+ All Categories
Home > Documents > everyspec.comeveryspec.com/MIL-SPECS/MIL-SPECS-MIL-E/download.php?... · MIL-E-22267A (d)...

everyspec.comeveryspec.com/MIL-SPECS/MIL-SPECS-MIL-E/download.php?... · MIL-E-22267A (d)...

Date post: 07-Sep-2021
Category:
Upload: others
View: 1 times
Download: 0 times
Share this document with a friend
20
ll!llL:E-22267A 31 MAY 1963 1 SUPERSEDING MIL-E-22267(Wep) -11 APRIL 1962 MIH\TARY Specification . EX~LOSIVE ,, !l’his speoijication has ~O~l?OSITIO~S, HBX TYPE .. been approved by the” Department of Defense and is mandato~ fo~ use by the Department of the Armv, the Navy, and the Air Force. / ‘1. SCOPE . ,. 1.1 Scope. This specification covers three explosive compositions of the HBX type. , These are: HBX-1, HBX–3 and H-6. 1.2 Classification. The explosive.composi- tions shall be of the following. grades,, as specified (see 6.2). ~ Grade A — HBX type compositions ‘prepared from new ,- components \Grade B — HBX type compositions , prepared from re- claimed explosives 20’APPLICABLE DOCUMENTS .2.1 The following documents of the issue in effect on dat,e of invitation for bids or request for proposal, form a part of the specification to the extent specified herein. SPECIFICATIONS FEDERAL RR-S-366 Sieves; Standard, for Testing Purposes MILITARY JAN-T–248 —Trinitrotoluene (TNT) MItiR-398 RDX MIL-C-401 — Composition B MIL-A-512 —Aluminum Powder, Flaked, Grained and Atomized MIUC-3301 — Compound, Asphaltic, Hot-Melt (Cavity Lining) ,. MIL-C-13573 — Calcium Chloride, Anhydrous MIL-C-18164 — Composition D–2 MIL-C-51077 —Calcium Silicate, Technical STANDARDS - MILITARY MIL-STD-129 — Marking for Ship- ment and Storage PUBLICATIONS BUREAU OF NAVAL WEAPONS OP 400 General instructions foi the Design, Manufacture and Inspection of Naval Ordnance Equip- ment OD 18796 Advisory Process for the Preparation of ‘m Downloaded from http://www.everyspec.com
Transcript
Page 1: everyspec.comeveryspec.com/MIL-SPECS/MIL-SPECS-MIL-E/download.php?... · MIL-E-22267A (d) Temperature The temperature shall be recorded, prior to, during, and after each phase of

ll!llL:E-22267A

31 MAY 1963

1 SUPERSEDINGMIL-E-22267(Wep)

-11 APRIL 1962

MIH\TARY Specification.

EX~LOSIVE

,,!l’his speoijicationhas

~O~l?OSITIO~S, HBX TYPE

..

been approved by the” Department of Defense and ismandato~ fo~ use by the Department of the Armv, the Navy, and the Air Force.

/‘1. SCOPE .

,.

1.1 Scope. This specification covers three

explosive compositions of the HBX type.

, These are: HBX-1, HBX–3 and H-6.

1.2 Classification. The explosive.composi-

tions shall be of the following. grades,, as

specified (see 6.2).

~ Grade A — HBX type compositions‘prepared from new

,- components

\Grade B — HBX type compositions, prepared from re-

claimed explosives

20’APPLICABLE DOCUMENTS

.2.1 The following documents of the issue

in effect on dat,e of invitation for bids or

request for proposal, form a part of the

specification to the extent specified herein.

SPECIFICATIONS

FEDERAL

RR-S-366 — Sieves; Standard, for

Testing Purposes

MILITARY

JAN-T–248 —Trinitrotoluene (TNT)

MItiR-398 — RDX

MIL-C-401 — Composition B

MIL-A-512 —Aluminum Powder,Flaked, Grainedand Atomized

MIUC-3301 — Compound, Asphaltic,Hot-Melt (CavityLining),.

MIL-C-13573 — Calcium Chloride,Anhydrous

MIL-C-18164 — Composition D–2

MIL-C-51077 —Calcium Silicate,Technical

STANDARDS - “

MILITARY

MIL-STD-129 — Marking for Ship-ment and Storage

PUBLICATIONS

BUREAU OF NAVAL WEAPONS

OP 400 — General instructions

foi the Design,

Manufacture and

Inspection of Naval

Ordnance Equip-

ment

OD 18796 — Advisory Process for

the Preparation of

‘m

Downloaded from http://www.everyspec.com

Page 2: everyspec.comeveryspec.com/MIL-SPECS/MIL-SPECS-MIL-E/download.php?... · MIL-E-22267A (d) Temperature The temperature shall be recorded, prior to, during, and after each phase of

t/

‘MI&E-22267A :,.,, ..-,-,HBX Type Explo-,. .: ..:.. . sives

(Copiesof specifications,s$andards,drawings,andpublicationsrequiredby suppliersin connectionwithspecificprocurement functionsshould be obtainedfrom the procuring activityor i=m‘directedby thecontractingofficer.)

INTERSTATE COMMERCE ‘. ...COMMISSION

49 CFR 71-90 — Interstate Commerce‘,,

-Commission Rulesand Regulations forthe Transportation

., . . of Explosives andOther Dangerous.’ .... . .... . -.4.

-Articles “.<. .(The InterstateCommerce Commission Regula-,

tionsare now a part of the Code of FederalRegula-tionsand are avaiIablefrom the SuperintendentofDocuments, ‘Government l%inting Office,Washing-ton 25, D. C. (Orders for the above publicationsshould cite “the latest issue and supplementsthereto),?)

3. REQUIREMENTS

3.1 Preproduetion samples. Unless other-wise specified in’ the contract or order, thepreprodudtion samp~e shall be- prepared byusing the methods and procedures pk.oposedfor the production lot. The sample shall-betested as specified in Section 4 herein for thepurpose of determining. that..the. compositionmeets the requirements of this specification.Provision of the sample shall be as specifiedin 4.3.1. .

. .. .

,-TABLE I;Grade

,... .

.,

..

3.2 Form. Unless’otherwise specified in thecontract or Order, ‘Explosive Composition,IIBX Type, shall be supplied in the form ofbuds or as strips. Approximate dimensionsof the. strips shall be 11/2 inches wide, 1 inchdeep”and 3 inches long (see 6.2).

3.3 HBX preparation. Advisory, processtechniques outlined ‘in-publication OD–18796may be” used- in the batching and prepara-tion of ,HBX compositions. However, whenthe applicable advisory process techniquesare used, the”, order in which aluminumpowder and calcium chloride ‘are added inthe HBX formulations shall be mandatoryand in accordance with the batching. proce-dures of OD–18796. During batching, themixtures shall. be free from” foreign rnde-rials and visible impurities ‘other than ‘thepolymerized organic material, derived fromthe desensitizer compounds or hot melt inthe Grade B compositions. .

.“.3.4 “’”Components. The components used in

the preparation of the Grade A HBX com-

position. shall comply with the specifications

listed in 2.1 and shall be of the following

grade or class’” as applicable.

Composition B ‘Grade A

TNT .Grade I ““

Aluminum .” .- Type 111, Grade F,

Powder ‘- ‘ Class 7

3.5 Grade A compositions. The.coniposition

of the Grade A HBX composition shall con-

form to the- ‘“nearest-tenth percent as re-

quired in Table I when ,tested as specified

in 4;4.3,2 or 4.4.3.3. . 2,. .,-. ,-.

A compositions ,... -..

HBX-1 HBx-3 H-6Ingredient Percentbyweight Percentbyweight Percentbyweight

* RDX plusnitrocellulose........................................ 40.4 A 3.O”yo ‘, 3+.3 * “3.070 45.1 * 3.0%plus ** Calcium Chloride , .. ...-plus ***Calcium Silicate

. ... ..

TNT ............................................................................. 37.8 * 3.0’%0 29.0 & 3.0% 29;2 + 3;0’%

Aluminum’ .................................................................. 17.1‘& 3.070 34.!3’$ 3.O~o .2i.o”~3.0%..

