for purifying acetylene gas. Jan. 3.
234. C- S. Snell. Improvements in apparatus for com-pressing or intensifying gas, air, or the like. Jan. 4.
235. C. S. SnelL Improvements in apparatus for com-pressing or intensifying gas, air, or the like. Jan. 4.
291. J. St. C. Legge and T. P. R. Bradshaw. Improve-ments in fire-lighters and fuel. Jan. 5.
366. M. LieskL An improved acetylene gas generatingapparatus, Jan. 6.
388. S. J. Earl. Improvements in acetylene lamps andgenerators. Jan. 6.
410. E. J. Duff. Improvements in gas producers. Jan. 8.558. J. C. C- Read and C. E. Sage. The manufacture
of an improved fuel, and apparatus therefor. CompleteSpecification. Jan. 9.
792. G. Birch. Improvements in and connected withincandescent gas burners. Jan. 13.
830. W. ^ Peck. Improvements in apparatus for car-Luretting air. Jan. 13.
COMPLETE SPECIFICATIONS ACCEPTED.
1898.
21,067. F. Brown. Apparatus for use in the productionof oxygen gas. Jan. 10.
1899.631. J. H. H. Duncan. Incandescence burners and
mantle supports. Dec. 29.
Jan.31,mo.] THE JOURNAL OF THE SOCIETY OP CHEMICAL INDUSTRY. 91
682. E. Seiffert and J. D. Tomlinson. Apparatus forthe production and supply of acetylene gas. Dec. 29.
2178. C. Clamond. Apparatus for incinerating incan-descent mantles. Jan. 17.
2186. E. S. Bond, Apparatus for generating, storing>and supplying acetylene gas. Jan. 10.
2502. A. McDougalL Purification of coal-gas. Dec. 292832. S. Chandler, jun., and J. Chandler. Apparatus
for washing or scrubbing gas. Dec. 30.4115. J. Caldicott. Acetylene gas generators. Dec. 29.4365. J. R. Wighani. Burning acetylene gas. Dec. 29.6116. E. J. Dolan. Acetylene gas burners. Jan. 17*12,139. ST. A. Guillauine. Gas generators. Jan. 17.15,977. W. Higgins and H. Sandilands. Apparatus for
the production of acetylene gas. Jan. 10.22,516. A. Stern. Regulated liquid trap for the gas-
delivery pipes of acetylene gas generators. Dec. 30,22,527. W. P. Thompson.—From the firm of Gebriider
Buxbaum, Germany. Improvements in apparatus forcarburetting air or producing " air-gas." Dec. 30.
23,032. J. Y. Johnson.—From Compagnie FranQaise de['acetylene dissous, France. Acetylene gas burners for usein incandescent lighting. Dec. 29.
23,179. T. G. Turner. Gas apparatus and more particu-larly means for generating acetylene gas. Jan. 10.
23,309. G. G. Smith. Acetylene gas generators. Jan. 10.23,937. A. E. Adolfsson. Acetylene gas generating
apparatus. Jan. 10.23,988. H. H. Leigh.—From J. W. Carey, Queensland.
Means for regulating the supply of water to acetylene gasgenerators. Jan. 10.
III.-DESTRUCTIVE DISTILLATION, TAR
PRODUCTS, ETC.
APPLICATIONS.
1900.243. E. Sorel. The extraction of benzoles dissolved by
heavy oils and separation of their constituents. CompleteSpecification. Jan. 4.
355. A. Ramage. Improvements in or relating to retortsfor the distillation of shale coal and other bituminoussubstances or minerals, also applicable to retorts for thecalcining of ironstone and similar substances. Jan. 6.
408. J. Beveridge and The Linlithgow Oil Company, Ltd.Improvements in and relating to retorts for distilling shaleand like minerals, and for dealing Avith the burnt or spentshale. Jan. 8.
Co^riPLETE SPECIFICATION ACCEPTED.
1899.
27,559. T. Wilton. Manufacture and purification ofanthracene and other substances. Dec. 30.
IV.—COLOURING MATTERS AND DYES.
APPLICATIONS.
25,069. H. E. Newton. — From The Farbenfabrikenvormals F. Bayer and Co., Germany. The manufacture orproduction of carbaraic ethers. Dec. 18.
25,080. J. Y. Johnson.—From The Badische Anilinand Soda Fabrik, Germany. The manufacture and producetion of new colouring of the anthracene series. Dec. 18.
25,269. F. Raschig. Process for the separation ofmetacresol and paracresol. Dec. 20.
25,288. J. Y. Johnson.—From The Badische Anilin andSoda Fabrik, Germany. The manufacture and productionof new colouring matters and of products for use therein.Dec. 20.
