MILITARY_SPECIFICATION.pdf
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DOD-B-82669(OS) - MILITARY SPECIFICATIONS
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DOD-B-82669(OS)
19 January1979
SUPERSEDING
Ws 2101 30July 1965
MILITARY SPECIFICATION
BUTYL SEBACATE,DI-NORNIAL
This specificationis approvedfor use by the Naval Sea Systems Command,Departmentof the Navy, and is available for use by all Deparbnentsand Agencies of the Deparbnent of Defense.
1. SCOPE
1.1 Scope. Thisspecificationcoverstherequirementsforone typeof di-n-butylsebacatesuitableforuse in themanufactureof propellants.
2. APPLICABLEDOUJMEWS
2.1 Governmentdocuments.The followingdocumentsof the issuein
effecton dateof Invltatlonforbidsor requestforproposalforma part of thisspecificationto the extentspecifiedherein.
STANDARDS
MILITARY
MIL-STD-1OS
MIL-STD-129
MIL-ST’D-1218
PUBLICATIONS
NAVALSEA SYSTEMSCCMWND (CODEIDENT10001)
OD 43852 Determinationof Sodiumin Propylene GlycolDinitrateby theAtomic AbsorptionMethod
(Copiesof specifications, standards,drawings,andpublications requiredby contractorsin connectionwithspecificprocurementfunctions shouldbe obtainedfromtheprocuringactivityor as directedby the
SamplingProceduresandTablesfor Inspectionby Attributes
Marking for Shipment and Storage
ACS Chemicals contracting officer). - -
Beneficial comments (recommendations, pertinent datawhichmaybe of use in be addressed to: Commanding Officer, ization/Documentation Division (501), additions, deletions) and any improving this document should Naval Ordnance Station, Standard- IndianHead, MD 20640, by using the self-addressed Standardization Document (DDForm1426)appearing at the end of this
ImprovementProposal documentor by letter.
FSC 6810
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IXID-B-82669(OS)
2.2 Otherpublications.The followingdocumentsform a part of
this specificationto the extentspecifiedherein. Unlessotherwise indicated,the issuein effecton date of invitationfor bids or requests for proposalsshallapply.
NATIONALM~OR FREIGHTTRAFFICASSOCIATION,INC.,AGENT
NationalMotor FreightClassification
(Applicationfor copiesshouldbe addressedto the AmericanTrucking Associations,Attn: TrafficDepartment,1616P Street,Washington,DC 20036). “
UniformClassificationCommittee,Agent.
UniformFreightClassification
(Applicationfor copiesshouldbe addressedto the cationCommittee,Room 1106,222 SouthRive~sidePlaza, AMERICANtiCIETYFOR TESTINGAND MATERIAL,S
ASTM D-270 SamplingPetroleum
UniformClassifi- Chicago,IL 60606).
(ASTM)
and PetroleumProducts
ASTM D-1209 Colorof ClearLiquids(Platinum- CobaltScale)
(Applicationfor copiesshouldbe addressedto theilmericanSociety for TestingandMaterials,1916Race Street,Philadelphia,PA 19103),..
3. REQUIREMENTS
3.1 Physicaland chemicalrequirements,The physicaland chemical propertiesof the di-n-butylsebacateshallconformto the limitsspecified in TABLEI when testedas specifiedherein. If the individualor composite specimens(see4.2.3)fail to conformto any of the requirementsspecified, the lot shallbe rejected.,,I
TABLE I. Physicaland chemicalrequirements
Requirements Test ~~ Property “
Minimum Maxti Method
Color (Pt-CoScale) 10 4,3,2.1 Acidity (as acetic acid) (% bywt) - 0,05 4.3;2,2 Saponificationnumber 350 360 4,3,2,3 Refractiveindex (nD25°C) .1.4385 1,4405 4,3,2.4 Moisture(%bywt) O*15 4,3,2,5 Sodium(ppm) “= 1.0 4,3,2,6
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DOD-B-82669(OS)
e 3.2 Workmanship.The di-n-butylsebacateshallbe a waterwhite, homogeneousliquid,free fromdirt,sediment,and othersuspendedforeign matterwhen examinedvisuallyby transmittedlight.
4. QUALITYASSURVKX PROVISIONS
4.1 Responsibilityfor inspection.Unlessothewise specifiedin
the contract,the contractoris responsl%lefor the performanceof all inspectionrequirementsas specifiedherein. Exceptas otherwisespecified in the contract,the contractormay use his own or any otherfacilities
● suitablefor the performanceof the inspectionrequirementsspecified herein,unlessdisapprovedbythe Government.The Governmentreserves the rightto performany of the inspectionsset forthin the specification where such inspectionsare deemednecessaryto assuresuppliesand services.
conformto prescribedrequirements.
