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Disclosure to Promote the Right To Information Whereas the Parliament of India has set out to provide a practical regime of right to information for citizens to secure access to information under the control of public authorities, in order to promote transparency and accountability in the working of every public authority, and whereas the attached publication of the Bureau of Indian Standards is of particular interest to the public, particularly disadvantaged communities and those engaged in the pursuit of education and knowledge, the attached public safety standard is made available to promote the timely dissemination of this information in an accurate manner to the public. इंटरनेट मानक !ान $ एक न’ भारत का +नम-णSatyanarayan Gangaram Pitroda “Invent a New India Using Knowledge” प0रा1 को छोड न’ 5 तरफJawaharlal Nehru “Step Out From the Old to the New” जान1 का अ+धकार, जी1 का अ+धकारMazdoor Kisan Shakti Sangathan “The Right to Information, The Right to Live” !ान एक ऐसा खजाना > जो कभी च0राया नहB जा सकता ह Bharthari—Nītiśatakam “Knowledge is such a treasure which cannot be stolen” IS 3708-5 (2005): Methods of Test for Natural Rubber Latex, Part 5: Determination of KOH-number [PCD 13: Rubber and Rubber Products]
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Page 1: IS 3708-5 (2005): Methods of Test for Natural Rubber Latex ...

Disclosure to Promote the Right To Information

Whereas the Parliament of India has set out to provide a practical regime of right to information for citizens to secure access to information under the control of public authorities, in order to promote transparency and accountability in the working of every public authority, and whereas the attached publication of the Bureau of Indian Standards is of particular interest to the public, particularly disadvantaged communities and those engaged in the pursuit of education and knowledge, the attached public safety standard is made available to promote the timely dissemination of this information in an accurate manner to the public.

इंटरनेट मानक

“!ान $ एक न' भारत का +नम-ण”Satyanarayan Gangaram Pitroda

“Invent a New India Using Knowledge”

“प0रा1 को छोड न' 5 तरफ”Jawaharlal Nehru

“Step Out From the Old to the New”

“जान1 का अ+धकार, जी1 का अ+धकार”Mazdoor Kisan Shakti Sangathan

“The Right to Information, The Right to Live”

“!ान एक ऐसा खजाना > जो कभी च0राया नहB जा सकता है”Bhartṛhari—Nītiśatakam

“Knowledge is such a treasure which cannot be stolen”

“Invent a New India Using Knowledge”

है”ह”ह

IS 3708-5 (2005): Methods of Test for Natural Rubber Latex,Part 5: Determination of KOH-number [PCD 13: Rubber andRubber Products]

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IS 3708 (Part 5) :2005

ISO 127:1995

*%’w-

W$lm’)- Tmd&Rn%wMJTwf?Fi7

$lTJT 5 ihfl-.wx. * m m

Indian Standard

METHODS OF TEST FOR NATURALRUBBER LATEX

PART 5 DETERMINATION OF KOH NUMBER

(Second Revision )

ICS 83.040.10

,.!

,

@ 61S 2005

BUREAU OF INDIAN STANDARDSMANAK BHAVAN, 9 BAHADUR SHAH

NEW DELHI 110002

September 2005

ZAFAR MARG

Price Group 3

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Rubber and Rubber Products Sectional Committee. PCD 13

NATK3NAL FOREWORD

This Indian Standard (Part 5) (Second Revision) which is identical with ISO 127:1995 ‘Rubber, naturallatex concentrate — Determination of KOH number’ issued by the International Organization forStandardization (ISO) was adopted by the Bureau of Indian Standards on the recommendations of theRubber and Rubber Products Sectional Committee and approval of the Petroleum, Coal and RelatedProducts Division Council.

The text of ISO Standard has been proposed to be approved as suitable for publication as an IndianStandard without deviations. Certain conventions are, however, not identical to those used in IndianStandards. Attention is particularly drawn to the following:

a) Wherever the words ‘International Standard’ appear referring to this standard, they shouldbe read as ‘Indian Standard’.

b) Comma (,) has been used as a decimal marker while in Indian Standards, the currentpractice is to use a point (.) as the decimal marker. “

The concerned Technical Committee has reviewd the provisions of the following International Standardsreferred in this adopted standard and has decided that they are acceptable for use in conjunction with ,this standard:

International Standard Title

ISO 123:2001 Rubber latex — Sampling

ISO 124:1997 Latex, rubber — Determination of total sokk conteqt

ISO 125:1990 Natural rubber latex concentrate -- Determinafti”of alkalinity

ISO 976:1996 Rubber and plastics — Polymer dispersion and rubber Iatices —Determination of pH

ISO 1802:1992 Natural rubber latex concentrate — Determination of boric acidcontent

For tropical countries like India, the standard temperature and the relative density shall be taken as27 * 2°C and 65 * 5 percent relatively.

