1、METRICDISTRIBUTION STATEMENT A. Approved for public release; distribution is unlimited.MIL-DTL-11361E13 June 2007SUPERSEDINGMIL-M-11361D24 December 1992DETAIL SPECIFICATIONMAGNESIUM CARBONATEInactive for new design after 14 Oct 1997.This specification is approved for use by all Departments andAgenci
2、es of the Department of Defense.1. SCOPE1.1 Scope. This specification covers magnesium carbonate to be used in smoke mixtures.2. APPLICABLE DOCUMENTS2.1 General. The documents listed in this section are specified in sections 3 or 4 of thisspecification. This section does not include documents cited
3、in other sections of this specifica-tion or recommended for additional information or as examples. While every effort has beenmadetoinsurethecompletenessofthislist, documentusersarecautionedthatthey mustmeetall specifiedrequirementsofdocumentscitedinsections3or4ofthisspecification, whetherornot they
4、 are listed.2.2 Government documents.2.2.1 Specifications, standards, and handbooks. The following specifications, standards,and handbooks form a part of this document to the extent specified herein. Unless otherwisespecified, the issues of these documents are those cited in the solicitation or cont
5、ract.AMSC N/A FSC 6810Comments, suggestions, or 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, yo
6、umaywanttoverifythecurrencyofthisaddressinformationusingtheASSIST Onlinedatabaseat http:/assist.daps.dla.mil.Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-DTL-11361E2FEDERAL STANDARDSFED -STD -313 - Material Safety Data, Transportation Data and
7、 Disposal Data forHazardous Materials Furnished to Government Activities(Copies of these documents are available online at http:/assist.daps.dla.mil/quicksearch/ orhttp:/assist.daps.dla.mil or from the Standardization Document Order Desk, 700 Robbins Ave-nue, Building 4D, Philadelphia, PA 19111-5094
8、.)2.2.2 OtherGovernmentdocuments,drawings,andpublications. ThefollowingotherGov-ernment documents, drawings, and publications form a part of this document to the extentspecified herein. Unless otherwise specified, the issues of these documents are those cited inthe solicitation or contract.U.S. ENVI
9、RONMENTAL PROTECTION AGENCYEPA Method 6010B - Inductively Coupled Plasma-Atomic Emission Spectrometry(Copies of these documents are available online at www.epa.gov or from the U.S. Environ-mental ProtectionAgency, Ariel Rios Building, 1200 Pennsylvania Avenue, N.W., Washington,DC 20460.)2.3 Non-Gove
10、rnmentpublications. Thefollowingdocuments forma partofthisdocumentto the extent specified herein. Unless otherwise specified, the issues of these documents arethose cited in the solicitation or contract.ASTM INTERNATIONALB 527 - Standard Test Method for Determination of Tap Density of MetallicPowder
11、s and Compounds(Copiesofthisdocumentareavailablefromwww.astm.orgorASTMInternational,100BarrHarbor Drive, West Conshohocken, PA 19428-2959.)2.4 Orderofprecedence. Intheeventofaconflictbetweenthetextofthisdocumentandthereferences cited herein, the text of this document takes precedence. Nothing in thi
12、sdocument,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.Provided by IHSNot for ResaleNo reproduction or networking permi
13、tted without license from IHS-,-,-MIL-DTL-11361E33.2 Chemicaland physicalcharacteristics. The magnesium carbonate shall conform to thechemical and physical characteristics of table I.TABLE I. Chemical and physical requirements.Characteristic Requirement Test ParagraphAssay (as MgO), percent by weigh
14、t 40.0 to 43.5 4.4.1Matter insoluable in HCl, percent by weight, maximum 0.02 4.4.2Water-soluable substances, percent by weight, maxi-mum0.50 4.4.3Calcium (Ca), percent by weight, maximum 0.45 4.4.4Arsenic (As), ppm, maximum 2 4.4.5Lead (Pb), ppm, maximum 10 4.4.5Other Heavy metals, ppm maximum 20 4
15、.4.5Iron (Fe), percent by weight, maximum 0.02 4.4.6Moisture, percent by weight, maximum 1.0 4.4.7Particle size distribution: 4.4.8Average particle size, microns, maximum 20Average particle size, microns, minimum 7Distribution shape Single modeTap density, grams per milliliter, minimum (dry basis) 0
16、.2 4.4.9Tap density, grams per milliliter, maximum (dry basis) 0.6 4.4.9Thermal Characteristics: 4.4.10Peak of first endotherm, temp. range (_C) 235 to 250Loss after first endotherm, percent by weight,minimum4Peak of second endotherm, temp. range (_C) 435 to 4504. VERIFICATION4.1 Classification of i
17、nspections. The inspection requirements specified herein are classi-fied as follows:(a) First article inspection (see 4.2)(b) Conformance inspection (see 4.3)Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-DTL-11361E44.2 First article inspection.
