NAVY MIL-A-82667 1-1977 AMMONIUM PERCHLORATE HIGH PURITY《高纯度高氯酸铵》.pdf

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1、MIL-A-82667/l(OS)31 Janq 1977MIuTARY sPmIFmATImAMmNIuMPEKmmATE, HIGHPURITYZhis detail spcificationis approvedfor use by thePthe suppliermay utilizehis own facilitiesor any ccamxcial laboratoryacceptableto theGOvermmt. The Governmnt reservesthe right to performany of the inspectionsset forth in the s

2、pecificatim where such inspectionsare deemednecessarybassure,suppliesand servicesconformto prescribedrequirements.4.2 Lot. A lot shallconsistof the totalquantityof cross-blendedmaterial.-r non-cross-blendedmaterial,a lot shallconsistof thequantityproducedin a singlebatch,or when manufacturedby a con

3、tinuousprocess,a lot shallconsistof the totalquantityoffhold the weicdxsdti nearest 0.1mg, in approximately 45 ml of-w mix.3Add 1.0 ml of 0.25% diphenylcarbazi e solution in alcohol and mix. Prepare a blank in the same mnnerand add standard (O.0004 g/ml) potassium chrmate solution until the colormat

4、ches that ofin the specimenPercentagewhereA = volumeW = weightthe saqle solution.as potassium chrmateof potassium chromateof standardpdassimof sample, gCalculate the Wcentaqe of chrcmtesby the foll&g foa:= 0.04Awchmmte solution added to blank,4.5.6 D.terrdnation of sulfates. Sulfates shall be detenn

5、ind inaccordancewith OD 18996.nil4.5.7 Detenninationof sulfated ash. Sulfated ash, weighed as sodiumsulfate (Na-$3fi) and calculated as sodium perchlorate (NaCIO) shall bedetermin&l Gy %. followingmtlmd. Grind-at least 5 g of &id sample toa fine Pm&r. Add 0.2 g of sample to a previously igniteiland

6、taredsilica crucible. Cover. Heat carefully with a Bunsen flame until deco-mpositionoccuxs. Continue the ignition of -11 increments mtil the entfiesample has decomposed and the volatile salts have beeridriven off. ZWLOWthe crucible to cool. Add 3 ml of concentrated sulfuric acid, heat again, (and co

7、nplete the volatilizationof sulfuric acid at a dull red heat. Coolin a desiccator and weigh. Calculatespecimn as sodium perchlorate by thePercentage of scdium perchloratethe percentage of tilfated ash in thefollowing formula:= wt of residue x 122.5 x 100wt of sanple x 71 ,= wt of residue x 172.5wt o

8、f sample4.5.8 Deternination of iron as ferric oxide (F.7Q.(a) F&agents: Hydrochloric acid, concentrated,Anerican MealSociety (ACS)reagentI Nitric acid, concentrate, ACS reagentSulfuric acid, concentrated,ACS rementAnmmnium thi&nate, 1%,soiution ofACS reagentIron wire, ACS reagentPotassim permanganat

9、ereagent(b)Apparatus: 50-ml Nessler tubes8(KMnO)1% solutionof ACS.,Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-Mm-A-82667/l(0S)II(c)Procedure: ligh accurately0.10g of brightironwire. (Anequimlent weightof any other recognizedprimazystandad, with

10、approximatelymdified preparationpmcedure, my be substitutedfor the ironwire standard.)Dissolvethe ironwire in 5 ml of commtrati ric acid. -f-the solutionto a l-litervolumetricflaskand diluteto volum. This isthe stmdard solutim. TO the ash fromthe sulfatedash procedure,asspecifiedin 4.5.7,add 1 ml of

11、 mncentra hydrochloricacid and 1 mlof cmoentrated nitricacid. Transfertoa50inl beakerwith aminimumof distilledwater and boil to drynesson a hot plate. Moistenthe reshwith 2 dropsof concentratedhydmchlm ic acid,and wash with distilledwter into a 10H glassstqpemd volumetricfI.ask.Accuratelytransfera35

12、+nlportion of thestmdard solutionto a second100+nlglass-pperedvolumetricflask. Add 2.0ml of concentratedsulftmicacid, 2 dropsofpotassiumpermmgana solution,and 10 ml of 1% annmniumthiocyanaesolutionto each flask. Diluteto volume,d well, and transferto50+ilNesslertubes. The sampleshallbe no darkerthan

