mibs-51132a (kj) military specification

MIbS-51132A (KJ)~

RIGS-51132 (MU)27 January 1964 ,

MILITARY SPECIFICATION

Smnm WwmmmYL cELLmmE(Pm AMMUNITION USE)

(NaCMC)

1. SCOPE

1.1 This specification covers the mlnlmum requ~nts forsodium carboxymethyl cellulose (NaCMC) as the granulating agent Inthe manufacture of lead azitle.

2. APPIJCABLE D~

2.1 The following documents of the issue In effect on date ofinvitation for bids or requests for proposal form a part of thisspecification to the extent specified herein.

SPECIFICATXXW

FEDERAL

PPP-D-723 -PPP-D-729 -

MILITARY

MIL9P-112 -

MILX-45208

STANDARM

MiLITARY

MIL-STD-105

MIIA7I!D-109MIIFSTD-129

Drums$ FiberDruma8 Metal, 55 Gallon (for shipment ofnoncorrosive material)

PackagXn.gand Packing for Overseas ShipmentDrums$ Plywood (for drums whose we ht of

7contents does not exceed 200 poundsInspection Requirements; GeneralSpeclficatlon for.

Sampling Procedures and Tables forInspection by Attributes (ABC-S_lOS)Quality Assurance Terms and Definitions.I&rki@ for Shipment and Storage.

MIIAYTD-1235 - Single and Multilevel Continuous SamplingProcedures and Tables for Inspection byAttributes.

-

I

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MILS-51132A (MU)

(Copies of speclficatfons, standards, drawings and publicationsrequired by suppliers In connection with specific procurementfunctions should be obtained from the procuring activity or asdirected by the contracting officer. )

2.2 Other publications.-The following documents form a partof this specification to the extent specified herein. Unlessotherwise indicated, the Issue in effect on date of invitationfor bids shall apply.

American Society for Testing and Materials (ASTM) -ASTM StandardsASTM-D-1439-64T, “Tentative Methods of Testing Sodium

Carboxymethylcellulose”(Copies may be purchased directly from ASTM, 1916 RaceStreet, Philadelphia 3, Pa.)

UNIFORM FREIGHT CLASSIFICATION PUBLICATION(Application for copies of these freight classificationrules should be addressed to the ConsolidatedClassification Committee, 202 Chicago Union Station,Chicago 6, 111.)

AMERZCAN TRUCKING ASSOCIATION PUBLICATIONNational Motor Freight Classification Rules and ContainerSpecifications. -

(Application for copies should be addressed to the AmericanTrucking Association, 1424 16th Street N.W., Washington, D.C.)

3. REQUIREMENTS

3.1 Material.-The material used in the manufacture of sodiumcarboxymethyl cellulose shall be such as to produce a finishedproduct conforming to the requirements stated in Table I whendetermined as specified in the applicable paragraphs of section 4.3.

Table I

Color and form.-Whlte to cream colored powder free fromgritty particles, vlslble Impurities and foreign matter whentested as specified In 4.3.1.

Moisture .-10.0 percent maximum (max.) when tested as speclfledin 4.3.2. -

viscosity.-A 2 percent solution at 25 degrees C. - 300centipoises (cps.) mfnlmum (min.) and 750 CPS. max. whentested as specified fn 4.3.3.

sodium chloride.-4.O percent max. when tested as specifiedIn 4.3.4.

Sulfated Ash.-2O percent max. when tested as sPeclfled in4.3.5.

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KIL-S-51132A (Mu)

Insoluble Matter.-lO percent max. when tested as specified in4.3.6.

pH Value.- 6 min. and 8 max. when tested as specified in 4.3.7.Degree of Etherlflcation (D.E. ).-O.45 min. and 0.63 max. when

tested as specified in 4.3.8.Purity.- 90.0 percent min. when tested as specified in 4.3.9.

3.2 Worlananshfp.-Aclds shall not be used to alter the pHvalue of the sodium carboxymethyl cellulose (NaCMC).

4. QUALITY ASSURANCE PROVISIONS

4.1 General quality assurance provisions.-Unless otherwisespecified in the contract or purchase order, the suppller isresponsible for the performance of all inspection requirements asspecified herein. Except as otherwise specified, the supplier mayutilize his own facilities or any commercial laboratory acceptableto the Government. The Government reserves the right to performany of the Inspections set forth In the specification where suchInspections are deemed necessary to assure supplies and servicesconform to prescribed requirements. Reference shall be made toStandard MIL-STD-109 in order to define terms used herein. Theprovisions of Specification MIL-A-2550 shall apply.