****Wax PIUS lecithin............................................ 4.7 * l.oqo 4.9’:*’71;09Z 4.7 * l.oyo

*iVote.All of the RDX component and portionsof t~e TNT and wax are added as CompositionB.*,*A separa~,calcium chloridedeterminationneed onlybe done ifrequiredin the contractor order (see

,:-

2

Downloaded from http://www.everyspec.com

Page 3: everyspec.comeveryspec.com/MIL-SPECS/MIL-SPECS-MIL-E/download.php?... · MIL-E-22267A (d) Temperature The temperature shall be recorded, prior to, during, and after each phase of

,:,

I MIIcE-22267AI! 6.2 ). “Percentage requirement of Calcium Chloride is 0.5% “’~ 0.17’.. 3. ,.1

**’; ‘Calcium ‘Silicate shall be determined as specified in 4.4.1.2 when used in the forrn.ulation of HBX COrn-

i ‘pounds. The Calcium Silicate content shall ,be a minimum of 1:25 weight percent of, the TNT content of the

ii ]1 mixture and shall only be used in the HBX compositions when specified by”the procuring agency (see 6.2).

Calcium Silicate is designated for use only in Army formulations of HBX type explosive compositions.~, ~ **** The major portion of the wax and all of the nitrocellulose and lecithin are added as Composition

D-2. ,, . .,,!’ I\ ~

I ,.... ,. ;:,,II! .3.6 Grade, B compositions. The composi- qumed ‘in Table II “when’determined as speci-,I~ I ~ tion .of the Grade ,B HBX Composition’ shall fied in” 4;4.3.4. .,,

I‘, ~ I conform ,to’ the nearest tent$ percent as re- ‘.

II, ~ “ ‘“ ‘ “’; ““,! 1 ~

.: TABLE II.Grade B cow~positions.,. ,.

l\ HBX-1 HBX-3 H-6Ingredient Percentbyweight Percentbyweight Percenthyweight

11 i ! RDX plus nitrocellulose............................’............. 40.4 A 3.0% : 31:3 A 3.076 ‘ 45.1 ~ 3.O~o \1! 1’I : plusGatcium Chloride “ ‘i, II plus * Calcium Silicate ‘ , ,,. , ~ ,. ,,, ,

II TNT ............................................................................1!

37.8 ~ “3.0% 29.0 k 3.()~o 29.2 A 3.O~o.-,

! Aluminum ...............................................................'..17.1 * 2.OYO 34.8 a 3.0% 21.0 ? 3.O~o,.

!~1 Wax plus lecithin ,.,..,... .... .... ..........., 4.7 * lj)yd “4.9A ‘1.O?’O 4.7 * 1.0%

Hot melt (asphalticliningmaterial)— rnaximufi allowable0.75%.,

;I A separateCalcium Chloridedeterminationneed only be done if required in the contract or ‘order. An1 additional one half percent of Calcium Chloride shall be added whenever preparing the reclaimed explosive

1 for re-use. percentage requirement is ().77. A 0.39’.. “.

i ~ ;,., .,

* The calcium silicate content’ shall be a minimum of 1.25 weight percent of the TNT content of the! mixture and” “shall ‘only be used in the HBX compositions when specified by the procuring agency (See 6.2).I Calcium Silicate shall be determined as specified in 4.4. 1.2.i

,.

i.:

iI I 3.7 Moisture. The moisture content of the ble documents which form a part of this~,~’ HBX compositions when tested ‘as specified\ I ,

specification shall be referred in writing toin 4.4,4, shall be” as” follows: the procuring agency or appointed agent for11 I! 1 Grade A - 0.20”% MAXIMUM “‘ ‘, interpretation and clarification.

II1]1, “Grade B — 0.50$!6 MAXIMUM “,.

3.11 Process verification and lot accept-! ., ante tests. Unless otherwise specified in theI 3.8 Vacuum stability. The maximum’ vol- contract or order, the process verificationi’ ume of gas liberated by the” HBX composi- used as> the inspection’ system and lot ac-

~ I ;tions when tested as specified “in 4.4:5 shall~., ceptance tests shall be conducted on eachbe 2cc/gram/48 hours at 100°C. “~. ~~~ lot.”of HBX explosive composition. I

I ~:,,. .,, 3.9 Requests for deviation. Requests for 4. QUALITY ASSURANCE PROVISIONSi

deviation from this specification or appli- ,I ..’., ~ble documents which form a part of this 4.1 Unless otherwise specified in the con-!‘i specification shall be “as set forth in OP “400. tract or purchase order, the supplier is re-i ‘i, sponsible for the performance of all inspec-

3.10 Conflicting requirements. Conflicting tion requirements as specified herein. Ex-1, requirements arising between this specifica- cept as otherwise specified,”the supplier mayi tion and any other specification or applica- utilize his own facilities or any commercial

j , I : 3>~

~,, i :

I/ I i~

Downloaded from http://www.everyspec.com

Page 4: everyspec.comeveryspec.com/MIL-SPECS/MIL-SPECS-MIL-E/download.php?... · MIL-E-22267A (d) Temperature The temperature shall be recorded, prior to, during, and after each phase of

MIL-E-22267A

laboratory acceptable to the Government.The Government reserves’the right to per-forni any of the inspections set forth in thespecifications where such inspections aredeemed necessary. to assure supplies andservices conform to prescribed requirements.

“4.2 .Lot” size. For the purpose of sampling,a lot of any HBX composition shall be limitedin weight to 1300 pounds maximum and toone batch from a single vessel.

4.3 sampling.

4.3.1 Preproduction samples. After awardof contract but prior to entering quantityproduction, a preproduction sample shall be,prepared for inspection and acceptance teststo determine “conformance of the sample withthe. requirements of the specification (see6.2). The sample shall be manufactured bythe procedure and processes and at the samelocation proposed by the contractor for theexecution of the contract, The sample will be.supplied in bud form, strips or poured intotrays to a thickness of approximately oneinch as specified by the procuring activity.(see 6.2). When preproduction sample hasbeen approved, the contractor will be noti-fied and will be authorized by the procuringactivity to proceed with production. Anyproduction started’ before such approvaIshall be at”the contractor’s risk.” Preprod’uc-tion samples accepted will be applied as partof, the quantity specified by the contract ororder. Packaging, and shipment ,of the sam-ple will be “inaccordance with Section 5.,,, ,

4.3.1.1 Preproduction sampk for subse-quent contracts. The necessity for a prepro-duction sample will be determined by theprocuring activity when production under a

,.

i

new contract by the same contractor at thesame location follows the preparation of- anyHBX Imposition cover4d by this specifica-tion.

4.3.2 Samples for destructive trots.

4.3.2.1 Sample for chemical compositionanalysis. A wafer sample approximately fourinches in diameter by one quart& inch thickis taken from the stream of the explosive asit is being withdrawn f or use. The sample istaken by catching a portion of the moltenexplosive, from the approximate center ofthe batch, and pouring into shallow ahuni-num mold of the dimensions given above.Tags, embedded in each sample while molten,identify the source of the sample.

4.3.2.2 Sample for moisture a?udwj.s. Ik-serve 50 grams of the sample from 4.3.2.1and place in a closed container to be usedin the moisture analysis.

4.4 Test procedures.

.44.1 Process verification. Unless otherwisespecified in the contract or order, proc~sverification used as the inspection systemshall be subject to Government verificationat the time the first batch is prepared andat random intervals during the production,but not less than once during each week ofcontinuous operation. Verification will con-sist of surveillance of the process and re-lated equipment to determine that practices,methods and procedures are being properlyapplied, and ,that the products are-producedunder the requirements. of this specification.A record “shallbe made of each batch d ex-plosive prepared to insure that the followingrequirements have been met:

(a) Explosive components Components shall meet the requirements of 3.4.

; (b) Composition The quantities of each component required shall be cal-culated and weighed to give the correct composition~Component weights may be calculated from Table III.

(c) Order of addition The order of “addition shall be “recorded. Order of addi-!- .,,”.- .,,’. tion shall be mandatory as specified in 3.3. .

