ARMY MIL-DTL-150 E-2008 POTASSIUM CHLORATE TECHNICAL《氯酸钾技术》.pdf

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1、INCH - POUNDDISTRIBUTION STATEMENT A. Approved for public release; distribution is unlimited.MIL-DTL-150E5 August 2008SUPERSEDINGMIL-P-150Dw/Amendment 128 April 1999DETAIL SPECIFICATIONPOTASSIUM CHLORATE, TECHNICALInactive for new design after 19 Apr 1996.This specification is approved for use by al

2、l Departments andAgencies of the Department of Defense.1. SCOPE1.1 Scope. Thisspecificationcoversthree gradesandsevenclassesoftechnical gradepotas-sium chlorate (KClO3).1.2Classification. Potassiumchlorateshouldbeofthefollowinggradesandclassesasspeci-fied (see 6.2).Grade A - Low bromateGrade B - Hig

3、h bromateGrade C - With magnesium carbonateClass1 - No.80sieve,nominalClass 2 - No. 100 sieve, nominalClass3 - No.60sieve,nominalClass 4 - No. 100 sieve, nominal, fineClass5 - No.50sieve,nominalClass 6 - No. 325 sieve, nominalClass7 - No.80sieve,nominal,fineAMSC N/A FSC 6810Comments, suggestions, or

4、 questions on this document should be addressed to: U.S. Army EdgewoodChemicalBiologicalCenter, ATTN: AMSRD-ECB-ENA-S, 5183BlackhawkRoad, AberdeenProvingGround, MD 21010-5424 or emailed to SpecsTeamapgea.army.mil. Since contact information canchange, youmay want toverify the currency of thisaddressi

5、nformationusingthe ASSIST Online databaseat http:/assist.daps.dla.mil.Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-DTL-150E22. APPLICABLE DOCUMENTS2.1 General. The documents listed in this section are specified in sections 3 or 4 of thisspecif

6、ication. This section does not include documents cited in other sections of this specifica-tion or recommended for additional information or as examples. While every effort has beenmade toinsure the completenessofthislist, documentusersare cautionedthatthey mustmeetall specifiedrequirementsofdocumen

7、tscitedinsections3or4ofthisspecification, whetherornot they are listed.2.2 Non-Governmentpublications. Thefollowingdocuments forma partofthisdocumentto the extent specified herein. Unless otherwise specified, the issues of these documents arethose cited in the solicitation or contract.AMERICAN CHEMI

8、CAL SOCIETYACS - Reagent Chemicals, 10th edition.(Copies of this document are available from http:/pubs.acs.org/reagents or AmericanChemical Society, 1155 Sixteenth Street, N.W., Washington, DC 20036.)ASTM INTERNATIONALD 1193 - Standard Specification for Reagent WaterE 11 - Standard Specification fo

9、r Wire Cloth and Sieves for Testing Purposes(Copiesofthisdocumentareavailablefromwww.astm.orgorASTMInternational,100BarrHarbor Drive, West Conshohocken, PA 19428-2959.)2.3 Orderofprecedence. Intheeventofaconflictbetweenthetextofthisdocumentandthereferences cited herein, the text of this document tak

10、es precedence. Nothing in thisdocument,however, supersedes applicable laws and regulations unless a specific exemption has been ob-tained.3. REQUIREMENTS3.1 Firstarticle. Whenspecified(see6.2),asampleshallbesubjectedtofirstarticleinspec-tion in accordance with 4.2.3.2 Appearance. Potassiumchlorate s

11、hallbe awhite, crystallinepowder whentestedasspe-cified in 4.4.1.3.3 Chemical characteristics. Potassium chlorate shall conform to the applicable chemicalcharacteristics of table I when tested as specified therein. For Grade C, Tricalcium Phosphate,inaquantitynotexceeding0.25percentofthe weightofpot

12、assiumchlorate, maybe mixedwithpotassium chlorate to prevent caking.Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-DTL-150E3TABLE I. Chemical characteristics.Characteristic Percent by weight TestP hGrade A Grade B Grade CParagrapMoisture, maximu