25,511. B. Willcox.—From The Badische Anilin and SodaFabrik, Germany. The manufacture and production of anew azo colouring matter and of lakes therefrom. Dec. 23.
25,754. R. B. Ransford.—From L. Cassella and Co.,Germany. Improvements in the manufacture of colouringmatters. Dec. 30.
1900.
49. H. E. Newton.—From The Farbenfabriken vormalsF. Bayer and Co., Germany. The manufacture or pro-duction of aromatic hydroxy compounds. Jan. 1.
50. H. E. Newton.—From The Farbenfabriken vormalsF. Bayer and Co., Germany. The manufacture or pro-duction of aromatic aldehydes. Jan. 1.
130. R. B. Ransford.—From L. Cassella and Co., Ger-many. Improvements in the manufacture of dyestuffs.Jan. 2.
530. H. E. Newton.—From The Farbenfabriken vormalsF. Bayer and Co., Germany. See Class XX.
832. The Societe Franchise de Couleurs d'Aniline ^ dePantin. Improvements in the preparation of colouringmatters for dyeing cotton. Filed 13 Jan. Date applied for13 June 1899, being date of application in France.
COMPLETE SPECIFICATIONS ACCEPTED.
1899.3672. H. H. Lake.—From K. Oebler and Co., Ger-
many. Manufacture of poly-azo-dyestuffs. Dec. 29.4799. H. Pauly. Manufacture of derivatives of iminotri-
acetonamine. Jan. 10.4818. H. E.Newton.—From The Farbenfabriken vormals
F. Bayer and Co., Germany. Manufacture or production ofdvestuffs for cotton. Jan. 10.
5018. H. E. jSTewton.—From The Farbenfabriken vormalsF. Bayer and Co., Germany. Manufacture or production ofnew anthraquinone derivatives. Jan. 10.
5039. A. G. Green, A. Meyenberg, and The ClaytonAniline Company, Ltd. Manufacture and production ofcolouring matters containing sulphur. Dec. 30.
5218. O- Imray.—From The Farbwerke vormals Meister,Lucius, and Briining, Germany. Manufacture of acetyl-diamido-diphenylamine sulphonic acid and its homologues,Jan. 10.
5325. C. D. Abel.—From The Actiengesellschaft furAnilinfabrikation, Germany. Manufacture of black dye-stuffs for directly dyeing cotton. Dec. 29.
5393. C. D. Abel.— From The Actiengesellschaft furAnilinfabrikatiou, Germany. Manufacture of new deriva-tives of oxydiphenylamine. Dec. 29.
5766. C. D. Abel.— From The Actiengesellschaft furAnilinfabrikation, Germany. Manufacture of an aromaticdinitro compound and a new diamido compound derivedtherefrom. Jan. 17.
6583. C. D. Abel. —From The Actiengesellschaft furAnilinfabrikation, Germany. Manufacture of black disazocolouring matters. Jan. 17.
7020. C. D. Abel. —From The Actiengesellschaft fiirAnilinfabrikation, Germany. Process for the production ofdimethyl ether of sulphuric acid. Jan. 17.
7022. C. D. Abel. —From The Actiengesellschaft furAnilinfabrikation, Germany. Manufacture of a black-browndyestuff directly dyeing cotton. Jan. 17.
7023. C. D. Abel. — From The Actiengesellschaft fiirAnilinfabrikation, Germany. Manufacture of blue dyestuffsdirectly dyeing cotton. Jan. 17.
7348. C. D. Abel. —From The Actiengesellschaft fiirAnilinfabrikation, Germany. Manufacture of a brown dye-stuff directly dyeing cotton. Jan. 17.
7349. J. Imray. — From La Societe Anonyme desMatieres Colorantes et Produits Chimiques de St. DenisFrance. Manufacture of black substantive sulphuriseddyestuffs. Jan. 17.
a20,102. C. K. Mills.—From L. Cerf, France. Obtaining
derivative of phenol-1.2-methanolsulphonimide. Jan. 10
92 THE JOUENAL OF THE SOCIETY OF CHEMICAL INDUSTBY. [Jan. 3],
.—TEXTILES: COTTON, WOOL, SILK, ETC.
APPLICATIONS.
25,610. A. E. Donisthorpe, G. White, and G.E.Ellis.Improvements in or relating to coloured yarns and in fabricsor articles produced therefrom. Dec. 28.
25,638. E. Simon. Apparatus for mercerising cottonfabrics under tension. Complete Specification. Dec. 28.
25,719, A. Baumann. The manufacture or productionof a peculiar lustrous decorative effect on woven fabrics.Dec. 30.