18、4.2.1 Lotting. The first article lot shall consist of at least 50 kg of magnesium carbonatemanufactured using the same methods, materials, equipment, and processes as will be usedduring regular production. The first article sample shall be submitted for inspection and ap-provalinaccordancewiththeter
19、ms ofthe contract. Ifthere isanychangeofvendors,methods,materials, equipment, facilities, or ifthere is a break 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
20、shall randomly select three representative samples, ofapproximately one kg each, from the first article lot of magnesium carbonate and place eachsample 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
21、the inspec-tions specified in the classification of characteristics in 4.3.5.4.2.4 Acceptance criteria. If any first 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 magnes
22、ium carbonate produced by one manufac-turer, at one plant, from the same materials, under the same manufacturing conditions, and atthe same time. The minimum lot size shall be 500 kg. In the event the lot is a batch operation(see 6.7), several batches may be mixed together to form a lot, provided th
23、e batches are sub-jected to some physical mixing operation intended to make the final product uniform and ho-mogenous.4.3.2 Sampling. The contractor shall randomly select three representative samples, ofapproximately one kg each, from the lot of magnesium carbonate and place each sample in aclean dr
24、y container labeled to identify the lot represented.4.3.3 Inspection procedure. Each magnesium carbonate sample shall be inspected in ac-cordance with the classification of characteristics in 4.3.5. Failure of any sample to conform toany characteristic in the classification of characteristics based
25、acceptance criteria specifiedtherein shall be cause for rejection of the lot represented.4.3.4 Inspection characteristics. Critical characteristics are characteristics whose noncon-formancetospecifiedrequirementsislikelytoresultinhazardousorunsafeconditionsforindi-viduals who use or maintain the pro
26、duct. Characteristics whose nonconformance to specifiedrequirements 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 t
27、o reduce materially the usability of theProvided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-DTL-11361E5item for its intendedpurpose. Minor characteristics are characteristics whose nonconformancetospecifiedrequirementsisnotlikelytoreducemateriallythe
28、operationorusabilityoftheitemfor its intended purpose.4.3.5 Classification of characteristics. Conformance inspections shall be as specified inthefollowing classification of characteristics paragraphs.Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-M
29、IL-DTL-11361E6CLASSIFICATION OF CHARACTERISTICSPARAGRAPH TITLE DRAWING NUMBER4.3.5(a) Magnesium carbonate SHEET 1 OF1CATEGORY CHARACTERISTICSAMPLING ANDACCEPTANCECRITERIAREQUIREMENTPARAGRAPHINSPECTIONMETHODCritical None definedMajor101 Chemical and physical properties Note 1. 3.2a. Assay 4.4.1b. Mat
30、ter insoluable in HCl 4.4.2c. Water soluable matter 4.4.3d. Calcium content 4.4.4e. Arsenic, lead and otherheavy metals content4.4.5f. Iron content 4.4.6g. Moisture content 4.4.7h. Particle size 4.4.8i. Tap density 4.4.9j. Thermal characteristics 4.4.10NOTES:1. Sampling shall be in accordance with 4
31、.3.2. One specimen shall be taken from eachsample to perform each test.Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-DTL-11361E74.4 Tests.4.4.1 Assay (see 6.5). Dissolve 5 g of 8-hydroxyquinoline (oxine) in 12 milliliters (mL) ofglacial acetic
32、acidand dilute to 100 mL withwater. Filter if necessary. Weigh tothe nearest0.1milligram (mg) approximately 0.2 g of specimen and transfer to a 250 mL beaker. Add 30 mLof water and just sufficient concentrated hydrochloric acid to dissolve the specimen. Dilute toabout 100 mL with water. Dry a filter
33、ing crucible to constant weight at 105 to 110_C, cool in adesiccator, and weigh to the nearest 0.1 mg. Add 2 g of ammonium chloride to the specimensolution and add concentrated ammonium hydroxide to a pH of 10 to 11. Heat the solution to70 to 80_C and add dropwise, while stirring, 13 mL of the 8-hyd
34、roxyquinoline solution. Addmore ammonium hydroxide, if necessary, to maintain the pH at 10 to 11. While keeping thetemperature between 70 to 80_C, mechanically stir the mixture for 15 minutes. Filter throughthe weighed crucible. Wash the precipitate well with small portions of a 1 percent ammoniumhy