13、m 0.05 0.05 0.05 4.4.2Assay (as KClO3), minimum 99.5 99.5 96.5 4.4.3Water-insoluble matter, maximum 0.02 0.10 3.2 4.4.4pH of water-soluble matter 5to8 5to8 - - - - 4.4.5Hypochlorites To pass test To pass test To pass test 4.5.6Chlorites To pass test - - - - - - - - 4.5.7Chlorides (as KCl), maximum 0

14、.10 0.10 0.10 4.5.8Bromates (as KBrO3), maximum 0.02 0.10 0.10 4.5.9Heavy metals To pass test To pass test To pass test 4.5.10Alkaline earths To pass test To pass test - - - - 4.5.11Sodium, maximum 0.04 0.04 0.04 4.5.12Magnesium carbonate content - - - - - - - - 3.0 0.2 4.5.133.4 Granulation charact

15、eristics. Potassium chlorate shall conform to the applicable granu-lation characteristics of table II when tested as specified in 4.4.14.TABLE II. Granulation characteristics.Sieve SizeNPercent by weight passingNo.Class 1 Class 2 Class 3 Class 4 Class 5 Class 6 Class 7Min Max Min Max Min Max Min Max

16、 Min Max Min Max Min Max50 - - - - - - - - - - - - - - - - 98.0 - - - - - - - - - -60 - - - - - - - - 99.5 - - - - - - - - - - - - - - - - - -80 99.0 - - - - - - 60.0 - - - - - - - - - - - - - - 99.0 - -100 - - - - 99.9 - - - - - - 99.9 - - 85.0 - - - - - - - - - -140 45.0 55.0 - - - - - - - - 45.0

17、55.0 - - - - - - - - - - - -200 17.0 23.0 - - 5.0 - - - - - - 40.0 40.0 70.0 - - - - 90.0 - -325 - - - - - - - - - - - - - - - - - - - - 95.0 - - 60.0 - -Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-DTL-150E44. VERIFICATION4.1 Classification o

18、f inspections. The inspection requirements specified herein are classi-fied as follows:(a) First article inspection (see 4.2)(b) Conformance inspection (see 4.3)4.2 First article inspection.4.2.1 Lotting. The first article lot shall consist of at least 50 kg oftechnical potassium chlo-ratemanufactur

19、edusingthesamemethods,materials,equipment,andprocessesaswillbeusedduring regular production. The first article sample shall be submitted for inspection and ap-provalinaccordancewiththeterms ofthe contract. Ifthere isany changeofvendors,methods,materials, equipment, facilities, or ifthere is a break

20、inproductionof90 days or more, the con-tracting Officer shall be notified and at the discretion of the Government, a new first articlesample may be required.4.2.2 Sampling. The contractor shall randomly select three representative samples, ofapproximately one kg each, from the firstarticle lotof pot

21、assium chlorate andplace eachsam-ple in a clean dry container labeled to identify the first article lot.4.2.3 Inspection procedure. Eachfirst article sample shall be subjectedto all of the inspec-tions specified in the classification of characteristics in 4.3.5.4.2.4 Acceptance criteria. If any firs

22、t article sample fails to comply with any of the applica-blerequirements,thefirstarticlesampleshallberejected.4.3 Conformance inspection.4.3.1 Lotting. A lot shall consist of the potassium chlorate produced by one manufacturer,at one plant, from the same materials, under the same manufacturing condi

23、tions, and at thesame time. The minimum lotsize shall be 500 kg. Inthe eventthe lotis a batch operation(see6.3),severalbatchesmaybe mixedtogethertoformalot, providedthe batchesare subjectedtosome physical mixing operation intended to make the final product uniform and homogenous.4.3.2 Sampling. The

24、contractor shall randomly select three representative samples, ofapproximatelyonekgeach,fromthelotofpotassiumchlorateandplaceeachsampleinacleandry container labeled to identify the lot represented.4.3.3 Inspection procedure. Each potassium chlorate sample shall be inspected in accor-dance with thecl