1900.486. R. Weiss. Improvements in apparatus for treating
textile materials with circulating fluids. Complete Speci-fication. Jan. 8.
COMPLETE SPECIFICATIONS ACCEPTED.
1899.1358. J, Williams. Process of treating paper and fabrics
to render them waterproof and rot-proof. Jan. 17.3669. C. Wetherwax. Process of treating flax straw for
obtaining textile fibres therefrom. Dec. 29.4773, T. Pickles. Apparatus to be employed in con-
nection with the mercerisation of cotton or other fabrics.Jan. 10.
15,397. T. Robinson. Construction of machine for usein the mercerising of cloth. Dec. 30.
16,761. J. G. Lorraine,—From J. G. Pratt, United States.Apparatus for treating stalks of fibrous plants. Dec. 29.
22,391. E. Heusch. The production of imitation fabrics.Jan. 10.
VL—DYEING, CALICO PRINTING, PAPERSTAINING, AND BLEACHING.
APPLICATIONS.
25,076. C. F. Cross and G. A. Parkes. Improvements inbleaching, vegetable textile fabrics. Dec* 18.
25,388. J. Schmidlin and D. Schmidlin and Co., Ltd.Improvements in connection with drying textile yarns andfabrics in bleaching, printing and dyeing, finishing, andsimilar processes. Dec. 22.
25,603. W. E. Kay and The Thornliebank Company,Ltd. Improvements relating to the fixation of anilinecolours in calico printing. Dec. 28.
25,618. T. R. Shillitc—From J. R. Geigy and Co.,Switzerland. Process for the production of bottoms oncotton with the addition of rosin soap by means of .solubleand insoluble azo colours. Dec. 28.
1900.283. J. C. Chorley. Improvements in colouring-
vegetable textile fabrics. Jan. 5.
379, O. Hoffmann. Process for producing repetitions oflong suites of colours upon threads. Jan. 6,
459. R. Brandts. Improvements connected with thebleaching, dyeing, mercerising, steaming, and like treat-ment of the material wound in slubbincr a n ( j rovino-machines and with the subsequent spinning of the sametComplete Specification. Jan. 8.
501. J. Galbraith and W. M. Petrie. Improvements inthe printing of fabrics used for making dresses and otherarticles. Jan. 9.
509. J. Major and T. J. Wood, Improvements inapparatus for dyeing, bleaching, or otherwise treating copsof spun yarn. Jan. 9.
705. F. W. Golby.—From F. A. Reichman, Sweden.Apparatus for mordanting, bleaching, mercerising, dyeing"and drying, applied to broad-dressing machines. Jan. 11.
731. J. Major and J . T. Wood. Improvements in orapplicable to apparatus for dyeing, bleaching, or otherwise
. treating cops of spun yarn. Jan. 12.
COMPLETE SPECIFICATIONS ACCEPTED,
1899.
2707. H. Newell. "Jigger" machines for dyein"Jan. 17.
6244. J. Y. Johnson.—From The IJadische Auilin andSoda Fabrik, Germany. Production of fast black shadeson wool. Jan. 17.
7997. F. Barraclough. Apparatus for dyeing and other-wise treating yarn in cop and other similar compact form.Dec. 29.
18,690. E. Holken. Black dyeing. Dec. 29.21,488. L. Weldon. Machines for use in dyeing yarns,
Dec. 30.
VII.—ACIDS, ALKALIS, AXD SALTS.APPLICATIONS.
25,077. P. Pressneck. Improvements in the manufactureof acetic acid. Dec. 18.
25,081. B. J. B. Mills.—From A. Lumiere and L. Lumiere,France. The manufacture of persulphate of sodium.Complete Specification. Dec. 18.
25,161. A, Wenck. Improved process for the pro-duction of strontium carbonate. Complete Specification.Dec. 19.
25,297. E. Edwards.—From The Krauschwitzer Thon-waarenfabrik fiir chemische Industrie (vormals L. Rohr-mann), Company, Germany. Improved process andapparatus for the production of acetic acid of high per-centage and in large qnantities by means of fractionaldistillation. Dec. 20.
25,648. W. S. Squire. Apparatus for the production ofliquid sulphur dioxide from mixed gases containing thesame. Dec. 29.
1900.212. A. C. Girard. See Class XXII.335. G. E. Davis and A. R. Davis. An improved process
for the elimination of impurities from certain metallicsolutions. Jan. 5.
COMPLETE SPECIFICATIONS ACCEPTED.
1898.26,169. J. L. Kessler. Apparatus for concentrating sul-
phuric acid. Jan. 17.