4.1.1 Contractor inspection system.-The contractorstiall provide and maintain an effective inspection system incompliance with the requirements of specification MIL-I-45208.If due to the nature of the manufacturing process, the contractordesires to utilize a quallty assurance system which Is at variancewith the quality assurance provisions o? Specification MILI-45208and other documents referenced herein, he shall submft a writtendescription of the system to the contracting officer for approvalprior to initiation of production. It shall Include a descriptioncovering controls for lot formation and Identification, inspectionsto be performed, inspection statfons, sampling rocedures, methods

7of inspection, (measurfnq and testing equipment and provislonsforcontrol and disposition or non-conforming material. The writtendescription will be considered acceptable when, as a minimum, Itprovides the quallty assurance provisions required by the provisionsof 4.2 and 4.3 and the other dGcUmentS referenced herein. Thecontractor shall not be restricted to the Inspection station orthe method of Inspection listed In this specification provided thatan equivalent control is Included In the approved quality assuranceprocedure. In cases o? dispute as to whether certain procedures ofthe contractors system provide equal assurance, the comparableDrocedure of this speclflcatlon shall apply. The contractor shall;otlfy the Governmentthe written procedureby this spec:flcatlon

of, and obtain approval for, any changes tothat effects the degree of assurance requiredor other documents referenced herein.

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MII#j-51132A (MU)

4.1.2 Submission of product .-At the time the completed lotof product Is submitted to the Government for acceptance, thecontractor shall supply the followtng Infomatlon accompanied bya certificate which attests that the in!’ormatlonprovided fscorrect and applicable to the product submitted:

a. A statement that the lot compltes w%th all qualltyasswance provisions of the approved current written descriptionof the system.

b. Number of units of product inspected.c. Results obtained for all inspection performed.d. Speclflcatlon number and date, together with an

identlflcatlon and date of changes.e. CeFtiflcat@s of analysis on all material procured

dtrectly by the contractor when such material Is controlled byClov$nnment specifications listed in any of the contractual documents.

f. Number of batches In the lot.Date submitted.

The cert&Zcate shall be signed by a responsible agent of thecertifying organization. TM initial certificate submitted shallbe substantiated by evidence of the agent?s authority to bind hlsprincipal. Substantiation of the agentss authority will not berequired wtth subsequent certificates unless, during the course of’the contract, this authority is vested in another agent of thecertifying organization.

4.1.3 Government verification.-Using the contractor~s writtenquality assurance procedure$ this detail specifications theapplicable drawings and other contractual documents as a mldesthe Gwernment inspector shall verify at unscheduled Intervalsall qua2Sty assurance operat~ons perfomned by the contractor.Verification will be In accordance with Speciflcatlon MIGI-45208and will be performed to the extent necessary to assure compliancewith the contractual requirements. Severity of Governmentinspection of Individual characteristics w121 be directly relatedto the seriousness of the classification assigned. In no instwcewill a characteristic classified ‘Scrltlcal”be accepted solely onthe basis of contractor’s records.

4.2 Inspection provisions

4.2.1 Lot formation.-A lot shall consist of one or more batchesof sodium carboxymethyl cellulose, produced by one manufacturer, inaccordance with the same speclflcatlon$ or same specification revision,under one continuous set of operating conditions. Each batch shall

consist of that quantity of sodium carboxymethyl cellulose that hasbeen subjacted to the same unit chemical or physical process

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NIL-S-51132A (MU)

intended to make the final product homogeneous. The product shallbe submitted for inspection in accordance with Standard MILAYI’D-105(or Standard MIL-STD-1235 when applicable).

4.2.2 Examination.-Sampling plans and procedures for thefollowing classification of defects shall be in accordance withStandard MIL-STD-105. Continuous sampllng plans, in accordancewith Standard MIG=STD-1235 may be used If approved by the procuringactivity. Also, at the option of the procuring activity, AQLJSand sampling plans may be applied to the Individual characteristicsllsted using an AQL of 0.25 percent for each mijor defect and anAQL of 0.40 percent for each minor defect.

4.2.2.1 Drums, prtor to filling (Polyethylene llner).

Categories Defects Method of Code No.Inspection (see 6.3)

Crlttcal: None defined.