25、assification ofcharacteristics in4.3.5. Failureof anysample toconform toanycharacteristic in the classification of characteristics based acceptance criteria specified thereinshall be cause for rejection of the lot represented.Provided by IHSNot for ResaleNo reproduction or networking permitted witho

26、ut license from IHS-,-,-MIL-DTL-150E54.3.4 Inspection characteristics. Critical characteristics are characteristics whose noncon-formancetospecifiedrequirementsislikelytoresultinhazardousorunsafeconditionsforindi-viduals who use or maintain the product. Characteristics whose nonconformance to specif

27、iedrequirements is likely to prevent performance of the tactical function of a major end item arealsocritical characteristics. Major characteristicsare characteristicswhose nonconformance tospecified requirements is likely to result in failure or to reduce materially the usability of theitem for its

28、 intended purpose. Minor characteristics are characteristics whose nonconformancetospecifiedrequirementsisnotlikelytoreducemateriallytheoperationorusabilityoftheitemfor its intended purpose.4.3.5 Classification of characteristics. Conformance inspections shall be as specified in thefollowing classif

29、ication of characteristics paragraphs.Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-DTL-150E6CLASSIFICATION OF CHARACTERISTICSPARAGRAPH TITLE DRAWING NUMBER4.3.5(a) Potassium Chlorate, Technical SHEET 1 OF1CATEGORY CHARACTERISTICSAMPLING ANDACC

30、EPTANCECRITERIAREQUIREMENTPARAGRAPHINSPECTIONMETHODCritical None definedMajor101 Appearance Seenote1 3.2 4.4.1102 Chemical propertiesa. Moistureb. Assayc. Water-insoluble matterd. pH of water-soluble mattere. Hypochloritesf. Chloritesg. Chloridesh. Bromatesi. Heavy metalsj. Alkaline Earthsk. Sodiuml

31、. Magnesium carbonateSeenote1 3.34.4.24.4.34.4.44.4.54.4.64.4.74.4.84.4.94.4.104.4.114.4.124.4.13103 Granulation properties Seenote1 3.4 4.4.14NOTES:1. Sampling shall be in accordance with 4.3.2. One specimen shall be taken from eachsample to perform each test.Provided by IHSNot for ResaleNo reprodu

32、ction or networking permitted without license from IHS-,-,-MIL-DTL-150E74.4 Tests.4.4.1 Appearance. Visually examine approximately 50 grams (g) of the specimen for formand color.4.4.2 Moisture. Heata moisture dishanditsstopperinanovenat 100 to 110Cfor 1 hour,cool in a desiccator, and weigh to the ne

33、arest milligram (mg). Transfer approximately 10 g ofthe specimen to the dry dish. Stopper and weigh to the nearest mg. Heat unstoppered in anoven at 100 to 110C for 1 hour. Cool in a desiccator. Replace the stopper and weigh to thenearest mg. Repeat the heating for 1/2 hour periods until successive

34、weighings differ by nomorethan1mg. Thetotaltimeofheatingshallnotexceed5hours. Calculatethepercentmois-ture as follows:Percent moisture =100AWwhere: A = Weight loss in grams after heating, andW = Weight in grams of specimen.4.4.3 Assay (as KClO3).(a) Ferrous ammonium sulfate solution. Dissolve 40 g o

35、f ferrous ammonium sulfateFe(NH4)2(SO4)2S6H2Oinacold5+95solutionbyvolumeofsulfuricacidanddiluteto1literwith the sulfuric acid solution. Titrate with 0.1N potassium permanganate solution and calcu-late the volume in milliliters (mL) of potassium permanganate solution equivalent to 1 mL ofthe ferrous

36、ammonium sulfate solution. Determine equivalency under the same conditions oftest as in (b) except that no potassium chlorate will be present.(b) Procedure. Weigh to the nearest 0.1 mg approximately 0.8 g of the specimen. Dis-solve in water and dilute to 500 mL in a volumetric flask with water. Tran