1899.2497. R. Warner, J . Wade, and C. T. Fox. Manufac-
ture of calcium carbide, and apparatus therefor. Jan. 10.4609. S. J . Boulouvard. Method of purifying hydro-
chloric acid. Jan. 10.5037. J. Mactear. Obtainment of cvano^en compounds.
X - fir J °Jan. i7. .
24,307. T. Wilton. Manufacture and purification ofalkaline cyanides. Jan. 10.
VIIL—GLASS, POTTERY, AND ENAMELS.
APPLICATIONS.
25,139. P. T. Sievert. Improvements in the manufactureox sheet glass. Dec. 19.
25,461. JVL Jones. A new or improved portable devicefor the spraying of colour for the decoration of pottery andthe like. Dec. 23.
25 652. J. R. W. Woodward and X. Collier. Improve-
AlU t T ki i h d
ImP™vements in pressing glass
1900.y *** C> S c W i m P - Improvements in kilns
10 * " " &^ t h e l i k*' Complete Specific.-
Jan. 31,1900.] THE JOUKNAL OF THE SOCIETY OF CHEMICAL INDUSTRY. 93
378. A. Berrenberg aud 0 . Hellstern. Iinprovements inthe manufacture of glass articles, shades, reflectors, and thelike, and in apparatus therefor. Jan. 6.
759. J, J. Griffin and Sons, Ltd., and J. L. Sclanders.Improvements relating to the production of pictures ordesigns in relief on vitreous and other surfaces. Jan. 12.
COMPLETE SPECIFICATIONS ACCEPTED.
1899.522. P. T. Sievert. Manufacture of compound glass and
metal plates or articles. Jan. 17,20,936. A. Metz. Manufacture of plain and ornamental
or decorated ceramic ware aud moulded articles, panels,cornices, and the like. Dec* 30.
21,265. C. H. W. Ruhe. Glass-blow in? machines. Dec. 29.
25,214. J. C. Sellars. Improvements in the manufactureof hollow building blocks and tiles. Dec. 20.
25,431. W. C. Broughton. A new or improved methodof treating a disintegrated slate mixture for the manufac-ture of useful and ornamental articles. Complete Specifica-tion. Dec. 22.
25,734. P. Timofeeff. Improvements in the manufactureof artificial stone and cement for building, paving, railway-sleepers, and other purposes. Dec. 30.
1900.255. J. Leverson,—From J. Steinbach, Austria-Hungarv.
Process for producing porphyry, asphalt, cement slabs orplates. Jan. 4.
552. E. Gobbe. Improvements in cement furnaces.Jan. 9.
572. J. Oddie and W. A. Oddie. An improved cement.Jan. 10.
791. H. Schurholz. Process for the production ofartificial stones. Jan. 13.
COMPLETE SPECIFICATIONS ACCEPTED.
1899.3859. H. A. H. Moore. Manufacture of a substitute for
•china stone. Dec. 29.4252. P. Runge. Process of and apparatus for burning
cement in blast furnaces. Jan. 10.20,929. G. de Bruyn. Artificial building stone. Dec. 30*22,714. C. Straub. Plaster, cement, and the like.
»ec. 30.33,458. M. Miinch-Phipps. Fireproof ceilings. Jan. 17-23,964. C. Czerny and C. Schlirnp. Hydraulic presses
for use in the manufacture of blocks of artificial stone andthe like. Jan. 10.
X.—METALLURGY, MINING, ETC.
APPLICATIONS,
25,207. J. W. Worsey and J. H. Lancashire. Improve-ments in the treatment of copper or antimonial ores, orcopper matte, or the like containing gold or silver or both.Dec. 20.
25,479. H. Le Neve Foster. Improvements relating toiron manufacture. Dec. 23.
25,594. F. Eppler. Improvements in and relating to theprocess of galvanically inlaying metal on materials. Com-plete Specification. Dec. 27.
1900.
253. G. E. Davis and A. R. Davis. An improved processfor separating lead from zinc when both metals exist togetherin solution as nitrates or chlorides, or partly as nitrates andpartly as chlorides, Jan. 4.
2G9. A. James. Improvements in apparatus for pre-cipitating gold and silver from their solutions. CompleteSpecification. Jan. 4.
335. G. E. Davis and A. R. Davis. See Class VII.365. A. James. An improved furnace for melting
metallic precipitates or residues. Jan. 6.393. J. D. Mattison. Improved means applicable for
use in forming and otherwise working metals. Jan. 6.472. G. Harrison. — From Messrs. C. Casoretti and
F. Bertani, Italy. An improved process and apparatusforobtaining zinc" from its ores. Complete Specification.Jan. 8.
710. G.E.Davis and A. R. Davis. An improved pro-cess for the treatment of certain mixed sulphide ores forthe recovery of their valuable constituents. Jan. 11.