Major : AQL 0.25 percent101. Liner Cut$ torn or punctured..Visual

Minor: None defined.

4.2.2.1.1 Drums~ prior to filling (alternative

Critical: None defined.

Major: AQL 0.25 percent101. laminations or coatings

incomplete....................VISW1


01001

method).

4.2.2.2 Drums, prior to closing (Polyethylene liner)

Categories Defects Method ofInspectIon


Major: AQL 0.25 percent101. Liner not completely sealed...Vlsual


01002

Code No.

02001

5

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4.2.2.3

(m)

Drum, sealed (steel)

Method Of Code No.Inspection

Categories Defects

Crit$cal: None deftned

Major:101 ● Closing ring damaged or not

Prop8rly po~ittoned EUOit doesnot close drum Properly..c..lrlsualal

Minor: AQL 0.40 percent201. Flarklngmisleading or

unidentifiableeo..............maml

4.2.2.4 Drum, sealed (ftber)

Categories Defects Method ofInapeotlon

Crltlcal: None deftned

Major: AQL 0.25 percent101* Weight of contentsO.........o.Scale102. Closure incomplete or damaged

to the extent that contentssift out......................vlsual

Minor: AQL 0.40 percent201● Markings misleading or

unidentifiable................Visual

4.2.2.5 Drum, sealed (plyuood)

Categories Defects Method ofInspection


14aJor: AQL 0.25 percent.101 ● Weight of contents ............Scale102 ● Strapping missing or broken...Visual

03001

03002

Code No.

04001

04002

04003

Code No.

0500105002

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MIL-S-51132A (MU)

Minor: AQL 1.0 percent201. Strapping mi;.located..........Visual 05003202. Marking misleading or

unidentifiable................Visual 05004

4.2.3 Determination of color and form, moisture, viscosity,sodium chloride, sulfated ash, insoluble matter, pH value, degreeof Etherification and purity (see 3.1 and 4.3.1 to 4.3.9) Major defect.

4.2.3.1 Testing

4.2.3.2 Sampling by lot.-A random representative sample ofapproximately three ounces from each of 10 containers shall beselected from each lot. When lots are comprised of 10 containersor less, each container shall be sampled to form a 30 ouncecomposite sample.

4.2.3.2.1 Preparation of composite.-Approximately three ounce.samples of sodium carboxymethyl cellulose shall be removed fromeach container:of-theten containers In order to obtain a thirtyounce sample..-If thereare less,than 10 containers, equal -.primary”samples in sufficient quantity to.totalthtrty-ounces, shallbe removed fromeach container. The individual primary samplesshall then be combined In order to form a homogeneous composite sampleof thirty ounces and subjected to the tests spectfied,tn 4.3. Ifthe composite sample falls M comply with any of the requirements

%/’ specified, the lot shall be rejected on a major defect basis.

4.3 Test methods and procedures

4.3.1 Color and physical form.-Code Number 06001.-Determlnethe color and physical form by visual examination.

4.3.2 Moisture content.-Code Number 07001

4.3.2.1 Determine the moisture content in accordance with themethod described In ASTM-D-1439-64T.(NOTE: Save this sample for the determination described in4.3.5. Do not use this sample for any other determinations listedbelow) ●

4.3.3 Viscosity.-Code Number 08001

4.3.3.1 Determine the viscosity tn accordance with the methoddescribed in ASTM-D-1439-64T.

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MILMS-51U!RA (Ml?)

4.!5.4 Sodiu5 chloride contentO-Code Niaib3r0$001

$.3.4,1 Dotermlne the sodtum chloride eontrmt in accordancewith the m@4MxA deecrlbed tn ASTWD-1439-64T.

4.3.S Sulfated Ash.-Coda Nwnber 10001

403.5.1 Ap_tua

Poredain (Ignttion) crucibleHotplateMuffl@ FlaFrlaceK#es2ec8tor

4.3.5.2 neagcwlts

Nltrle Acids 70 percent$ A.C.S. gradeSulfuric Acids 95 percent$ A.C.S. -e

4.3.5A Acm.arately wel~t a 3 to !5@m. ~le of the driedmaterial obtat.ned fr~ 4.3.2 into a tared pormlsh (tgnition)cructblo. Plato orwlble and content= into a fharnace maintainedat 600 degrees plw or mlnue 50 degrees C. f’er1S zttnutos. Removefrom fuxTMN2eIand Ceole Add 2 ml, Or concentrated auli%r%c ac%d&and5 drops of 70 percent nitric acid to the crucible. place crucibleand contents en a hot plate until acid 10 oomplotely evaporated.Rmmove crnac$ble~ hot plate and again place in fumaca maintainedat 600 degrees plus or minus 50 degrees C. Allow to remain In furnacefor 1 hour. Remove fro@Bfurnace, cool in a ~estccator and we%gh.Calculate the sulfated af4hcontent as follows;