For the purpose of deciding whether a particular requirement of this standard is complied with the finalvalue, observed or calculated, expressing the result of a test or analysis, shall be rounded off inaccordance with IS 2:1960 ‘Rules for rounding off numerical values (revised)’. The number of significantplaces retained in the rounded off value should be the same as that of the specified value in this standard.

,.

,

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i“,I,.

WARNING — Persons using this standard should be femiliar with normel laboratory prectice.Thisstandard does not purport to addressall of the safetyproblems, if any, associatedwith its use. It is

j

the resnonsibilitvof the user to establishappropriatesafetyend health practicesand to ensureI

~

IS 3708 (Part 5) :2005ISO 127:1995

Indian Standard

METHODS OF TEST FOR NATURALRUBBER LATEX

PART 5 DETERMINATION OF KOH NUMBER

(Second Revision )

compliancewith-any national regulatory conditions.

1 Scope

This International Standard specifies a method for thedetermination of tne KOH number of natural rubberlatex concentrate which is presewed wholly or in partwith ammonia. The method is applicable to Iaticescontaining boric acid. The method is not applicable toIatices preserved with potassium hydroxide. It is notnecessarily suitable for Iatices from natural sourcesother tha; Hevea brasiliensis, orthetic rubber, compounded latex,artificial dispersions of rubber.

2 Normative references

for Iatices of syn-vulcanized latex or

The following standards contain provisions which,through reference in this text, constitute provisions ofthis International Standard. At the time of publication,the editions indicated were valid. All standards aresubject to revision, and parties to agreements basedon this International Standard are encouraged to in-vestigate the possibility of applying the most recenteditions of the standards indicated below. Membersof IEC and ISO maintain registers of currently validInternational Standards.

ISO 123:1985, Rubber /atex — Sampling.

ISO 1241992,Rubber Iatices — Determination of totalsolids content.

ISO 125:1880, Natural rubber latex concentrate — De-termination of alkalinity

.,

1), Rubber IaticesISO 976:— — Determination of PH. $,, ,.?‘@

ISO 1802:1885, Natura/ rubber /atex concentrate —Determination of boric acid content.

“1

3 Definition

For the purposes of this International Standard, thefollowing definition applies. .

3.1 KOH number (of latex):The number of gramsof potassium hydroxide equivalent to the acid radicals “’lcombined with ammonia in latex concentrate contain-ing 100 g of total solids.

(Definition taken from ISO 1382:1982, Rubber — VO-

cabulary/Add.2:1982.)

4 Reagents

During the analysis, use only reagents of recognizedanalytical grade and only distilled water free of dis-solved carbon dioxide, or water of equivalent purity.

1) To be published.

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IS 3708 (Part 5) :2005

ISO 127:1995

,.!,

4.1 Potassium hydroxide, standard volumetricsolution, c(KOH) = 0,1 mol/dm3, carbonate-free.

4.2 Potassium hydroxide, standard volumetricsolution, c(KOH) = 0,5 mol/dm3, carbonate-free.

4.3 Formaldehyde,45 g to 50 g in 1 dm3 of solutionIc(HCHO) = 1,5 mol/dm3 to 1,67 moi/dm31, acid-free,prepared by diluting concentrated formaldehyde withwater and neutralizing with 0,1 mol/dm3 potassiumhydroxide solution (4.1 ), using as indicator the faintpink colour of phenolphthalein.

Determine the concentration of the formaldehydesolution as described in annex A.

5 Apparatus

Standard laboratory glassware, plus the following:

5.1 pH-meter,conforming to ISO 976 but capable ofbeing read to 0,01 units.

5.2 Glass alectrode,of a type suitable for use insolutions of pH up to 12,0.

5.3 Mechanical stirrar, with earthed motor andglass paddle, or magneticstirrer.

NOTE 1 An automatic titrator may be used provided it hasbeen checked as giving the same result as the standardmethod.