817- A. W. Tangye. Improvements in the process^ ofand apparatus for oxidising or roasting ores containingmetallic sulphides, and for the production of gases suitablefor the manufacture of sulphuric acid. Jan. 13.
COMPLETE SPECIFICATIONS ACCEPTED.
1899.2366. C. T. Batclielor. Method of recovery of tin from
tin-plate waste and other waste tin products. Dec. 29.2747. W. A. Macfadyen. Concentrating and separating
certain metals from their ores. Jan. 17.4234. J. Armstrong. Treatment and reduction of oxi-
dised carbonate or combined ores, and in obtaining metalstherefrom. Jan. 10.
20,939. L. Perin. Manufacture of moulded blocks ormasses of steel and other materials. Jan. 17.
22,689. G. Harrison.—From The Xew Process CoatingCompany, United States. Galvanising apparatus. Jan. 10.
23,014. A. Germot. Process of treatment of lead oresfor obtaining metallic lead. Dec. 30.
24,135. J. Gitsbam. Method or process for the extrac-tion and recovery of zinc from sulphide ores. Jan, 10.
XI.—ELECTRO-CHEMISTRY AND ELECTRO-METALLURGY.
APPLICATIONS.
25.490. M. A. P. Monnier. Improvements in secondarybatteries. Dec. 23.
25.491. P. Marino. Iinprovements in accumulatorbatteries. Complete Specification. Dec. 23.
25,721. A. Pallavicini. Improvements in plates forstorage batteries. Complete Specification. Dec. 30.
1900.216. R. Rodrian. Improved manufacture of active mass
for accumulator batteries. Jan. 3.466. \V. J. Wells and Allan and Adamson. Improve-
ments in apparatus for facilitating the escape of gas fromelectric storage batteries or accumulators, Jan. 8.
595. J. de Burgue and R. Sunye. New process of totalsuppression of motive power as well as of electric energyin the industrial production of carbides. Jan. 10.
638. E. A. Le Sueur. Improved electrode, Jan. 11.
675. H. H. Lake.—From R. C. McCartney, United States.Improvements in or relating to electric batteries. CompleteSpecification. Jan. 11.
813. Z. Stanecki. Improvements in the manufacture ofaccumulator plates. Complete Specification, Jan. 13.
COMPLETE SPECIFICATIONS ACCEPTED.
1898.
19,876. O. J. Steinhart, J. L. F. Vogel, and H. E. Fry.Electrolytic separation of zinc from zinc oxide. Dec. 29.
19,878. O. J. Steinhart, J. L. E. Vogel, and H. E. Fry.Manufacture of anhydrous zinc chloride. Dec. 29.
THE JOURNAL OF THE SOCIETY OF CHEMICAL INDUSTRY. [Jan. si, woo.
1899.1844. L. Champagne. Manufacture of plates for secon-
dary batteries. Dec. 29.3648. A. J. 0 . Chalanclre, L. J. B. Colas, and C. J.
Gerard, Electrolysis of salts in solution, and apparatustherefor. Dec. 29.
5099. E. Goller. Storage plates for accumulators, andprocess for the manufacture of the same. Jan. 10.
5322. J. H. Lamprey. Apparatus for the production ofozone by electricity. Jan. 17.
5468. A. Zimmermann.—From Dr. Courant, Germany.Electro-deposition of metals. Jan. 17.
5781. IL L. P. Le Verrier. Electrolysis and electro-lytical apparatus. Jan. 17.
20,986. W. W. Hanscom and A. Hough. Machines forand method of making electrodes for storage batteries.Jan. 10.
23,040. A. J. Boult.—From F. Stormer, Germany.Apparatus for the electrolysis of alkali chloride solutions.Dec. 29.
23,728. M. Wuillot. Manufacture of lead plates forsecondary batteries. Dec. 30.
23,755. J. D Darling and C. L. Harrison. Electrolyticapparatus. Dec. 30.
33,813. Siemens Bros.— From Siemens and Halske,Aktiengesellschaft, Germany. Galvanic batteries. Dec. 30.
24,230. J. L. Roberts. Anode or other electrode for usein electrolysis, and process for making same. Jan. 10.
24,723. F. E. Hatch. Process of smelting ore, andelectric furnaces therefor. Jan. 17.
XII.—FATS, OILS, AND SOAP.
APPLICATIONS.
25,112. W. Fox and T. II. Kingscote. Improvements inoil filters and separators. Dec. 19.
25,225. J. Whiteley and T. Halliwell. Improvements inand connected with toilet and other soaps. Dec, 20.
25,228. J. HeywoocL Improvements iu apparatus forextracting oil from dirtv waste. Dec. 20.