37、sfer a 50 mL aliquotto a 500 mL Erlenmeyer flask and dilute to 150 mL with water. Add 10 mL of a 1 + 2 solutionby volume of sulfuric acid. Insert a Bunsen valve in the flask and heat the contents almost toboiling. Add 50 mL of the ferrous ammonium sulfate solution prepared as specified in (a) bymean

38、s of a pipet and boil the solution for 2 minutes. Cool the solution, loosen the valve, add5mLofconcentratedphosphoricacidand10mLofa10percentsolutionofmanganesesulfate.Titrate the excess offerrousionwith0.1Npotassiumpermanganate solutionto afaint pinkendpoint. Calculate the percent potassium chlorate

39、 as follows:Percent potassium chlorate =0.2043A(BC)(100D)Wwhere: A = Normality of the potassium permanganate solution used,B = Milliliters of the potassium permanganate solution equivalent to the totalvolume of ferrous ammonium sulfate solution added,Provided by IHSNot for ResaleNo reproduction or n

40、etworking permitted without license from IHS-,-,-MIL-DTL-150E8C = Milliliters of potassium permanganate solution required for titration of theexcess ferrous iron,D = Percent moisture calculated in 4.4.2, andW= Weight in grams of specimen.4.4.4 Water-insolublematter. Dryafilteringcrucibleofsufficient

41、poresizetopreventclog-ging to constant weight at 100 to 110C. Cool in a desiccator and weigh to the nearest 0.1 mg.Weightothenearest0.1gapproximately50gofthespecimenanddissolveinapproximately800mL ofwater. Filter the solutionthroughthe weighed crucible and washthe residue with 5 por-tionsofhotwater.

42、 Retainthefiltrateforsubsequentdeterminations. Drythecrucibleandresi-due for 3 hours at 100 to 110C. Cool in a desiccator and weigh to the nearest 0.1 mg.Calculate the percent water-insoluble matter as follows:Percent water-insoluble matter =100AWwhere: A = Weight in grams of residue, andW= Weight i

43、n grams of specimen4.4.5 pH ofwater-solublematter. Coolthe filtratefrom 4.4.4to roomtemperature. Trans-fertoa1litervolumetricflaskanddilutewithwatertothemark. DeterminethepHofaportionof this solution by means ofa suitable standardized pH meter. Save the remaining solutionforlater use.4.4.6 Hypochlor

44、ites. Toa200 mLaliquotofthe solutionfrom 4.4.5,addastripofpotassiumiodide-starchpaper. There shall be no immediate appearance ofa blue color whichindicatesthe presence of hypochlorites. If the test for hypochlorites is negative, retain this solution for4.4.7, if required. Disregard the test for chlo

45、rites if hypochlorites are present.4.4.7 Chlorites. If a negative test for hypochlorites was obtained in 4.4.6, add 5 mL of0.1Nsulfuricacidtothesolutionandtestwitha freshstripofpotassium iodide-starchpaper. Thereshall be no immediate presence of a blue color which indicates the presence of chlorites

46、.4.4.8 Chlorides. To a 100 mL aliquot of the solution from 4.4.5, add 1 mL of a 5 percentsolutionofpotassium chromate andtitrate to a permanent faint blood-red tinge with 0.1Nsil-ver nitrate solution. Calculate the percent chlorides as KCl as follows:Percent chlorides =7.456ABWwhere: A = Milliliters

47、 of silver nitrate solution used,B = Normality of silver nitrate solution, andW= Weight in grams of specimen in aliquot from 4.4.5.Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-DTL-150E94.4.9 Bromates.4.4.9.1 Starchindicatorsolution. Mix2gofsolublestarchandseveralmilligramsofmercu-ric iodide, CP grade, (as a preservative) with a little water. Add the mixture slowly to 500 mLof boiling water. Allow the liquid to boil for 5 minutes; then c