13、 the standami.4.5.9 DeterRuna tionofsodium andpbas sium.4.5.9.1 Preparatim of reagents. Quantitativelytransfer1.9066gof potassiumchlorMe (KC.1)and 2.5416g of sodiumchloride (NaCl)into?Xdlllatdy250ml of water.?* l-literVolumtiic flasksmn9 appml to dissolvethe saltand diluheto volumewith water. Each s

14、olutionContaims1 rqhnl of cation. Fran these stock solutions,transferaliquots= othervolmtric flasksand dilutewithwater so that at l-t fourstandardsolutionsare preparedin the range0.005to 0.03mg/ml.for thepotassim ion and 0.001to 0.005ml for the scdiumion.4.5.9.2 Preparationof standardcurves. Ileterm

15、inethe net emissionin lxmnsof percentageof transmittanceof the s&ndard solutionsusingawavelengthof 766.5nanomtres (ml for * mtassi i and 589 forthe sodiumion. minimumpracticalslit-widthshouldbe used. Prewa grapheitherby plottingabsorhnce versusconcentrationon linearcoor-dinatesor the percentageof tr

16、ansmittanceversusconcentrationon semilcgcoordinates. Fit a straightlineto the points.4.5.9.3 Analysisof sap le. Quantitativelytransfer4.0 g of ammnium.perchlorate,weighedto the nearestntg,intia 100* volmtric flask.Dissolvein distilledwker and dilubsto vokm. Determineby plOtkk9th-epercen12qeof transm

17、ittanceof each s solution,a distilledwaterblank solution,and the samplesolution. Read the concentrationof thesampledirectlyfrom the standardcurve.4.5.9.4 Calculation. Calculatethe -Po-ssiumand sodiumcontentasfollows:Percentageof potassiumand sodium= 10 ( + k)w%=% =w =assium concentrationsodiumconcen

18、=ation asweightof sample,gas read from sarda.rdcum=, W/mlread from standard cume, rnl9Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-mLrA-82667/l(OS)4.5.10 Determinationof nonalkalimetals as oxides. This determ&tionshall& in accordancewith OD 18995.

19、4.5.11 Determinationof surfacemisture. Surfacemisture shallbedeterminedin accordancewith ASIME 203-75if a directtitrationisused and ASTM D 1348-61if a back titrationmethod is used. In eithercase a 1:1mthanol:benzene mixtureshallbe used as the camier solution./ 4.5.12 Determinationof totalmoisture. T

20、otalmisture shallbedetermined in accordancewith TME 203-75using 1:3methanol:idineas the carrier.4.5.13 Determinationof water insoluble. Dissolve25.0g of thesamplein 175ml ofdistilledwater and filterthe solutionthroughataredcrucibleof fineporosity.Washwith distilledwater, for 1.5hours at 105”C,cml, a

21、nd weigh. Calculatethe percentageofinsoluble as follows:Watf?rPercentageof water insoluble = (wtof residue,g)100wtof sample,g4.5.14 Determhlationof ether solublesas organicmaterial. Transfer25 t 0.1 g of the spximn intoan extractionthinbleof a Soxhletextractionapparatus. Extractwith 100ml of anhydro

22、usethylether for2 hours. Transferetherextractto a taredVycor dish and evaporateto (drynesson water bath. Run ablank deternun“ationon 100ml ether. Theincreaseinweightms the blank is calculatedas organicmaterialas follows:Percentageof ether solubles= (increasein wt, g - wt of blank,g)100I.wt of sample

23、,g4.5.15 Determination”of totalvolatiles. IYansfera 10-gportionof sample,weighedto the nearest0.1nq, to a taredwide-formnbisturedish and weigh. Place in a gravity-convectionoven and allowto rmainfor 2 hoursat 177 I 2“C. Cool in a desiccatorandweiqh. Calculatethepercentageof volatilematteras follows:

24、Percentageof volatilematter= (Wl- 2)1OOs1 whereW1. ight of dish plus SFiITe,92 = %eightof dish plus sqle afterh-ting,s = weightof sample,g 94.5.16 Determinationof stability. For heat stabilitydetermination,transferfour 10 g portionsof sampleto 60 mndiameter almimmweighingdisheswhichhave previouslybe