25,357* B. J. 13. Mills. — From A. Lumiere and A.oSTicolle, France. Improvements in the manufacture ofsoap. Complete Specification. Dec. 21.
1900.
430. G. Weber. Improved method of purifying turpen-tine or pine oiJ. Jan. 8.
624. C. J. Rohr. Improvements in the manufacture ofresin soaps suitable for sizing paper. Complete Specifica-tion. Jan. 10.
COMPLETE SPECIFICATIONS ACCEPTED.
1899.21,713. S. Bender. Apparatus for recovering oils from
condensation water by filtration. Dec. 29.22,147. J. Craveri. Composition for wax tapers for
friction matches. Dec. 13.
XIII.—PAINTS, PIGMENTS, VAKNISHES,EESINS, INDIA-RUBBEB, ETC.
APPLICATIONS,
25,130. W. E. S. Bunn and E. J. Case. An improvedmanufacture of lead oxide and white lead, and apparatustherefor. Complete Specification. Dec. 19.
25,233. W. Peel. An improved substitute for vulcanite.Dec. 20.
25,317- G. E. A. Holdsworth. Improvements in anti-fouling composition for ships' bottoms and submergedstructures. Dec. 21.
25,494. Siemens Brothers and Co., Ltd., and W. Diesel-horst. An improvement in the manufacture of gutta-percha.Dec. 23.
1900,
36. H. Kelway-Bamber. A process for renovatingvulcanised and waste rubber, and rendering it fit to beagain used as fresh rubber. Jan. 1.
52. A. Kronstein. Improved manufacture of varnishes,balsams, and resins. Jan. 1.
371. F.Schmidt. Improvements in the manufacture ofgraphited carbon. Complete Specification. Jan. 6.
COMPLETE SPECIFICATIONS ACCEPTED.
1899.14,227. W. R. Lake.—From F. A. M. Kaempff, Ger-
many. Process for the production of a material or sub-stance resembling ebonite. Jan. 10.
19,361. A. E. Lefebvre. Preservative fluid or paint.Dec. 29.
21,134. M. Frank. Insulating material. Dec. 29.22,971, L. Burger. Manufacture of bronze printing
materials. Dec. 29.
XIV.—TANNING, LEATHER, GLUE, AND SIZE.
APPLICATIONS*
25,049. W. Heaton. A new or improved composition ormaterial applicable for the soles and heels of boots andshoes and other purposes. Dec. IS.
1900.1. J. Pullman and E. E. Pullman. Improvements ID
apparatus for stoning and reducing the thickness of skinsin the process of leather dressing and for reducing andequalising the thickness of other fibrous and other sub-stances. Jan. 1.
567. W. H. Glaus and A. Eee. Improvements in themanufacture of dyed leather. Jan. 10.
COMPLETE SPECIFICATIONS ACCEPTED,
1899.1263. T. Lomas. Gelatine drying. Jan. 10.1317. L. Friedlander. Process for treating hides.
Jan. 17.
XV.—AGRICULTURE AND MANURES.APPLICATIONS.
25,086. A. Szigeti. Improvements in instruments forinoculating vine plants with di-sulphidc of carbon. Com-plete Specification. Dec. 18.
25,150. A. Wenck. Improvements in the manufactureof artificial manure. Complete Specification. Dec. 19.
25,653. J. Frost. Improvements in the treatment ofsludge or sewage deposit and fecal or refuse matters ordeposits for the production of manure. Dec. 29.
COMPLETE SPECIFICATION ACCEPTED.
1899.4966. C. Ranson and H. Gouthiere. New or improved
process for the recovery of the sulphurous acid used toenrich phosphatic chalk. Jan. 10.
XVI.—SUGARS, STARCHES, GUMS, ETC.APPLICATIONS.
1900.258. A. Classen. Process for converting cellulose and
starch into fermentable sugar. Complete Specification.Jan. 4. r
259. A Classen. Process for converting wood intofermentable sugar. Complete Specification. Jan. 4.
COMPLETE SPECIFICATIONS ACCEPTED.
1898.19,957. E. Shaw. Apparatus suitable for preparing
syrup for use in the manufacture of sweetmeats. Dec. 29.
Jan. si, woo.] THE JOUENAL OF THE SOCIETY OF CHEMICAL INDUSTRY. 95
1899.
6127. J . Kunstner. Treatment of concentrated or viscidsolutions for obtaining solid particles therefrom in the formof powder. Jan. 17.
22,715. J. Kitsee. Bleaching of sugar juices. Jan. 10.23,158. J. McNeil and C. McNeil. Apparatus for
evaporating or concentrating saccharine or other crystallisahleliquids. Dec. 29.