4.2 Inspectionprovisions.
4.2.1 Lot formation. If the process is a batch operation, each batch shall be a lot (see 6.3). If the butyl sebacate is produced in a continuous process, a lot shall consist of material produced by one plant of one manufacturer, with no change in the process, materials or conditions and offered for acceptance at one time.
o Sampling from tank cars shall be conducted in
4“2”2 -D-27,.accordance WI Sampling from smaller containers shall be conducted as follows: A random sample shall be taken from each lot, in accordance with MIL-STD-105, Inspection Level S-2, acceptance number zero.
If there are fewer than three containers in a lot, each container shall be sampled. In all other cases, no fewer than three containers shall be selected. A 500 milliliter (mL) specimen shall be remov+ from each container in the sample and placed in a clean, dry container (nonreactive with di-n-butyl sebacate) with a tight fitting closure. The container shall be labeled to identify the lot and container from which it was taken.
. 4.2.3 Test specimens. A composite specimen shall be made with equal portions horn each specimen and the composite shall be tested as specified in 4.3. If there are fewer than three specimens, each one shall be tested as specified in 4.3..
4.3 Qualtiyconformanceinspection. The materialshallbe subjected to all the followinginspectionsand testsfor acceptance.When specified in the contract(see6.2],the suppliershallsubmita reportgivingthe resultsobtainedfor all inspectionsand testsperformedand a certified statementthat the lotmeets all the requirementsof this specification.
Unlessothenwi.sespecified,all chemicalsshallbe ACS gradein accordance with MIL-STD-1218and distilledwater shallbe used. Whereapplicable, blankdeterminationsshallbe run and correctionsappliedwheresignificant.
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BO1l-B-82669(0S)
4.3,1 Visualinspection.All samples shall be visually inspectedto determine confomce to the workmanshiprequirementsof 3.2.
4.3.2 Test ~thods and procedures,
4.3.2.1 Deteztninationof color. The color of
shall be determinedin accordancewith ASTM D-1209, di-n-butylsebacate platinum cobalt scale.
4.3.2.2 Determinationof acidity. Measure 100 rnL of ethyl
almhol into a flask, add three drops of phenolphthaleinindicator,and titrate the alcohol to a faintpink color with O.lN sodium hydroxide solution. Add an accuratelyweighed 30 to 40 gram(g) portion of the sample to the alcoholicsolution. Titrate the mixture with O.llT sodium hydroxide.
Calculatethe percentageof acidity as acetic acid as follows: -
Precent bywt acetic acid = 6.005 VN
G where:
v= N= G= sodiumhydroxiderequired for titrationof sample,mL normalityof sodium hydroxidesolution weight of sample, g
4,3.2.3 Determinationof saponificationnunber. Transfer 0.8 g weighed to k 0.1 milligram (nig)-ofthe sample to an appropriatesize flask,and, add 50 mL of 0.5N alcoholic”potassiumhydroxideby means of a-calibrated burette or pipette,.(0.5N alcoholicpotassium hydroxide is prepared by adding o, 28 g of potassiumhydroxideto 1 liter of 95-percentethyl alcbhol).‘Fit -the flask to a reflux condenserby means”of ground joints and heat ,ona water 1 bath until the precipitationappears to be complete. Add approximately 1
15 mL of water to dissolve the potassiumsebacateand reflux o.na water bath’for not less than 60 minutes with occasionalwhirling of the flask.
Wash down the sides of the reflux condenserand the ground joints with approximately25:mL of the water. Cool the solution to 25°Cand titratewithstandard0.5Nhydrochloricacidusingphenclphthaleinindicator.
Protectsamplesolutionfromcarbondioxideduringheatingandcoolingwith an ascariteguardtube. At the sametime,conducta blankdetermination on 50 m of alcoholicpotassiumhydroxidewhichhasbeencarried throughthe completeprocess.Calculatethe saponificationntmiberas follows:
Saponification where:
VI .
V2 .
N= w= number’(mg.potassiqnhydroxideper g) = (VI - Vp)x N x 56.1
‘w volume of hydrochloricacid solutionrequired for blank titration,(mL) volwne of hydrochloricacid solutionrequired for the sample titration, (mL) normlity of the hydrochloricacid solution weight of san@ez,(g)
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IXD-B-82669(CE)
followingprocedure
Abberefractuneteror equivalent:
shall
a. Wipe with cautionto preclude scratchingthe prism surfaceof the refract-ter with a tissue wet with methanolor xykne, and then with a dry tissue. Adjust the temperatureof the water bath and the velocityof the circulatingfhid so that the themxneter reads 25.OOf 0.1“C.
b. Rotate the body of the instrumentand the nnving arm away from the operator until the interfacebetween the prims is hori.mntal. Loosen the
. prism clamp anddrop the lower prism. With a glass stirringmd, add a few drops of the sample liquid to be tested to the lower prism. Bring the prim faces together and lock the prism clamp. Rotate the instmnt to the normal viewing position. Adjust the mirror to reflect light into the
‘. telescope.