4

Downloaded from http://www.everyspec.com

Page 5: everyspec.comeveryspec.com/MIL-SPECS/MIL-SPECS-MIL-E/download.php?... · MIL-E-22267A (d) Temperature The temperature shall be recorded, prior to, during, and after each phase of

MIL-E-22267A

(d) Temperature The temperature shall be recorded, prior to, during, andafter each phase of batching.

(e) Agitation Agitation shall be maintained from the time of the addi-tion of the first component until the kettle has beendrained.

(f) Mixing time The mixing time following the addition of the last com-ponent.

TABLE.III.HBX compositions(Percent by weight)

., HBX-1 HBX-3 H-6

CompositionB ....................................”. 66.08 51.33 74.20

CompositionD-2 “....:............................. 4.66 4.73 4.69

Aluminum ..........................’.................. 17.10 34.75 20.61

AdditionalTNT .................................. 11.66 8.69 —

Calcium Chloride..;............................. 0,50 0.50 0.50CalciumSilicate ...................................,” .0,471 0.36’ .0.371

Eachcomponentshallbe basedon thepercentby “weightlimitation,listedin Table I or II for each HBXformulation.

1Whena~ecitiedby theprocuringactivity,CalciumSilicateusedintheformulationofHBX componentsshallbe a minimumof. 0. —-,—t. —-—.-—. -. . . . “..,”. .. —.. —.

4.4.1.2 Determination of Calcium Silicate.When specified by the procuring activity(see 6.2), Calcium Silicate used in the HBXcomposition shall be determined by visualverification of the weight of calcium silicateadded to the batch. Quantities added shallbe calculated in terms of weight percent ofthe TNT content.

4.4.2 ‘Lot acceptance tests. Unless other-wise, specified in the contract or order, sam-ples’ selected from each inspection lot shallbe subjected to all the requirements andtests of this specification. Failure of theHBX compositions to meet any of the re-quirements or tests of this specification shallbe considered cause for rejection of the lot.

.4.4.3 Composition analysis?.

4.4.3.1 Sample preparation.. Reduce sam-ple through a 20 mesh screen (U. S. Stand-ard Sieve Series) using a wooden’ mor@w andpestle. ...

4.4.3.2 Method of analysk. Grade A.

4.4.3.2.1 Determination of aluminum.Weigh accurately a sample calculated to con-tain 0.4 grams of TNT into a tared sinteredglass filtering crucible, medium porosity, 30-ml capacity. Extract on a Fisher filtratorwith ethylene chloride (purified 1, 2 dich-loroethane) at approximately 20° ‘C., 5 equalportions totaling, 45 ml, contact time of 1minute each. Collect filtrate in a 50 ml vol-umetric flask. Reserve filtrate for TNT de-termination.

The residue remaining on the filtering cru-cible is extracted with hot cyclohexanone(highest purity grade) at approximately100° C. Five consecutive 3 second extrac-tions of 3 ml each with continuous” vacuumfiltration and no stirring are made. This isfollowed by four consecutive 30 second ex-tractions of 10 ml each with stirring. Afterthe cyclohexanone extraction, wash downthe sides of the crucible with approximately2 ml of reagent grade acetone. Repeat for atotal of 3 washings. Dry in an oven at 90° C~ 10° C. for 30 minutes, cool @ a desic-cator and weigh. The residue is aluminum.

5

Downloaded from http://www.everyspec.com

Page 6: everyspec.comeveryspec.com/MIL-SPECS/MIL-SPECS-MIL-E/download.php?... · MIL-E-22267A (d) Temperature The temperature shall be recorded, prior to, during, and after each phase of

MILi-E-22267ii

Percent aluminum= (A-B) (100).,.

w..;.;,,,

A = Weight of crucible plus aluminutilresidue

B = Original weight of “empty crucible

W = Weight of sample

4.4.3.2.2 TNT determination. Dilute theTNT filtrate obtained in 4.4.3.2.1 to 50-rnlwith ethylene chloride. Compare its spectralabsorbance at 20° .C. with that “of a solution(0.400 grams of TNT/50-ml ethylene chlo-ride) at 367 millimicrons. TNT is deter-mined by reference to a graph prepared inadvance from known solutions. The prepara-tion of the solutions and the graph is de-scribed in 4.4.3.5.1. A Beckman DK–2 orequivalent spectrophotometer may be usedto determine the spectral absorbance.

The spectral absorbance may be measuredon a Beckman DK–2 recording spectro.photo-meter under the following conditions:

(a)

(b)

(c)

(ii)

(e)

(f)

(g)

(h)

(i)

10 mm cell with a 9 mm spacer

Wavelength setting of 367 mi]]imi-

crons

Time constant of 0.6

Scanning time of 1

Scale expansion – 2X

Sensitivity – 11.5

Absorption scale of – 0.3 + 0.7

Hydrogen lamp

Photomultiplier position – 1X :

Percent TNT = A x 100—w

. A = Weight of TNT from graph

,W = Weight of sample “‘

4.4.3.2.3 Detwvnindion of wax + lecithin.A separate 3 gram portion of the HBXsample is accurately weighed and transfer-

6

red to small test tube: Accurately weigh thetest tube and contents. Heat tube and con-tents to 90° C. stirring vigorously. Transferthe test tube to a water bath used to main-tain the prisms of an Abbe’ refractometerat 50.0° C. & 0.5’ C. After cooling, reweightube and contents to determine loss of te-trachloroethylene due to volatilization. Theexact amount of tetrachloroethylene lost inheating shall be replaced and the test tubereplaced in the water bath. Set the refrac-tometer to read 1.4910 as the refractiveindex of tetrachloroethylene at 50.0° C. &0.5° C. Pour several drops of the super-natant liquid in the test tube ,onto the prismsof the refractometer. The prisms are quicklyclosed and at the end of 30 seconds the indexof refraction to sodium D light is determined.The wax + lecithin concentration is deter-mined by reference to a graph previouslyprepared from known solutions. The prep-aration of the solutions and the graph aredescribed in 4.4.3.5.2.

. . Percent” wax + lecithin = (C) (100)

w

C = Weight of wax + lecithin fromthe. graph

W = Weight of the sample

4.4.3.2.4Determination of calciumride: Weigh accurately a 2 gram HBXwle into a tared sintered glass filtering

chlo-sam-cru-

cible, medium porosity, 30-ml caPacitY.Using a Fisher filtrator with water vacuum,extract sample with 100 ml of distilled water,-10 extractions, 10 ml each, of 30 secondsduration. Collect filtrate in a 250 ml 13rlen-meyer flask. Cool to room temperature.

Add 2 ml of 0.1 M potassium chromate indi-cator to the filtrate. For the preparation ofthe 0.1 M potassium chromate see 4.4.3.5.3.Titrate to the end point with 0.1 N silvernitrate. For the preparation of the 0.1 Nsilver nitrate see 4.4.3.5.4. The end point isnoted by the first appearance of a permanentcolored precipitate of silver chromate. Theend point should be determined by using a

Downloaded from http://www.everyspec.com

Page 7: everyspec.comeveryspec.com/MIL-SPECS/MIL-SPECS-MIL-E/download.php?... · MIL-E-22267A (d) Temperature The temperature shall be recorded, prior to, during, and after each phase of

white background or by transferring filtrateplus a minimum of distilled water washingsto a white casserole. !

percent Calcium Chloride =,,’

(V) .(N) (0.0555), (100)

MIL-E-22267A

final rinse of the crucible contents with 5ml of benzene saturated with RDX. Collectthe filtrate which contains TNT and wax ina 100-ml volumetric flask. R&serve the filtrateto determine the TNT content. Aspirate thecrucible for 1 minute after the final rinse.

w.

,,.

V = ml of s“i]ver nitrate ;N = Normality of silver nitrate

0.0555 = Millequivalent weight of, calciumchloride

W = Weight sample

4.4.3.2.5 Determination of RD.X + nitro-cellulose. The percentages of. TNT, calciumchloride, aluminnm, and wax + lecithin areadded and their sum subtracted from 100percent. The remainder is taken to be thepercentage of RDX plL~snitrocellulose.

4.4.3,3 Alternate method’of analysis. GradeA.