XVII.—BREWING, WINES, SPIRITS, ETC.
APPLICATIONS.
25,418. M. P. Hatschek. Improvements in the manu-facture of bakers, yeast. Dec. 22.
26,562. S. lcard. An improved method of determiningthe strength of alcoholic solutions, and instruments forapplying such method. Dec. 27.
1900.48. H. A. Hohson. The production of a concentrated
hopped wort. Jan. 1.93. T. W. J. Leuze. A new or improved process of and
apparatus for manufacturing vinegar. Jan. 2.356. A. Ferguson. A method of treating the waste pro-
ducts from distilleries and hreweries so as to produce as aby-product a valuable material therefrom. Jan. 6.
828. G. Ullrich. Improvements in apparatus for heatingor cooling and mixing brewers' mash and similar materials.Complete Specification. Jan. 13.
COMPLETE SPECIFICATIONS ACCEPTED.
1899.174S. J. C. Stead. Process for the purification of waste
liquors from distilleries. Dec. 29.2228. H. V. Laer. Means or process for treating yeast.
and wasting of grain for use in colouring and increasing thepalate fulness of heer. Jan. 10.
3415. J. J. Knight and J . Sampson. Treatment andpurification of the waste liquors of spirit distilleries, and inthe manufacture of useful products therefrom. Dec. 29.
23,057. A. Meyer. Fermenting process, especially foruse in brewing. Jan. 10.
XVIII.—FOODS, SANITATION, ETC., ANDDISINFECTANTS.
APPLICATIONS.
A.—Foods.25,329. E. von I?abler. An improved process for
pasteurising and sterilising milk and other liquids. Dec. 21.25,484. A. Giirber. An improved process for the pro-
duction of condensed milk. Dec. 23.25,554. J. Flockhart. Improved apparatus for raising
and sterilising milk, also applicable for other purposes.Complete Specification. Dec. 27.
25,760. J. T. Knowles.—From G. Eichelbaum, Germany.A manufacture of an improved food from yeast. Dec. 30.
B.—Sanitation.25,085. A. Schantz. Improvements in and relating to
the purification and filtration of water, and apparatustherefor. Complete Specification. Dec. 18.
25,458. W. Watson. Improvements in the method ofand apparatus for treating or purifying and cooling sewageand other effluent waters. Dec. 23.
1900.75. W. D. Scott-Moncrieff. Improvements in or relating
to the bacterial purification of sewage. Jan. 2.245. C. A. Sahlstrom. Improvements in the process and
apparatus for the purification and treatment of sewage.Jan. 4.
550. R. F. W. Smith and The Pioneer Investment Trust,Ltd. Improvements in the bacterial treatment of sewageeffluent and the like. Jan. 9.
Improve-
C—Disinfectants.
1900.
577. J- St. C. Legge and J. P. K. Bradshaw.ments in disinfectants. Jan. 10.
COMPLETE SPECIFICATIONS ACCEPTED*
A.—Foods.1899.
5939. A, Kutschbach. Molasses food compound. Dec. 30.23,360. Montgomerie and Co., Ltd., and J. Montgomerieo
Manufacture of a concentrated extract or food product.Dec. 30.
J5.—Sanitation.
1899.1641. H. Tulloch. Purification of sewage and other
polluted waters. Jan. 17.
C.—D isinfectants.
9400. Adam's Manure and Chemical Company, Ltd.,.and H. E. Macadam. Compound for dipping sheep andother purposes. Jan. 17.
XIX.—PAPER, PASTEBOARD, ETC.
APPLICATION.
25,434. O. Imray.—From The Farbwerke vormals Meis*ter, Lucius und Briining, Germany. Improvements in themanufacture of celluloid in films, pellicles, and other forms.Dec. 22.
COMPLETE SPECIFICATIONS ACCEPTED.
1899.1358. J. Williams. See Class V.3091. J. White. Apparatus for straining paper pulp..
Jan. 17.15,748. W. L. Wise.—From Hoffnuiigsthaler Papier-
fabrik A. and K. Geldmacher, Germany. Manufacture ofpaper. Jan. 10.
20,667. E. C. Staples, F. Greenwood, W. Brearley, and!D. Woodhead. Water and grease proofing of paper,,packing papers, cardboard, and the like, and articles madetherefrom. Dec. 30.
XX.-FINE CHEMICALS, ALKALOIDS,ESSENCES, AND EXTRACTS.
APPLICATIONS.
^ 25,151. C. K. Mills.—From A. Lumiere and L, Lumiere>France. ^ Improvements in the manufacture of organiccombinations of anhydride of benzoic or thiosulphamide.Complete Specification. Dec. 19.