25、en heatedto approately 700”Cand COOled.Placeon sheflocated4 inchesfrcmtop of gravity-mnvectionoven.Maintainoven temperatureat 177Ct 2C. Remve one samplefromthe ovenafter2 hours and an additionalsampleeveryhour thereafter. Cool thesamplein a desiccator20 to 30 minutes. Add approximately5 g of ccoled1

26、0Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-IIbsaetOamixtur e of 100ml distilledwater,iodide (XI),and 5 ml of 0.2%-staxchsolution.nerchlorate. IhesolutionshallremainalmostMIIL-A-82667/l(OS)0.5 g granularpotassiumStir to dissolveannwniumcolorless

27、. Xmmdia* appar-).anteof violetor blue indicatesdecmpsition. Repeatthe procedurefor each,sampleremved fromthe oven.4.5.17 Detemurla“ tionof pH Zd 50 ml of hot, freshly-boileddistilledwater to 20.0g of Specinten.Stir and cool m room temperature(20to 25C)and allow the precipitateto settle. Measurethe

28、pH on a suitile .po-tio-meber havingglass calmel electrodes.4.6 Physi&L testprocedUres.4.6.1 Color. Dissolvea 10 g portionof samplein 100 ml of waterand transfer100ml of solutionto a Nesslertube. Cmpare with a standardcon 0.005g of po-sim te (4 ) W liter. mleshallkenodarker than thes.4.6.2 Friabilit

29、y. This test shalllx?perfomed on Type I material.There is no friabilityrequirementfor II.4.6.2.1 APparatus. me followingapparatusshallbe requird:(a)Ox&s qmating-siftingmachine,or equivalmt(b)M 110. 100 U.S. StandardStainless-SteelSievesP RR-S-366(c)One hundred3-Nanass beadsI (d)Stainless-steel& lid

30、and pan(e) ma c.4.6.2.2 Procedure. Triplicatetests shallbe performedin accordancewith the foil- :(a)Place 100 g of sampleon a no. 100 U.S. Standardstainless-SteelSievewith stainless-steelpan and coverlid.(b)Placeassemblyon siftingmachineand shakefor 30 t 1 minutes.(c)Weigh out 50 t 0.01g of samplere

31、mining on * no. 100 sieveand add to the secondno. 100 sievewith one hundred3- glassbeads.Assemblewith coverand pan.(d)Place assemblyon the siftingmachine,attachclaws oneach sideof the sieve,and shakefor 30 A 1 minutes.(e)Weigh ammt of samplepassingthroughthe no. 100 sieve.(f)Qculate as follms and re

32、portthe averageof the tests:Rercen&ge of friability= * passing sieve 100initialWt4.6.3 Granulation.4.6.3.1 I- “cle sizedistribution.11Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIG&82667/l(os)I4.6.3.1.1 Procedure. Particle-size distribution shal

33、lbein accordance with the following:(a)Iagent: Tricalcium phosphate (ZCP)conditioner(b)Apparatus:(1)Sieve shaker: A Tyler “-Tap” or its equivalentand cover and automatic tircer(2) Sieves: One set, includfiq 8-inch diamtex, U.S.4determkdwith ,mpanStandardSieves no. 18, 20, 50, 70, 100, 140 200,andRR-

34、S-366.(c)Relative humidity: The atmsphere in thesieving analyses shall be maintained at a relativethan 70%. Very moist or very dry atnmsphere cause325 &o&oming toroan used for thehumidity not greatererroneous resultstespecially with saes containing substantialcentages of fine particles.(d) lhspectio

35、n: Sieves shall be Lispecteddaily for visible evidenceof damage or failure, especially near the periphery of the cloth, andchecked by running a standard sample on which the results shall not varynmre than l.% from the previously established-averagevalue for each sieve.A master set of sieves shall be

36、 kept as a standard, to detectwear on thesieves that are in rejular use.(e)Blending: Blend the composite sample carefully in the .sanecontainer, and weigh out 100.0 g. Add 1.0 g of ICPconditioner,and &ixthoroughly by shaking for 1 minute iria l-pint glass jar. q(f)Procedure: Asseni31ethe sieves in n