6 Sampling

Carry out the sampling in accordance with one of themethods specified in ISO 123.

Carry out the determination in duplicate.

Weigh, to the nearest 0,1 g, into a 400 cm3 beaker atest portion (mass m) of the test sample containingapproximately 50 g of total solids. If necessa~, adjustthe alkalinity to (0,5 * 0,1) % ammonia calculated withrespect to the water phase by adding, while stirring,the required quantity of formaldehyde solution (4.3).

Calculate the volume of formaldehyde solution to beadded from the formula

m(l 00- WTS)(A -O, 5)

1134C(HCHO)

when? c(HCHO) is the actual concentration, expressedin moles per cubic decimetre, of the formaldehydesolution (4.3).

iXlute the latex with water to about 30 % total solids.

lnseR the electrodes of the pH-rneter (5.1) into thediluted latex concentrate and record the PH.

If the initiil pH k 16as ?han’ 16,3, akwvty add 5 cms of0,5 mol/dr# potassium hydroxide solution (4.2) whilestirring slowly with the glass paddle or magnetic stir-rer (5.3). Record the resultant equilibrium pH reading.Whh continued stirring, add 0,5 moi/dr# potassiumhydroxide solution (4.2) in 1 cr# increments at regular(e.g. 15s) intervals, recording ths resultant equilibriumpH after each addition. Continua until the end-pointhas been passed.

If the initial pH is 10,3 or higher, omit the initial ad-dition of 5 cm3 at one time and proceed directly to“add 0,5 mol/dms potassium hydroxide solution (4.2)in 1 cms increments” as described above.

The end-point of the titration is the point of inflf?XiOt7 Of

the titration curve of the pH-value against. the volume,in cubic centimetres, of potassium hydroxide solution.At this point, the slope of the curve, i.e. the first dif-ferential, reaches a maximum and the second differ-ential changes from a pasitive to a negative value. Theend-point shall be calculated from the second differ-ential on the assumption that the change from a posi-tive to a negative value bears a linear reiation to theaddition of potassium hydroxide during the 1 cm3 in-tewal involved.

An example of a typical titration and the calculation ofthe end-point is given in annex B.

The results of duplicate determinations shall agree towithin 5 ‘Yo (m/m).

7 Procedure

Calibrate the pH-meter by the method specified in ISO976. If the total solids (WTJ and alkalinity W of thelatex are not known, determine them in accordancewith ISO 124 and ISO 125 respectively. If the latexcontains boric acid and the content is not known,determine it in accordance with ISO 1802.

8 Expression of results

Calculate the KOH number, expressed as a per-centage by mass, of the latex concentrate from theformula

2

k

2

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IS 3708 (Part 5) :2005ISO 127:1995

561c.vw~~ m

where

\ c is the actual concentration, expressed inmoles of KOH per cubic decimetre, of thepotassium hydroxide solution (4.2);

V is the volume, in cubic centimetres, of thenominally 0,5 mol/dm3 potassium hydroxidesolution (4.2) required to reach the end-point;

wT~ is the total solids content, expressed as apercentage by mass, of the latex concen-trate;

m is the mass, in grams, of the test portion.

If the latex concentrate contains boric acid, subtractthe KOH number equivalent to the boric acid from theKOH number obtained above. Calculate the KOHnumber equivalent to the boric acid present from theformula

91X$

where WBA is the boric acid content, expressed as apercentage by mass.

9 Test report

The test report shall include the following information:

a)

b)

c)

d)

e)

f)

g)

a reference to this International Standard;

all details necessa~ for complete identification ofthe sample;

all details necessary for complete identification ofthe pH-meter used;

the result obtained;

the correction applied for boric acid, if present;

details of any operation not included in this inter-national Standard or regarded as optional;

the date of the test.

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IS 3708 (Part 5) :2005ISO 127:1995

Annex A(informative)

Determination of formaldehyde

The method given in previous editions of this inter-national Standard appears not to have been widely useddue to the fact that standard solutions of ammonia areconsidered to be unsatisfactory. Having regard to theconsistent quality of analytical-grade concentratedformaldehyde solution, the majority of users prepare astandard solution of formaldehyde directly.

Where it is necessary to determine the concentrationof the diluted formaldehyde, a variety of methodsexist and users are referred to the Encyc/opaedia ofIndustrial ChemicalInterscience (1971).information only.