25,152. B. J. B. Mills. — From A. Lumiere and L.Lumiere, France. The manufacture of organic psrsul-phates. Complete Specification. Dec. 19.
25,167. W. P. Thompson.—From The Firm of Schroderand Krumer, Germany. An improved process for obtaining;easily-soluble preparations containing quinine and caffeine.Complete Specification. Dec. 19.
25,510. J. Duncan. Improvements in the manufactureor preparation of extract of coffee or the like. Dec. 23.
25,735. C. D. Abel.—From The Actiengesellschaft fiirAnilinfabrikation, Germany. Manufacture of benzylsilicate. Dec. 30.
1900.
39. H. S. Wellcome and F. B. Power. Certain newsoluble compounds of manganese adapted to therapeuticpurposes. Jan. 1.
THE JOURNAL OF THE SOCIETY OF CHEMICAL INDUSTRY. [Jan. 31,1900.
349- B. J . White. Improvements in or relating to con-centrated extracts for use in the manufacture of beverages.Jan. 5.
530. H. E. Newton.—From Farbenfabriken vormals F .Bayer and Co., Germany. The manufacture or productionof chlorocarbonic ethers, and compounds therefrom. Jan. 9.
753. V. Rollet. Improvements relating to the saponi-fication of the ethylcarbonic ether and of the acetylortho-sulphamin-benzoic anhydride by means of glycerin. Jan. 12.
COMPLETE SPECIFICATIONS ACCEPTED*
1899.5461. C. D. Abel.— From The Actiengesellschaft fiir
Amlinfabrikation, Berlin, Germany. Production of acridine•derivatives. Jan. 17.
19,629. H. H. Lake.—From Chemical Work, formerlySandoz, Switzerland. Manufacture of saccharine. Jan. 17.
XXI.—PHOTOGEAPHY.
APPLICATIONS.
25,110. J. E. Thornton. Improvement in relation tostereoscopic photography. Dec. 19.
25,383. J . E. Thornton. Improvements in or relating tophotographic films. Dec. 22.
25,474. A. Hofmann. Improved apparatus and processfor use in colour photography and the like. Dec. 23.
1900.301. W. H. Babington. A method of producing a per-
manent likeness on copper or other known metals or alloysby the aid of photography for the purposes of decoration.Jan. 5.
470. B. J . B. Mills.—From La Societe Anonyme desPlaques et papiers photographiques A. Lumiere et ses fils,France. Reducing agents for photographic negatives.Jan. 8.
COMPLETE SPECIFICATIONS ACCEPTED.
1899.3560. W. N. L. Davidson. Colour photography. Jan. 10.4290. G. Selle. Process for the production of photo-
graphs in natural colours upon paper or other flexiblesupport. Dec. 30.
XXIL—EXPLOSIVES, MATCHES, ETC.APPLICATIONS.
25,033. A. J. Jacobs. Improvements in matches, fur ees,and the like for use with cigarettes and cigars. Dec.
25,242. J . W. Weston and J . C. Hamilton. Improvementsin explosive compounds for blasting purposes. Dec. 20,
25,686. F . Bender. Improvements in blasting cartridges,Dec. 29.
1900.
212. A. C. Girard. Improved manufacture of picratesJan. 3.
213. A. C. Girard. Improvements in or relating to themanufacture of explosive substances. Jan, 3.
214. A. C. Girard. Improvements in or relating to themanufacture of explosives, Jan. 3.
613. G. J . Batters. Improvements in explosive shells.Jan. 10.
COMPLETE SPECIFICATIONS ACCEPTED.
1899,3678. T. Pickles. Manufacture of tapers or wax matches
and the like. Jan, 10.5707. G. Smith and D. Corrie. Electric fuses for firing,
blasting, and other explosives. Dec. 30.5760. W. J. Oarsman. Manufacture of explosives speci-
ally applicable for use in coal mines. Jan. 17.6971. T.Jenkins. Detonating fog signals for railways and
analogous uses. Dec. 29.
23,954. J . W. Fowler. Detonators. Jan. 10.
XXIII.—ANALYTICAL CHEMISTRY.
APPLICATION,
618. J. Y. Johnson.—From The Chemische Fabrikvormals Goldenberg Geromont and Co., Germany. Im-proved manufacture or production of materials withplatinum surfaces for use as contact substance in chemicaloperations. Jan. 10.
PATENTS UNCLASSIFIABLE.
COMPLETE SPECIFICATIONS ACCEPTED.
1898.20,645. E. K. Maussner. Fire and waterproof material,
and method and apparatus for producing the same.Dec. 30.
22,085. A. J. Boult. — From A. Nieski, Germany.Treatment of materials for fireproof and preservativepurposes. Jan. 10.