4.4.3.3.1 Determination of RDX + nitro-cellulose. Weigh accurately a sample of HBXcalculated to contain between 0.35 and 0.40grams of TNT into a tared 100 ml beaker.Add 20 ml of RDX saturated benzene to thebeaker. The preparation of the RDX satu-rated benzene is described in 4.4.3.5.5. Coverbeaker with a watch glass and place on asteam bath for 30 minutes, swirl solutionfrequently. (An oscillating hot plate may beused if available. ) Do not boil the benzene!After removal from the steam bath, coolsample to room temperature. Allow a mini-mum of 1 hour cooling.

Make a quantitative, transfer of the sampleto the original tared filtering crucible. Filterusing a Fisher Iiltrator with water suction.Use a small polyethylene wash bottle whichcontains benzene saturated with RDX tomake the transfer. Make a total of 3 wash-ings of the beaker and residue on the oru-cible, using between 10 and 115ml. of ben-zene saturated RDX per rinse. Make a

The crucible plus its contents are placed ona Fisher filtrator and extracted with hotdistilled water, 3 portions of 5 ml each, 30seconds contact time for each washing. Thisis necessary to remove any calcium chloridethat may be remaining in the residue. Drycrucible and its contents in an oven at 90° C.& 10° C. for 1 hour. Cool the sample in adesiccator and weigh.

The crucible and its contents are placed ona Fisher filtrator, attached to a water aspi-rator. Extract the sample with four – 20-mlportions of hot, reagent grade, acetone. Al-low 30 seconds contact time between solventand sample before applying suction for eachextraction. Wash down the sides of the cru.cible with two additional portions of 10 mleach of hot acetone. Place crucible and itsresidue in an oven to dry at 90° C. & 10° C.for 30 minutes, cool in a desiccator andweigh. RDX and nitrocellulose are removedin the filtrate. Aluminum remains as the re-sidue on the crucible.

Percent RDX + nitrocellulose =

(A-B) (100)

w

A = Weight of sample plus cruciblebefore acetone extraction

B = Weight of residue plus crucibleafter acetone extraction

W = Weight of sample

4.4.3.3.2 Detemin.ution of aluminum. Thealuminum is the residue remaining on thecrucible after the acetone extraction.

Percent aluminum = (B-D) (100)

w

Downloaded from http://www.everyspec.com

Page 8: everyspec.comeveryspec.com/MIL-SPECS/MIL-SPECS-MIL-E/download.php?... · MIL-E-22267A (d) Temperature The temperature shall be recorded, prior to, during, and after each phase of

NIL-E-22267A

B = Weight of residue plus crucibleafter acetone extraction

D = Weight of original crucible

W = Weight of sample

4.4.3.3.3 Detemzinution of TNT. For meth-od of preparation and standardization ofsolutions needed in the TNT determinationsee 4.4.3.5.6 through 4.4.3:5.13.Dilute the TNT and wax filtrate obtained in4.4.3.3.1 to 100-ml with benzene saturatedwith RDX. Transfer a 10 ml aliquot of theTNT solution which contains 35-40 mg ofTNT to a 300 ml reduction flask (ScientificGlass Atiparatus Co. JD2776 or equivalent issatisfactory. ) Evaporate the benzene to dry-ness with a slow” stream of dry air (connecta drying tube between air supply and inlettube of flask.)

Dissolve the residue in 25 ml of reagentgrade glacial acetic acid (measure in a cy-linder.) Sweep the flask with N2 or “C02 gasfor 5 minutes. Pipette accurately 25 ml of0~2N titanous chloride solution into theflask. Add 25 ml of 6N HC1. A current ofC02 or N2 should be passed through thereaction flask during the refluxing, coolingand titration periods to prevent air oxidat-ion of the titanous ion. Reflux for 15 min-utes, using glass beads to reduce bumping.(Ground glass joints on the flask and con-denser are to be preferred. A Glass-Col heat-ing mantle is the most convenient source ofheat, though a hot plate may he used.) Coolthe flask to- room temperature’ without dis-connecting the” reflux condenser. (Lift theflask and condenser and substitute a pan ofcold water for the heater. ) Titrate the sam-ple in the flask with standard ferric am-monium sulfate (0.15N) solution, using amagnetic stirrer if available. As the endpoint is approached (the Ti (HI) color getslight) add 5-ml of 20 percent ammoniumthiocyanate and continue the titration to theappearance of the red color.

At least 4 ml of 0.15 N Fe (III) solution

“%

should be required in back titration. If less,repeat adding more Ti (111) solution in exc-ess to the TNT–wax filtrate. (If less than4 ml of Fe (HI) solution is used in the backtitration in either standardization of Ti (III)solution or in the determination of TNT, lowvalues may be obtained. If the excess Ti (111)at the end of the refluxing is too small, re-duction of the nitro groups may be incom-plete. On the other hand, if more than 10-mlof Fe (III) solution is used, an unnecessarilylarge excess of Ti (HI) solution is beingadded.)

Run a blank on a volume of RDX saturatedbenzene equal to the volume of the aliquotof sample solution used in the precedingtitration.

Percent TNT =

(0.1261) (AN-BF) – (CN-DF) (100)

w

A = ml of Ti (111) solution

N = Normality of Ti (III) solution

B = ml of Fe (111) solution

F = Normality of Fe (HI) solution

C =‘ ml Ti (III) added to blank

D = ml Fe (III) added to blank 0.01261gm TNT = 1 meq. of TNT

W = Weight of samplealiquot

AN-BF = Meq. Ti (111)RDX

CN-DF = Meq~ Ti (111)

represented by

used by TNT &

used by RDX

4.4.3.3.4 Determination of, calcium chlo-ride. Calcium chloride. is determined as in4.4.3.2.4. ~ “‘,.

4.4.3.3.5 Determinutkn of wax -1- lecithin.The pw-centages of ~TNT, RDX plus nitro-cellulose, calcium chloride, and aluminum areadded and their sum subtracted from 100

Downloaded from http://www.everyspec.com

Page 9: everyspec.comeveryspec.com/MIL-SPECS/MIL-SPECS-MIL-E/download.php?... · MIL-E-22267A (d) Temperature The temperature shall be recorded, prior to, during, and after each phase of

pqrcent, The remainder is taken to be thepercentage of wax plus lecithin.”

4.4.3.4 Method of analysis. Grade B.

4.4.3.4.1 Determiruztion of hot melt—Vis-&llY. Weigh accurately a 1 gram sample ofHBX into. a tared sintered glass filteringcrucible, medium porosity, 30-ml capacity.Using approximately 5 ml of ethylene chlo-ride, divided into 5 equal portions, 1 minutecontact time each, extract sample ,on a Fisherfiltrator with water vacuum. Collect filtratein a 50-ml volumetric flask and dilute to themark, with &hylene chloride. Compare’ thecolor of the filtrate visually with previouslyprepared, standards to determine the weightof hot melt present. The preparation of thehot melt standard solutions are described in4.4.3.5.14.

Percentage of hot melt =‘ (A) “(1OO)

w

A = Weight of hot melt from compari-son with standards

W = Weight of sample

4.4.3.4.2 Determination of hot melt —Spectrophotometer. Compare the spectral

~absorbance at 20° C. of the ethylene chloridefiltrate obtained in 4.4.3.2.1 or 4.4.3.4.1 withthat of a standard solution (0.4 gram ofTNT/50 ml of ethylene chloride) at 430 mil-limicrons. The weight of hot melt is deter-mined by’ reference to a graph’ prepared inadvance from standard hot melt solutions.The preparation of the solutions and graphare described in 4.4.3.5.14. The TNT + wax.+ hot. melt filtrate collected in 4.4.3.3.1,diluted to 50 ml with RDX saturated benzenemay be substituted for the ethylene chloride— TNT solution obtained in 4.4.3.4.1. Allgraphs and standard solutions needed willsubstitute RDX saturated benzene for ethy-lene chloride.