Unclamp the index am and nmve it to the far end of the scale.
Focusc;he telesmpe eyepiece sharplyon the crosshairs. Bring the divided field into view by roving the index am forward. The field maY kve a colored border, which can be ach.mnatizedby use of the mnpensators rotated by a pinion. The field will be sharpestwhen the edge is just turning blue.
Rring the field almst into coincidencewith the cm.sshairsby nwing the index arm. Adjust the mirror for the maximum illumination of the field.
Obtainthe finaladjustmmtof the fieldlineto the crosshairsby means of the fineadjustmentscrew.
d. Fbcusthe magnifier on the scale and rotate it so that the scale is well illuminated.Readthe scaledirectlyto threedecimalplacesand esti.mtethe figurein the fourthdecimalplace.
e. If the indexreadingdoesnot renai.nconstantwithinoneunit in the fourthdecimalplacefor 1 minute, it may indicate diffusionof =lvent remining on theprismsor insufficienttimeforthexnulequilibrium.Place a new San@e of the Mquid to be tested on the prism taking care that the prism is clean and dry. SUff icient the skmld elapse after placement of the dropto insurethatthe liquidfil.mis at theprim temperature.
. f. Reportthe readingobtainedas n#5°C.
4.3.2.5 Determinationof misture. lb the titrationflaskadd 75 to 100 mL of methanol.Titratethemethanolto a potentiometricend
. @nt withstabilizedKarlFischerreagent.‘Ihmsferan accuratelyweighed sampleof di-n-butylsebacate(5 to 15 g) to the titrationflask. Titrate the sample to as follows:
where:
K = F= w= a potenticmetric end point. G31culate the nmisture content
Percent moisture = 1OO(IQ?)
Karl Fischerre~gent rea@nt factor, g of weight of di-n-butyl w ‘ used in titration,mL waterpermL of reagent sebacate,’g
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I?3D-B-82669(@)
4.3.2.6 IHerminationof sodium. The sodiumshallbe determinedin accordancewith OD 43852exceptthat a factorof 1.17 shallbe used. ●
4.3.3 Rejectioncriteria.Failureof any,sampleto meet any require-ment of this specificationshall&, causefor rejectingthe lot or batch.
5. PACKAGING
5.1 Packaging.
5.1.1 Level C. The di-n-butyl sebacate shall be packaged in uniform quantities for shiprmat in accordance with the manufacturer’s cannercial practice. Packages shall be of uniform size, shape, and mterial.
5.2 Packing. ..
5.2,1 I..evelC. The di-n-butyl sebacate shall be packed in uniform quantities in such a mer as to assure carrier acceptance and tiford pro-tection against damge during direct shipment frcxnthe supply source to the first receiving activity. Containers used shall comply-with the Uniform Freight Classification, National hbtor Freight Classification, or other carrier regulations applicable to the tie of transportation. @ntainers shall be of uniform size, shape, and material.
5.3 Marking. In additionto any specialmarkingrequiredby the
contract,unit packagesand shippingcontainersshallbe markedin accordancewith WIL-ST!D-129. o
6. Nor’Es
6.1 Intendeduse. The di-n-butylsebacatecoveredby this specification is intendedfor use in the manufactureof propellant.
6.2 Orderingdata. Procurementdocumentsshouldspecifythe following:
6.2.1 Procurement requiremmts.
. Title, number, and date of this specification ;. Whether tank cars or containers are to be used for shipment
c. Size of containers required
d. Whether a certified analysis and/or test report is ~uired
6.2.2 Cbntractdata requirenx?nts.The itemsof deliverabledatawhich may be requiredby this specificationare citedin 4.3.
Data Requirement ApplicableDIIX
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‘IEstReport DI-T-2072 Certified Analysis
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IXXH3-82669(CX3)
e *DIW ( Data Item ~scriptiOns/D’D mm 1664) for the above data re@.re-ments are documented in the applicable ADL (Authorized Data List).
Such data will be delivered as identif @d on ampleted (numbered) DIW when specified on DD l?brms 1423 (Cbntract Data Requ.immnts Lists) and incorporated into applicable contracts.
6.3 Batch. A batch is defined as that quantity of di-n-but yl sebacatethat has been subjected to the sam unit chemical or physical process intended to nalse the final pzmduct hcmgeneous.
custodian :
NAVY - CE
Preparing Act ivity:
NAVY-(X
Project Number:
631 O-NA44
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OCUMENT IDENTIFIER ANO TITLE
DOD-B-82669(0S), BUTYLSEBACATE;D1-NORMAL
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