35、droxide solution. Dry and ignite the precipitate at 800_C for 20-30 minutes, cool in a desic-cator, and weigh to the nearest 0.1 mg. Calculate the percent magnesium oxide as follows:Percent magnesium oxide = 100AWwhere: A = grams of precipitate, andW= grams of specimen4.4.2 Matter insoluble in hydro
36、chloric acid. Drya filteringcrucible at100to105_C, coolina desiccator, and weigh to the nearest 0.1 mg. Transfer approximately 10 g of the specimen,weighed to the nearest 0.01 g, to a 250 mL beaker, mix with 100 mL of water, and add slowly,while stirring, 25 mL of concentrated hydrochloric acid. Boi
37、l the solutionfor 5minutes andfil-ter while hot. Wash the residue thoroughly with hot water and dry to constant weight at 100 to105_C.Coolindesiccatorandweightothenearest0.1 mg.Calculate thepercentmatterinsolu-ble in hydrochloric acid as follows:Percent matter insoluble in hydrochloric acid = 100AWw
38、here: A = grams of residue, andW= grams of specimen4.4.3 Water-soluble substances. Weigh to the nearest milligram approximately 2 g of thespecimenandboilwith50mL ofwater for5 minutes. Restore theoriginal volumewith hotwa-terandfilterwhilehot.Transfer25mLoftheclearfiltratetoaweighedplatinumdishandpla
39、ceonasteambathtoevaporatethewater.Evaporatetodrynessat105to110_C.Coolinadesicca-tor and weigh rapidly. Calculate the percent water-soluble substances as follows:Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-DTL-11361E8Percent water-soluble subs
40、tances = 100AWwhere: A = grams of residue, andW=gramsofspecimeninaliquotused4.4.4 Calcium content (see 6.5).4.4.4.1 Standard magnesium solution. Weigh to the nearest 0.1 mg approximately 0.5 g ofpolished magnesium metal ribbon and dissolve in 50 mL of hydrochloric acid (1 to 10).4.4.4.2 Ammonium hyd
41、roxide-ammonium chloride buffer. Dissolve 60 g of ammoniumchloride in about 200 mL of water, add 570 mL of concentrated ammonium hydroxide, and di-lute to 1 liter.4.4.4.3 Eriochrome black T indicator solution. Dissolve0.15gofEriochromeblackTand0.50 g of borax in 35 mL of methanol. Warm to effect sol
42、ution.4.4.4.4 Standard disodium dihydrogen ethylene diaminetetraacetate solution. Dissolve8.00 g of disodium dihydrogen EDTA in 2 liters of water. Pipet 10 mL of the standard magne-sium solution into a 250 mL Erlenmeyer flask. Add 25 mL of water, 10 mL of the ammoniumhydroxide-ammonium chloride buff
43、er, and 3 or 4 drops of the indicator solution. Titrateagainst a white background under an incandescent light with the disodium dihydrogen EDTAsolution to a pure end point having no trace of pink. Calculate the molarity of the disodiumdihydrogen EDTA solution as follows:M = 0.8224AVwhere: M = molari
44、ty of the disodium dihydrogen EDTA solution,A = grams of magnesium ribbon used in the preparation of the standardmagnesium solution, andV = milliliters of disodium dihydrogen EDTA solution used.4.4.4.5 Standardcalciumsolution. Dissolve1.0009gofcalciumcarbonatein5mLofhydro-chloric acid (1 to 1) and d
45、ilute to 1 liter with water. Pipet 30 mL of this solution into a 250 mLErlenmeyerflask,add25mL ofwater, 2mL of20 percentsodium orpotassium hydroxidesolu-tion, and1tabletofmurexide(ammoniumpurpurate)indicator(see6.8). Titratewiththestan-dard disodium dihydrogen EDTA solution against a white backgroun
46、d to match a blankprepared in the same manner. Calculate the molarity of the calcium solution as follows:Molarity of calcium solution = MV30Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-DTL-11361E9where: M = molarity of the disodium dihydrogen
47、EDTA solution, andV = milliliters of disodium dihydrogen EDTA solution used4.4.4.6 Procedure. Weigh to the nearest milligram approximately 2 g of the specimen andtransfer to a 250 mL Erlenmeyer flask. Add 10 mL of water and 5 mL of concentrated hydro-chloricacidinsmallportions, beingcareful notto lo
48、seanyofthe specimenbyspattering.Whensolution is complete, dilute to about 25 mL. Filter the solution through medium-texture filterpaper intoa 250 mL beaker andwashthe filter paper andresidue withsmall potions of hotwa-ter,notexceedingatotalof50mL.Carefullyevaporatethefiltratetodryness.Dissolvetheresi-duein9mLofwater,add1mLofsulfuricacid(1to4)andcool.Slowlyadd90mL ofmethanol,stirring constantly. Allow the solution to stand for about 2 hours until the precipitation is com-plete. Filter through a porcelain filtering crucible. Transfer the last traces of precipitate to thefil