Percentage of hot melt = (A) (100)( . ---- . . ... ,,, -,., ‘.. .,:,.. ..$,.

w-

MIL-E-22267A

A = Weight of hot melt obtained fromthe graph

W = ‘Weight 0$ sample

4.4.3.4.3 Determination of TNT — Spec-trophometer. Hot melt interferes with themethod for the absorbance of TNT as de-scribed in 4.4.3.2.2. Corrected TNT valuescan’ be obtained by comparing the TNT solu-tion “at 430 millimicrons in addition to 367millicrons. At 430 mu, the absorption is dueto the hot melt alone. Correct the weight forTNT obtained from TNT spectral absorbancegraph .by subtracting from it the value ob-tained from a correction graph prepared inadvance as described in 4.4.3.5.15. The TNT+ wax + hot melt filtrate collected in4.4.3.3.1, diluted to 50 ml with benzene satu-rated RDX may be”substituted for the ethy-lene chloride solution in 4.4.3.2.2. All graphsand standard solutions needed will substituteRDX saturated benzene for ethylene chlo-ride.

Percent TNT = (A - B) x 100

w

A = Weight of TNT from TNT spec-tral calibration graph

B = TNT correction value from theTNT correction graph

W = Weight of the sample

4.4.3.4.4 Deteminution of TNT — Titan-OU.Schloride method. Hot melt is present inthe TNT wax filtrate obtained in 4.4.3.3.1.This filtrate is used in the TNT determina-tion by the titanous chloride method. Hotmelt does not interfere with the TNT deter-mination.

4.4.3.4.5 Daterminutwn of aihuninwrn.Themethod described in 4.4.3,2.1 or 4.4.3.3.2 maybe used to determine the aluminum content.

,. ,., :, .4.4.3.4.6 Determination of RDX -?- nitro-

cellulose. The method described in 4.4.3.2.6o-r 4:4.3.3.1 may be use”d to.. determine theRDX + nitroceh.lose content.

‘ .9

Downloaded from http://www.everyspec.com

Page 10: everyspec.comeveryspec.com/MIL-SPECS/MIL-SPECS-MIL-E/download.php?... · MIL-E-22267A (d) Temperature The temperature shall be recorded, prior to, during, and after each phase of

MK-E-22267A

4.4.3.4.7 Determination of calcium. chlo-?-ide. The method described in 4.4.3.2.4 isused to determine the calcium chloride con-tent.

4.4.3.4.8 Determination of wax + lecithin.The percentages of TNT,’ RDX plus .nitro-cellulose, calcium chloride, aluminum, andhot melt are added and their sum subtractedfrom 100 peroent. The remainder is taken tobe the percentage of wax plus lecithin:

Where the method of analysis described in4.4.3.3 is not used in its entirety, the waxplus lecithin content can be determined asfollows :

The crucible plus residue obtained after theRDX saturated benzene extraction as de-scribed in 4.4.3.3.1 is extracted with. an ad-ditional 50 ml of RDX saturated benzene(5-10 ml portions, 30 seconds each.) Thesample is dried at 100° C. for 30 minutes.The crucible plus residue are cooled in adesiccator and weighed. The loss in weightof the sample is equal to the weight of theTNT + wax + hot melt extracted.

Percent wax -t- lecithin =

(A) — (B + C)

w

A = Loss in weight of sample afterRDX saturated benzene extrac-tion

W = Weight of sample

B = Weight TNT determined in4.4.3.2.2 or 4.4.3.3.3

C = Weight hot melt determined in4.4.3.4.1 or 4.4.3.4.2

The refractive index method for the deter-mination of ‘wax plus lecithin described in4.4.3.2.3 cannot be used when hotpresent.

4.4.3.5 Preparations of solutions,and standardization of solutions.

10

melt is

graphs

4.4.3.5.1 Preparation of TNT standardsolutions a,nd TNT spect?>al calibrationgraph. Prepare a stock TNT solution. Ac-curately weigh and transfer 8 grams of TNTinto a 500-ml volumetric flask. Dilute tomark with ethylene chloride.

Into each of seven — 50 ml volumetric flasks,‘pipette accurately the following quarkities ofthe TNT stock solution respectively, 22-ml,23-ml, 24-ml, 25-ml, 26-ml,’ 27-ml, 28-mLDilute with ethylene chloride to the mark.

Weight of TNT in each standard solu-,., tion = (A) (0.016)

A = Volume of TNT stock solutionadded to 50 ml volumetric flask

0.016 = Weight of TNT (gins) /ml ofTNT stock solution

Prepare the TNT spectral calibration graphby determining the absorbance at 367 muof the standard TNT solutions at 20° C.compared to a solution of 0.400 grams ofTNT/50 ml of ethylene chloride using 1 mmpath cells. Plot absorbance against weight ofTNT.

4.4.3.5.2 Preparation of wax standardsolutions and wax refractive index calibrat-ion graph. Prepare 3 gram HBX sampleswith different weights of wax and lecithin.The samples must be prepared with thesame materials used to prepare the HBXbeing analyzed. The weight of wax + leci-thin in the sample is based on the wax fromthe D–2 and Comp B (if used). The stand-ard wax samples are treated as described in4.4.3.2.3 to obtain the wax in solution.

Prepare” the wax refractive index calibrationgraph by determining the refractive indexof the various solutions of known wax con-centration tinder the same conditions de-scribed in 4.4.3.2.3. Plot the refractive indexreadings from the samples ,against weightof wax + lecithin.

4.4.3.5.3 Preparation of 0.1 M potassiumchromate solution. Accurately weigh 1.942grams of reagent grade potassium chromate

Downloaded from http://www.everyspec.com

Page 11: everyspec.comeveryspec.com/MIL-SPECS/MIL-SPECS-MIL-E/download.php?... · MIL-E-22267A (d) Temperature The temperature shall be recorded, prior to, during, and after each phase of

into a 100-ml volumetric flask. Dilute tomark with distilled water. Mix well.

4.4.3.5.4 Preparation of 0.1 N silver nitratesolution. Accurately weigh 16.989. gra~s Ofreagent grade silver nitrate into a liter volu-metric flask. Dilute; to mark with- distilledwater. It is not necessary to standardize thesilver nitrate solution if care is taken in thepreparation of the solution. Store the silver

‘nitrate solution in a dark place.,’

4.4.3.5.5 Preparation of l?DX ~atu~atecibenzene. To a gallon of reagent grade ben-zene, add RDX in excess of volubility, andstir for several hours. Let stand overnight.The solution should be prepared and kept atthe same temperature as will prevail at the‘time of filtering the extracted sample. Filtersolution just before” use.

4.4.3.5.6 Preparation of 20percent solutionof ammonium thiocyanate. Dissolve 60 gramsof reagent grade ammonium thiocyanate(NH,SCN) in 240-ml of distilled water.Filter until clear and store.

4.4.3.5.7 Preparation. of 6 N hydrochloricacid. Add 250-ml of reagent grade 38 percenthydrochloric acid to 250 ml of distilledwater. Mix well.

4.4.3.5.8 Preparation of 0.2 N titanouschioride solution. Mix 150-ml of 20 percenttitanous chloride solution with 100-ml of 38percent HC1 solution. (As the concentrationof the 20 percent titanous chloride variesfrom bottle to bottle, one may use an ad-justed volume for the preparation of addi-tional 0.2 N Ti (III) solution rather than the150-ml of 20 percent solution.) Dilute quan-titatively to 1 liter with distilled water. Mixby bubbling a stream of nitrogen or carbondioxide gas through the solution,” filterthrough. Whatman #41 (fluted) or equiv-alent paper, store in a system arranged sothat only COZ or N2 gas will be drawn intothe stock bottle as the solution is used.(Scientific Glass Apparatus Co. JB-7670,

lWIIrE-22267A

burette, automatic, for titanous chloridesolution, improved form; or J13-7615, bu-rette, automatic, or equivalent is satisfactory.Teflon stopcocks are to be preferred.)

4.4.3.5.9 Preparation of 0.15 N ferricammonium sulfate solution. Dissolve 75grams of hydrated ferric ammonium sulfate(FeNH1 (SO~) ~.12H20), reagent grade, in600-ml distilled yater. Add to this 25-ml of95 percent reagent grade sulfuric acid. Whendisolved, dilute with distilled water to 1liter; filter, mix thoroughly, and store.