A.1 Reagents

Analysis, Vol. 13, published byThe method given below is for

A.1.1 Sodium sulfite,anhydrous, analytical grade.

A.1.2 Sulfuric acid, standard volumetric solution,C(H2S04) = 0,25 mol/dm3.

A.1.3 Thymolphthalein, indicator solution.

Dissolve 80 mg of thymolphthalein in 100 cm3 of ethylalcohol and dilute with 100 cm3 of distilled water.

A.2 Procedure

Prepare a solution of 125 g of anhydrous sodium sul-fite (Al.1 ) in 500 cm3 of water and dilute to 1 dins.

Transfer 100 cms of the solution to a 500 cm3 conicalflask. Accurately weigh into the flask 6,0 g to 8,0 g ofthe nominally 50 g/dins formaldehyde solution (4.3)2,and swirl to mix thoroughly. Allow to stand for 5 rein,then titrate with 0,25 mol/dm3 sulfuric acid (Al .2) tothe first colorless end-point using thymolphthalein(Al .3) as indicator. Run a blank determination withthe soldium sulfite solution.

A.3 Expression of results

Calculate the formaldehyde content, expressed as apercentage by mass, of the formaldehyde solutionfrom the formula

30,03(VI - Vz) x 2c(HzS04)

1Oml

where

v, is the volume, insulfuric acid (Al .2)

cubic centimetres, ofused for the titration of

the test portion of formaldehyde solution;

v* is the volume, in cubic centimetres, ofsulfuric acid (A. 1.2) required for the blank;

C(H2SOJ is the actual concentration, in moles ofH2S04 per cubic decimetre, of the sul-furic acid;

ml is the mass, in grams, of the test por-tion of formaldehyde solution.

‘.,,

2) When analysing concentrated formaldehyde solution, 1,8 g to 2,0 g of solution is a more convenient amount to take

4

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IS 3708 (Part 5) :2005ISO 127:1995

Annex B(informative)

Example of a typical titration and calculationof end-point

TableB.1— Exampleof a typicaltitrationto show variationin pH

Volumeof KOHsolutionaddad FirstdifferencepH reading Seoonddiffarenoe

cm3 ApH/cm3 A2pH/cm3

Initial 10,09

5 10,460,09

6 10,55 0,010,10

7 10,65 0,010,11

8 10,76 0,030,14

9’ 10,90 0,040,18

10 11,08 0,060,24

11 11,32 0,070,31

12 11,63 –0,010,30

13 11,93 –0,090,21

14 12,14

In this example, the first difference reaches a maximum of 0,31 between 11 cms and 12 cms of potassiumhydroxide solution. The precise point of inflexion is calculated from the ratio of the adjacent seconddifferencevalues, i.e. 0,07/(0,07 + 0,01) = 0,875 of the difference between 11 cms and 12 cm3, i.e. 11,875 ems.

Figure B. 1 presents this data graphically to show the point of inflexion,

5

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IS 3708 (Part 5) :2005ISO 127:1995

!’/’

It/1

End-point

loA~567891011 1213V+

12,2-

~

12

11,8-

11,6-

11,4-

11,2-

11

10,8-

10,6 -

Volume of potossium hydroxide solution (cm’)

Figure B.1 — Illustrative curve showing change of pH during titration

6

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Bureau of Indian Standards

BIS is a statutory institution established under the Bureau of Indian Standards Act, 1986 to promote

harmonious development of the activities of standardization, marking and quality certification of goods

and attending to connected matters in the country.

Copyright

BIS has the copyright of all its publications. No part of these publications maybe reproduced in any form

without the prior permission in writing of BIS. This does not preclude the free use, in the course ofimplementing the standard, of necessary details, such as symbols and sizes, type or grade designations.Enquiries relating to copyright be addressed to the Director (Publications), BIS.

Review of Indian Standards

Amendments are issued to standards as the need arises on the basis of comments. Standards are alsoreviewed periodically; a standard along with amendments is reaffirmed when such review indicatesthatno changes are needed; if the review indicates that changes are needed, it is taken up for revision.Users of Indian Standards should ascertain that they are in possession of the latest amendments oredition by referring to the latest issue of ‘BIS Catalogue’ and ‘Standards: Monthly Additions’.

This Indian Standard has been developed from Doc: No. pCD 13 (1998).

Amendments Issued Since Publication

Amend No. Date of Issue Text Affected

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