Percent Sulf’atedAsh IEIA X MM

Where:A D we-t of’ashB ~ gins.of spaclmen

4.3.6 Dsoluble miatter.-CodeNumber 2101.

4.3.6.1 Ap~atu8

8 oz. @crew-top @ra to fit in cmtrlfugeCmtrifuge - International Size 1, Type C or equivalent.


.,

,’--

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.,.,,..

NIL-S-51132A (MU)

4.3*6.2 Procedure

Transfer a A gram sample of the NaCMC weighed to thenearest milligram to an 8 oz. bottle and add 200 ml. of distilledwater~ Mark the bettle with a crayon at the liquid level. Stirthe m$xture with a mechanical stirrer until the sample 1s completelydlepersed (usually about Xl minutes). Put the screw cap on thebottle and centrifuge for 30 minutes at 1500 rpm. Siphon off asmuch as possible of the aupernatant liquid without disturbing thesediment. Add water to the marks oap the bottles and shakevlgorlously to d%sperae the insoluble titer. Centrifuge again for30 minutes ●t 1500 rpm. Proceed as before until the sample hasbeen centrifuged four times. After the rinl centrifugatlon andremoval of supernatant liquid~ transfer quantitatively theinsoluble ~tter t+aa tared evaporating dish with the aid of adistilled water wash bottle. Evamrate most of the water on asteam bath and theC. plus or mlnua 2

,-.,... ... ..:,-,Caklate the‘,..,:,.:

Percent water

weight ofweight of

re~%due in an &en to constant weight at 100 degreesdegrees C, Cool

l.nsohible,matter..

lnsoiub26’&tter

dry restduesample

and weigh. -

as follows:

percent moisthe found in sample (4.3.2)

4.3.7 pl!value. -Code Nmber 12001.-In ● 100 ml. beakerdissolve a 1 gm. specimen of NaCMC (dry basis) In 100 ml. ofdistilled water. Determine the pl!at room temperature using anA. Beckman PH meter, or an approved equal.

4,3.8 D.E., - Code Number 13001

4.3.8.1 AppIPatMa. Mechanical pulverizer - Micro pulverlzer$ Type CF,

manufactured by Pulverizing Machine Co~ Sumnlt, N.J. or FllzwlllModel JT manufactured by W. J. Fltzpatrtck Co, Chicago, 111.have been found satisfactory.

b. Ah drive stirring apparatus.-A. ?!. Thomas CatalogueNumber 9224, wtth glass propeller has been found satisfactory.

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NIIeS-51132A (MU)

4.3.8.2 ReagentsDiphenylamine reagent - dissolve 0.5 gm. diphenylamlne

in 120 tia: 85 percent sulfuric acid.b. 0.5 Molar nitric acid - 26 ml. concentrated nitric

acid made up to a liter with distilled water.c. 95.0 percent ethyl alcohol.

4.3.8.3 Grinding.-Grind the spedmen on a mechanical@mrtzer so that it passes through a 10 mesh sieve.

4.3.8.4 Frocedure..To a 250 ml. beaker containing 100 ml.of 95 percent ethyl alcohol$ add 5 gm. of the NaCMC and agttatewtth a mechanical stirrer. Add slowly to the slurry~ while stirring,45 ml. distilled water and continue to stir for at least 5 minutes.Allow the solids to settle and decant the supernatant liquld.Add 100 ml. of 95 percent et.tiylalcohol and slurry for about 2mtnutese Allow the solids to settle and decant the supernatantliquid. Add 100 ml. of 95 percent ethyl alcohol and, whilestlrl?lng~add 5 ml. concentrated nitric acid and continue agitationfor 2 minutes, Heat and slurry on a steam bath and bogl for 5 m%nutes,remove and agitate again for at least 10 minutes. When the stirringis complete, filter through a Buchner”funnel (No. 1 Whatman filterpaper). Decant all the liquid through the funnel and draw.filtercake dry. Break up the filter cake thoroughly wtth the ald of ana~ber-policeman$ and slurry in the funnel with 50 ml. of 0.5 B!nitrtc acid. Drain and slurry agatn with 50 ml. of 0.5 M nitricac3d and drain, Wash the filter cake with distilled water untila portion of the filter cake$ treated with 4 to 5 drops ofdlphenylsmine reagent. en the spot plat.e9 does not produce a bluecolor. About 4 or 5 washings should suffice to give a negativetest for nitrates. Draw dry and fluff up the cake with a rubber-policeman. Slurry the cake in the funnel twice with 50 ml. portionsof acetone. Fluff up and draw M@ through the funnel for 2 to 3minutes. Transfer the cake to a we% hing dish and dry in an oven