‘4.4.3.5.10 Preparation of 0.200N p-nitro-aniline solution. Use p-nitroaniline with amelting point of 147-148° C., and recrystal-lize once from ethanol. Dry in a desiccator.For a 0.200 N soluticin weigh exactly 1.151grams of recrystallized p-nitroaniline, dis-solve in reagent grade glacial acetic acid,transfer to’ a 250-ml volumetric flask anddilute to the mark with glacial acetic acid.Mix well.

4.4.3.5.11 Compam”son of titanous chloride

and fem”c ammonium sulfate .golutions (de-termination of R). This value is necessaryin the determination of the normality of theTi (III) and the normality of the Fe (HI).R equals the ml of Ti (III) reacting with 1.00ml of Fe (III) solution.

Sweep the air from a 300-ml reduction flaskwith a current of nitrogen or carbon dioxidegas for 5 minutes. Continue to pass the cur-rent of nitrogen or” carbon dioxide gasthrough the flask until the titration is com-pleted.

Pipette 50.00 ml of approximately 0.15 NFe (111) solution into the air free reductionflask. Add 25 ml of 6N HC1 (use a cylinderto measure the HC1. ) Titrate with approxi-mately 0.2 N Ti (111) solution until near theend point (the Ti (III) color gets light.) Add5 ml of 20 percent ammonium thiocyanatesolution (by cylinder), and continue thetitration until the red color just disappears.

,,Repeat the procedure until two successive

11

Downloaded from http://www.everyspec.com

Page 12: everyspec.comeveryspec.com/MIL-SPECS/MIL-SPECS-MIL-E/download.php?... · MIL-E-22267A (d) Temperature The temperature shall be recorded, prior to, during, and after each phase of

MIL-E-22267A

I

I

values for R agree to within 1 part perthousand of their mean.

R=A—

B

A = ml of Ti (III) solutionB = ml of Fe (III) solution

4.4.3.5.12 Standardization of 0.2N titamOU-Schloride solution. Sweep the air from a300 ml reduction flask with a current ofnitrogen or carbon dioxide”gas f or 5 minutes.Continue to pass the current of gas throughthe flask until the titration is completed.

Pipette 20.00 ml of the 0.200 N p-nitroanilinesolution into the reduction flask. Pipette 25ml. of titan.ous chloride approximately 0.2 Ninto the same flask. Add 25 ml of 6 N HC1(by cylinder), and a few glass beads. Con-nect the reduction flask to a reflux condenserand boil for 15 minutes. Cool the flask toroom temperature without disconnecting thecondenser (lift the flask and condenser, re-move the heater, and let the flask down intoa pan of cold water.)

Titrate the excess Ti (111) with. Fe (III)solution. As the end point is approached,Ti (III) color gets light, add 5 ml of 20 per-cent ammonium thiocyanate (by cylinder),as an indicator and titrate to the appearanceof the red color.

Run a blank, substituting 20 ml of glacialacetic ‘acid for the p-nitroaniline solution..

Normality of Ti (III) solution =

4.000

‘ (A-RB) — (C-RD)

4.000 = Millequivalents of p-nitroanilinein 20.00 ml of 0.200 N solution

A = ml of Ti (III) solution

B = ml of Fe (III) solution

C = ml of Ti (111) in blank

D = ml of Fe (111) in blank

12

R = ml of Ti (111) qeacting with 1.00ml of Fe (-111) solution

The term (C-RD) should be zero. If thevalue lies outside the range + 0.10 and —0.10, either R is incorrect, or the acetic acidis contaminated. Repeat the determinationof” R. Continued high or low values for(C-RD) probably means impure acetic acid.

If normality of Ti (111) solution falls out-side of the range 0.19 — 0.22, add 20 per-cent titanous chloride solution or water asrequired. to bring normality to approximate-ly 0.2 N. Then repeat the determination ofR and repeat the determination of the nor-mality,

4.4.~.5.13 Determination of the normalityof the f em”c ammonium sulfate solution.Using the value of R and the value of thenormality of titanous chloride determined in4.4.3.5.11 and 4.4.3.5.12, calculate the nor-mality of the ferric ammonium sulfate solu-tion.

F = Normality of Fe (III) solution =(R) (N)

R = ml of Ti (III) solution reactingwith 1.00 ml of (Fe (III) solu-tion

N = Normality of Ti (III) solution

4.4.3.5.14 Preparation of tit melt stand-ard solutions and hot melt .spectraJ calib’r~tion graph. Prepare. a stock TNT solution byaccurately weighing and tran sf erring 8grams of TNT into a 500-ml volumetricflask. Dilute to mark with ethylene chloride.Prepare a stock hot melt solution using ma-terial conforming to Specification- MIL-C-3301. Accurately weigh and transfer 0.45grams. of hot melt into a beaker and dissolvein a 100 ml of ethylene chloride. Filter solu-tion through a sintered glass filtering cruci-

ble; medium porosity, .30-ml capacity untilfiltrate shows no sign of sedimentation..

To determine. weight of hot melt per ml offiltrate, accurately, pipette 15 ml of filtrate

Downloaded from http://www.everyspec.com

Page 13: everyspec.comeveryspec.com/MIL-SPECS/MIL-SPECS-MIL-E/download.php?... · MIL-E-22267A (d) Temperature The temperature shall be recorded, prior to, during, and after each phase of

into a tared evaporating dish with cover.Evaporate to dryness on a steam bath or hotplate below 75° C. Replace cover, cool ina desiccator to room temperature and weigh.

Weight of hot melt per ml of solution =

(A – B)

v

A = Weight of evaporating dish pluscover plus residue

B = Weight of evaporating dish pluscover

V = Volume of hot. melt filtrate pi-petted into evaporating dish

Into each of six — 50-ml volumetric flasks,pipette accurately 25 ml of the TNT stocksolution, add to each of the flasks respective-ly, by pipetting accurately, 0.5 ml, 1.0 ml,1.5 ml, 2.0 ml, 2.5 ml, 3.0 ml of the hot meltfiltrate. Dilute with ethylene chloride to themark.

Weight of hot melt in standard =(W) (D)

W = Weight of hot melt per ml ofsolution

D = ml of hot melt added to the st&d-ard

Prepare the hot melt spectral calibrationgraph by determining the absorbance at 430mu of the standard hot melt and TNT solu-tions at 20° C. compared to a solution of0.400 grams of TNT/50 ml of ethylene chlo-ride using 1 mm path cells. Plot absorbanceagainst weight of hot melt.

4.4.3.6.15 Preparation of the TNT correc-tion graph for the pretience of hot melt. De-termine the spectral absorbance of the hotmelt and TNT standard solutions at 367 mu,at 20° C., using 1 mm path cells. The pre-paration of the solutions is described in4.4.3.5.14. From this data determine the ap-parent weight of the TNT from the TNTspectral calibration graph described in

MIIFE-22267A

4.4.3.5.1. Subtract the actual weight of TNT(0.4 grams) in the standard hot melt sohl-tion from the apparent weight of TNT. Thisgives “the TNT correction value.

Determine the spectral absorbance of the hotmelt standard solutions at 430 mu as de-scribed in 4.4.3 .4.14..

For the TNT correction graph for the pres-ence of hot melt plot the absorbance of thestandard hot melt solutions at 430 muagainst the TNT correction values obtainedat 367 mu.

4.4.4 Moi&uve determination. Removesample of HBX from closed sample contain-er. Sample size shall be approximately 100grams for Grade A material and 50 gramsfor grade B material. Break up quickly andtransfer the sample to a tared liter Erlen-meym- flask with a ground glass neck. Stop-per flask and record weight of flask PIUSsample. (When sample is broken up, itshould be exposed to the air as little as pos-sible as the calcium chloride in the HBXquickly takes up moisture.)

To the flask containing the sample add 200ml of toluene and a magnetic stirring bar.Attach flask to a Bidwell-Sterling trap(graduated 5 ml in 0.1 ml.) To the top ofthe trap is attached a cold water condenser.(See Figure 1). (The use of Teflon sleeveson the ground glass joints in place of alubricant will facilitate the cleaning of theglassware.)