37、umerical order fran top tobottcm, with a pan under the stack. Transfer the material to the.topsieve, add the cover to the top of the stack, and place the set in theshaker. Set the timer to run 13 minutes, and start the shaker. menthe shaker has stoppd, remve tie stack of sieves. Starting tith the to

38、psieve, brush any material adhering to the bottom of the sieve into thenext lower sieve, and transfer the contents to a sheet of glazed pa.Use a brush to remve any material that remains within the sieve. Weighthe retained material to the nearest 0.1 g. Clean the material frcm theremining sieves succ

39、essivelyin the same inann=r adding each fraction tothe preceding ones. Record the cumulativeweight, tich is equal to thepercentage of cumulative retentionof the original sample (neglectingihetheconditioner,which is assumsd to pass to the pan).-4.6.3.1.2 Calculations.(a)Ihecalculations for the percen

40、tage of sample passing throughsieve shall be as follows:Percentage of weight (wtof sample - cumulative wt reiained) x 106passing through sieve = wt of sanqle(b)The calculations for the percentage of sample retaind shallbe as follows:12 *Provided by IHSNot for ResaleNo reproduction or networking perm

41、itted without license from IHS-,-,-MIxrA-82667/l(0S)I?ercentageofweightretied wtongiwn sievex 100ona givensieve = wtofsample(c) *ightedaverageshallbecalculatedasfollows:.= weightedaverageparticlesize,Mm= weightofsampleretainedon2&reshscreen,gWso =weightofsampleretiinedonSO-meshscreen,g90 =weightofsa

42、qleed on70msh screen89P?l(-jo=weicof sampleretainedon 1004n2shscreen%40 = VP+W ofqle ree cm140-mshscreen:200= -* ofsamplemta.medon2oo-meshscreen*9325- weightofsampleretainedon325-nEshscreen -weightofsanpleo nkottzmpan, g. 994.6.3.2!&peII “de size. ParticlesizeshallbedetaminedinacmrdancewithASU4B 330

43、-65.4.7 AcQqxxmcecriteria.Failuretoaxlfonntoanyofthercqlliremzltsshallbecauseforrejectionofthelot.4.8 . . . repackaging,pacldngal-tdmrkingshallbeinso=td toverifyconfo rmmoewitht her = of S=* 5.samp&g shallbeinaccordancewith_105 withanAQof2.5defective.5. PMXAGI?JG5.1 iltgandpaddnq Unlessothemisespeci

44、fiinthecontractororder,packagingandPack?”ahallbelevelc.5.1.1Levelc. unlesspackagingEJ&lg of zendse specifiedinthecontract(see6.2),aumnn.iumperchloramshal.lbeinacmrdamewithstan&Xlcmmrdal practiceapplicabletothetypeofmaterial.TbePackng andpackingslwll beefsuchconstmctionandmterialsthattheCrxltents- be

45、adequatelyProwctd againstlossorcontim. TheCmtdmra shallanlformto49CFR171-179.Dessicant,conformixtgtoTypeIof3464, sha.U.be includedin containersas specifiedin thecmdxact(see6.2).13Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-P!IIrA-82667/l(OS)5.2 M

46、arking.-ST&129 and 49the followirig:Marking of containers shall,be inCFT 171-179 and shall include, butaccordance withnot be limitd b,(a) Title, number, revision letter ad date of this specification(b)Lot number(c)ntract or purchase order number(d)Net weight(e)Mterial trade nam(f)Manufacturersname a

47、nd location6. NOTES6.1 Intended”use. The material is intended for use as an oxidiz&in solid propellantmanufacture for the CKU-5/A rocket catapult assemblyand other rccket motor applications.6.2 Ordering data. Procurement6.2.1 procurement reauirments:(a)Title, number, revision(b)Quantity required(c)

48、Place of inspectiondocuments should specify the following:letter and date of this specification(d) Place of delivery and desiccant required.(e)Amount of dessic&t required (see 5.1)(f)Packaging requirements if other than as specifid (see5.1)46.2.2 Contract data reauirts. !& items of deliv=able datare

49、qqired by this specificationare cited in the followingparagraphs:IParagraph4.4Data ReauirenentTest reportAicable DID * DIDCs (DataItem Descriptions/DDForm 1664) for the above datarequirement are docuna ted in the applicableADL (AuthorizedData List).Such data will be delivered as identifiedon conq?leted(nunbered)D