7maintained at 105 degrees C. f’or1 1 2 hours. COO1 in a desiccator.Place an accurately weighed portion cf approx~tely 1 gm. of thedried CMC cake in a 4CX2ml. beaker. Add 100 ml. of distilledwater and 25 ml. of standard N/3 sodium hydroxide} from a burette.Cover the beaker with a watch glass, heat to boiling on a hotplate and boil gently until completely dissolved (10-15 minutes1s usually sufftcien~.). Back titrate with standard N/3 hydrochloricacid to a phenolphthalein end pgfnt. Apply burette and temperaturecorrections. Calcula8.e the D.’E. as follows:

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-.

MIL-s-51132A (JK7)

Equation 1 - Calculation of Factor PI

~*(A’B)- (CD1u

Where:A _ ml. @ sod~um hydroxide ~~e~.B = normality of sod2um hydroxidec = ml. of hydrochloric acid WedD = normallty of h:nlrochloricacidw =-. of dried C~~Ccake wed

Equation 2 - Calculation for detemlnatioc of D.E.

DOE. = 0.162 M● OS8M

(NOTE: This is the D.E. value which should meet the require-nt ).

where:M = value obtained

4.3.9 Pur3ty-Code

4.3.9.1 Determinethe method deacrtbed in

. .

In Equation 1..

Number 14001

the purity of’the NaCMC ti.”accordancewithASTM-D-1439-64T.

5. PREPARATI(34FOR DELIvERY

5.1 Packi~

5.1.1 Drums.-Unleas otherwise specified in the contract orPurchase order, sodium carboxymethyl cellulose shall be packed tnnon-returnable fibers plywood or metal drum in accordance withSpeclflcatlon PPP-D-=723(Type 111, Grade A), MIL-P-112, andPPP-D-729 (Type III, pull Removable Head Type), respectively.Fiber and plywood dmms shall be furnished with a nominal 0.004inch thick polyethylene llner$ properly heat sealed or otherwiseclosed to affoti protection to the contents equivalent to thatgiven by a heat seal closure. (Alternately, an equivalent degreeof protection may be furnished by suitable laminations or coatingsof the Inner surface of the drum.) The drum shall be closed Inaccordance with Specifications PPP-D-723, PPP-D-729 and lJIIbP-112as applicable.

11


MIIA5-51132A (“&)

5.1.1.2 Level C.-sodium carboxymethyl cellulose shall bepacked to af’f’ordprotection against d-e during direct shipmentfrom supply source to the firs~ receiving ac:ivity for inmediateuse. Containers shall ccmply w~th Uniform Freight ClassificationRules and Container Spec%fieations for rail shipments or NationalMotor Freight Rules and Container Specifications for truckshtpments, as applicable.

5.2 Marking.-In addition to any spectal marking required bythe contract or purchase order, containers shall be marked inaccordance with Standard MIL-STD-129. Marking Shall Include$ butnot be limited to~ the following information:

a. Manufactur.er$snameb. Product designationc. Lot number’d. Date of manufacturee. The number of t’hisspecification

5.3 Storage llmitat%onf3.-Mf4terialshall be stored h aweatherproof’stcrage facility.

6. NOTES

6.1 Ordering data.-procurmment docmwks should specify thetitles number and date of this specification.

6.2 Intended use.-The sodium mrboxymethyl cellulose isintended for use as a granulating agent ifithe manufacture ofLead Azide.

6.3 Inspection code numbers.-~e five digit code mbersassigned to the inspections herein are to facalltate future datacollection and analysis by the Government.

custodian: Prepar%ng Activity:Army-w Arrq+lU

Project Number: 6810-A~03y

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GPO 0e4- 361


mibs-51132a (kj) military specification

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