Heat the assembly on a magnetic stirrer hotplate, with agitation provided by the mag-netic stirrer. Heat to boiling. (The toluene-water azeotrope condenses and falls backinto the trap. Water being heavier, collectsin the trap and the excess toluene returns tothe boiling flask. ) Continue boiling until nochange in the water volume has been ob-served for 15 minutes. Boil a minimum of1 hour.

CAUTION: Keep solution well agitated atall times. When solution begins distilling,

13

Downloaded from http://www.everyspec.com

Page 14: everyspec.comeveryspec.com/MIL-SPECS/MIL-SPECS-MIL-E/download.php?... · MIL-E-22267A (d) Temperature The temperature shall be recorded, prior to, during, and after each phase of

MIIrE-22267A

position flask so that an air space is between A = ml of waterthe flask and hot plate. This is to prevent ahot spot from building up in the chunk ex-

B = ml’ of water in to]uene

plosive. Sample should not be left unattended C = Density of water at temperatureduring the moisture determination. Care of the water bathmust be taken that the coldwater condenser W = Weight of the sampleis operating properly at all times. If the con-denser should fail to trap ‘the toluene and 4.4.5 Vacuum stability test. 100° C.the flash were to boil dry, there could be apossibility of overheating the explosive. 4.4.5.1 Calibration of glass tube. Deter-

Care should be taken to prevent condensa-tion of atmospheric moisture in the con-denser. Five minutes before heating is dis-continued wash down the condenser withtohxme to remove any water clinging to thetip of the condenser.

After the moisture has been collected, trans-fer the trap to a constant temperature bathat 40° C. & 2° C. Allow about 30 minutesfor trap contents to reach the temperatureof the bath. By means of a wire loop workany droplets of water trapped along the sideto the bottom of the trap. Read the volumeof the water collected.

Run a blank on the toluene to determinewater present in the toluene. Calculate thepercentage of water in the sample.

Percentage of water =

mine the volume in mls of the 15.5 cm heat-ing tube by running in mercury from aburet until the tube is filled to the level atwhich the ground glass joint of the capil-lary tube will make contact with the mer-cury. Subtract from the indicated buretreading, the volume of explosive used in thetest. The difference shall be represented bythe symbol A. Transfer 7.0 ml of mercuryto the cup at the lower end of the capillarytube. Clamp the tube in an upright verticalposition, and measure the height in mm ofthe mercury column in the capillary tube(approximately 25 mm.) Measure the lengthin mm of each of the 3 parts of the capil-lary tube and add these values to obtaintotal length. From the total length subtractthe height of the mercury column in thecapillary tube as previously obtained. Rep-resent this difference by the symbol B1.From the total length subtract the height of

(A — B) (.C) (100) the column of mercury in the capillary tubemeasured at the end of the test described in

w 4.4.5.1.

i

I 14

Downloaded from http://www.everyspec.com

Page 15: everyspec.comeveryspec.com/MIL-SPECS/MIL-SPECS-MIL-E/download.php?... · MIL-E-22267A (d) Temperature The temperature shall be recorded, prior to, during, and after each phase of

MIIrE-22267A

\

=—————-.—

———

-.

z

BIDWELL-STERLING DISTILLINGGRADUATED 5 ML.

WI

-&L ,,“,~

T p ~\”I

‘~“‘“v ‘ “““,,,,

1.1’11

IIq

~

JACKXT LENGTH - 300 MM=

\

.

Ii r

FIGURE 1. Moi&ure content appara tms

TPJ9.P. ..

Downloaded from http://www.everyspec.com

Page 16: everyspec.comeveryspec.com/MIL-SPECS/MIL-SPECS-MIL-E/download.php?... · MIL-E-22267A (d) Temperature The temperature shall be recorded, prior to, during, and after each phase of

IW.AI-22267A

Represent this difference by the syn@ol B.Determine the capacity of the capillary tubeper unit of length as follows: Transfer anaccurately weighed sample, of approximately10 gm. of mercury. to the cup at the lowerend of the capillary tube. Manipulate thetube so that when it is horizontal, mercuryis contained in a continuous section of thelongest part of the tube and measure thelength of the mercury column. Repeat thistwice with the mercury in 2 other parts ofthe long section of the tube. Calculate theaverage of the ‘3 measured lengths of themercury column. Represent the unit capaci-ty in ml per mm of the capillary tubing bythe symbol C. This can be obtained from theformula:

C=w

—’

c=

w=

.D =

L=

DL

Unit capacity of capillary tubingin ml per mm

Grams of mercury

Density” of mercury at tempera-ture of determination

Average measured Iengths of mer-cury column in mm

4.4.5.2 Test procedure. Transfer a 1 gramsample, dried at 65° C. for 2 hours, to theheating tube of the apparatus shown inFieare 2. Connect the capillary tube to theheating tube. Clamp the apparatus so thatthe long section of the capillary tube is in a

nearly vertical position. Transfer 7.0 ml ofmercury to the cup at the lower end of thecapillary tube. Connect a vacuum pump tothe lower end of the capillary tube andevacuate the system until the pressure isreduced to approximately 5 mm of mer-cury. (Evaluation of the capillary tubeis facilitated by placing the cup of thetube in a horizontal position so that mer-cury does not block the capillary open-ing. ) After evacuation, disconnect the pump.Seal the connection between the capillarytube and the heating tube with 1 ml of mer-cury. Measure the total vertical height ofthe column of mercury in the capillary tube.Measure and subtract the vertical height ofthe mercury in the cup. The difference shallbe represented by the symbol H1. Note theroom temperature (t 1) and the baromet-ric press~e. Subtract the value HI fromthe barometric pressure in mm. Representthis difference by the i~bol P1. Insertthe heating tube in a constant tempera-ture bath consisting of a solution ofglycerin and water (specific gravity 1.05).Maintain at a temperature of 100.OOC. &0.5° C. for 48 hours. Remove the heatingtube from the bath and allow to cool to roomtemperature. Measure the total verticalheight of the column of mercury in the cap-illary tube and subtract the vertical heightof the mercury in the cup. This differenceshall be represented by’ the symbol H. Notethe room temperature (t) and the barometricpressure in mm. Represent this differenceby the symbol P.

Downloaded from http://www.everyspec.com

Page 17: everyspec.comeveryspec.com/MIL-SPECS/MIL-SPECS-MIL-E/download.php?... · MIL-E-22267A (d) Temperature The temperature shall be recorded, prior to, during, and after each phase of

MWE-22267A .f

2.8 CM~

p-=i

26 OR 13 CM

1’15.5 m

,. ..,:.

.-

“!I

I ~~

$ vJ .-_._ .._—-.!

,., , ..—*

I

$J

IIFATING TU13E

1-’-1.5 (31

STGPPEI{ TO BE STANDARD TAPER’ 12/18,...

.,?, .,

8

CAPILLARY TUBING

6 TO 6.5 MM EXTERNAL DIA..

1 1.O.TO 2.OMM INTERNAL DIA

I

I

)

i.

,, FIGURE 2. Apparatus for 100° C vacuum stability test

,“,’ .”.:. ,“”’. ”,.,.

.7.

..’” .::!.

17

Downloaded from http://www.everyspec.com

Page 18: everyspec.comeveryspec.com/MIL-SPECS/MIL-SPECS-MIL-E/download.php?... · MIL-E-22267A (d) Temperature The temperature shall be recorded, prior to, during, and after each phase of

MIIi-E-22267A

4.4.5.3 Calcx.dation of liberated gas vol- described in 4.4.5.2, using the values de-ume. Calculate the volume of gas in ml, at scribed by the symbols in 4.4.5.2 and 4.4.5.1standard conditions, liberated in the test in the following formula:

[A + C(B-H)] 273 P [A + C(B1 — HI)] 273 PIv=

760(273 + t)

4.4.6Test equipment. The following itemsof test equipment are required to performthe Acceptance Tests set forth in this speci-fication: ,

5.

Moisture Apparatus Figure 1

Vacuum Stability Apparatus Figure 2

Standard Testing Sieves — top plate

bottom plate — Federal SpecificationRR-s-366

Balance — Accuracy & 0.1 mg.

PREPARATION FOR DELIVERY

5.1 Application. The packaging, packing,

and marking requirements specified herein

apply only to preproduction samples sub-

mitted to a government laboratory.

5.2 Packaging.

5.2.1 Level c. Unless otherwise specified,

the sample shall be packaged in moisture-

proof containers.

5.3 Packing.

5.3.1 ~evel C’. The preproduction sample

shall be packed in a manner as to coxnply in

all respects with Interstate Commerce Com-

mission regulations for transportation of

explosives and other dangerous articles.

5.4 Marking.

5.4.1 Special marlhkg. Marking of exteriorcontainers shall be in accordance with theCode of Federal Regulations, 49CFR 71-90.In addition, each container shall be marked

18

760 (273 + tl)

in accordance with applicable documents.

5.4.2 Normal marking. In addition to themarking required by contract or order, unitpackages and shipping containers shall be,marked in accordance with the requirementsof Standard MIL-STD-129 including ex-plosive lot number and date of manufacture.

6. NOTES

6.1 Intended use. The HBX type explosive

compositions are intend’ed for use in ammu-

nition.

6.2 Ordering data. Procurement documents

should specify the following:

a.

b.

c.

d.

e.

f.

$?.

h.

i.

Title, number and date of this speci-fication

Applicable drawings and other docu-ments

Grade of HBX type compositions(see 1.2)

Required form, buds, strips or other-wise (see 3.2)

Size of preproduction sample inpounds, and required form (see4.3.1)

Whether a calcium chloride deter-mination is required

Laboratory responsible for conduct-ing tests on preproduction samples

Specific provisions for delivery andtesting of preproduction samplesprior to production of the item

Specific provisions in the contract

Downloaded from http://www.everyspec.com

Page 19: everyspec.comeveryspec.com/MIL-SPECS/MIL-SPECS-MIL-E/download.php?... · MIL-E-22267A (d) Temperature The temperature shall be recorded, prior to, during, and after each phase of

or order when Calciu”rnSilicate isrequired in the formulation of.-HBX compositions (see 3.5)

j.: Specific provisions for acceptance in-,- spection by either. Government

agency or contractor. ; -. ..” . .. . .:

6.3 General safety precautions. The ‘pre-paration and handling of the items coveredby this specification; and the subassembliesthereof, involve hazardous operations andtherefore require. explosives+:safety -precau-tions. Use of this specification,- will not-beconstrued as to. relieve the...cont~,actor .ormanufacturer of responsibil.ity for the: safe-ty of his operations. Listed. below are-certainminimum provisions which a contractor. .ormanufacturer (who prepares the item cover-,.ed) should observe in order to ‘fulfill hisresponsibility for safety. -At-Bureau of -Naval‘Weapong~ Navy” Department, and other gov--ernment’ plants, these provisions are.’ mand-atory. Such other warnings ,and,. preeau-,tions, pertinent to the operational effective-ness or safety “during ‘preparation of. thespecified items, are in-eluded in detailed ‘tech-nical requirements of the specification.- ; :

6.3.1 All handling and batching operationsshould be conducted in. a neat and orderlymanner. ,. :----

6.3.2 Safd ‘equipment and methods shouldreutilized for transporting. and handling ex-plosives components and mixtures. Whererequired, remote controlled barricaded hand-ling equipment shall be used for explosivesoperations, such ,as mixing, pouring, weigh-ing, charging, sifting,. drying, casting, etc.

6.3.3 The” exposure of explosive materialsand related parts should be so controlled asto minimize the absorption of moisture fromthe atmosphere or other sources duringhandling and batching operations.

6.3.4 All explosive components and mix-tures should be stored in suitable storagemagazines located .in accordance with. Amer-

.. .. -.:...’.

MILE-22267AI

ican Table of Distances, (ATD) or other ap- ‘pljcable safety standards; and while in ‘ ~.piocess, in safety lockers and chests if in“loading rooms, or in “adequate ready or serv-“ice magazines located in accordance with“Intraplant distances when outside “of loading“rooms, For Navy managed explosive loadingplants, the provisions of the Armed ServicesExplosives Safety Board covering quantity-distance relations for explosives will apply.

~, 6.3.5 ‘Proper care must be exercised at all~times-to protect personnel from accidents,fires; or explosions, and to limit damage toequipment and loading areas; In this connec-.tionj the precautionary measures in the fol-lowing paragraphs should be observed.

,,. .

6;3.5.1 Employ, properly proportioned andproperly located protective barricades,screens or shields at all required points.

6.3.5.2 Keep only minimum limited quanti-ties of explosives components and explosivemixtures’ at each stage of operations.

6.3.5.3 Keep explosives and explosive corn-ponents in approved covered receptacles withcovers in place when material is not beingtaken out of or put into the receptacles.Where necessary, receptacles should be con-ductive to ground electrostatic charges.

6.3.5:4 Protect operations from electrosta-tic charges by effectively grounding all ma-chinery, equipment and fixtures; and, wherenecessary, employ suitable grounded conduc- ~tive coverings for floors, work benches andtables, and workers’ conductive shoes. Work-ers’ clothing of a type to minimize the ac-cumulation of static charges should be em-ployed. Fabrics such as silk and nylon, whichpromote static generation should be avoided.Additional precautions should include me-chanical shielding to contain fragments andblast, also electrical shielding from inducedelectric currents generated by sources suchas lightning, static, radiations from commu-nications apparatus, radar, or high frequen-

19

Downloaded from http://www.everyspec.com

Page 20: everyspec.comeveryspec.com/MIL-SPECS/MIL-SPECS-MIL-E/download.php?... · MIL-E-22267A (d) Temperature The temperature shall be recorded, prior to, during, and after each phase of

lWIIi-E-22267A

cy heat apparatus, etc. Additional ground-ing devices such as grounding bracelets forworkers should be employed where opera-tions are conducted with items which areunusually sensitive to initiation by staticelectricity. Where necessary for safety, hu-midity of work rooms should be appropriate-ly increased, as required, to lessen electro-static effects but without inducing excessivemoisture absorption by any of the compo-nents.

6.3.5.5 Protect all explosive operationsfrom effects of electric current originatingfrom equipment such as soldering irons,heaters, switches, wiring, motors, lights,test instruments, etc., by suitable insulation,grounding, separation or shielding. Suchelectric sources may initiate explosives byheat, sparks, arcs. Circuits may be inadver-tently ,completed, for example: from a de-fective soldering iron through a groundedcontact.

6.3.5.6 Enforce, where necessary, thewearing of suitable safety footwear, gloves,goggles, respirators, and impregnated gar-ments to protect personnel against burns,poisoning, and associated industrial hazards.

6.3.5.7 Allow no fires or exposed electricalor other sparking equipment, and little orno flammable material to be present in load-ing; handling and storage spaces. Enforceproper “Match”where necessary.

20

and “No Smoking” rules

6.3.5.8 Enforce good housekeeping andmaintain effective policing, inspection andsupervisory methods throughout the loadingarea and surroundings. Employ effective

.“cleaning methods periodically to minimizethe accumulation of explosives and explosivesdust and other contaminants upon, and as-sure its removal from floors, walls, ceilings,ledges, tables, benches, piping and equip-ment or the item loaded; also, clean up anyspilled material immediately:

6.4 Manufacture by government activities.When the HBX type explosive compositionsare to be prepared in accordance with thisspecification by government activities, therequirements given herein for bidders andcontractors shall apply to such governmentactivities.

Notice. When Government drawings, specifications,or otherdataare usedfor any purposeotherthaninconnectionwitha definitelyrelatedGovernmentpro-curementoperation,the UnitedStates Governmenttherebyincursno responsibilitynor any obligation“whatsoever;and the fact that the Governmentmayhave formulated,furnished,or in any way suppliedthe said drawings,specifications,or other data isnot to be r,egardedby implicationor otherwiseas inany mannerlicensingthe holderor any otherpersonor corporation,or conveyingany rights or permis-sion to manufacture;use, or sell any patentedinventionthat may in any way be relatedthereto.

Custodians: Preparing activity:Army—MU Navy—WepNavy—WepAir Force-OOA (Project 1375-0332)

1—— -L.—— — .— ,

Downloaded from http://www.everyspec.com


Recommended