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1、METHOD9030BACID-SOLUBLEANDACID-INSOLUBLESULFIDES:DISTILLATION1.0SCOPEANDAPPLICATION1.1Thedistillationproceduredescribedinthismethodisdesignedforthedeterminationofsulfidesinaqueous,solidwastematerials,oreffluents.1.2Thismethodprovidesonlyasemi-quantitativedeterminationofsu
2、lfidecompoundsconsidered"acid-insoluble"(e.g.,CuSandSnS2)insolidsamples.Recoveryhasbeenshowntobe20to40%forCuS,oneofthemoststableandinsolublecompounds,and40to60%forSnS2whichisslightlymoresoluble.1.3Thismethodisnotapplicabletooilormultiphasicsamplesorsamplesnotamenabletothe
3、distillationprocedurewhichcanbeanalyzedbyMethod9031.1.4Method9030issuitableformeasuringsulfideconcentrationsinsampleswhichcontainbetween0.2and50mg/kgofsulfide.1.5Thismethodisnotapplicablefordistillingreactivesulfide.Method9034orMethod9215maybeusedtoquantifytheconcentratio
4、nofsulfidefromthereactivitytest.RefertoChapterSeven,Section7.3.4.1forthedeterminationofreactivesulfide.1.6Thismethodmeasurestotalsulfidewhichisusuallydefinedastheacid-solublefractionofawaste.If,however,onehaspreviousknowledgeofthewasteandisconcernedaboutbothsolublesulfide
5、ssuchasH2S,andmetalsulfides,suchasCuSandSnS2,thentotalsulfideisdefinedasthecombinationofbothacid-solubleandacid-insolublefractions.Forwasteswhereonlymetalsulfidesaresuspectedtobepresent,onlytheacid-insolublefractionneedstobeperformed.2.0SUMMARYOFMETHOD2.1Foracid-solublesu
6、lfidesamples,separationofsulfidefromthesamplematrixisaccomplishedbytheadditionofsulfuricacidtothesample.Thesampleisheatedto70ECandthehydrogensulfide(H2S)whichisformedisdistilledunderacidicconditionsandcarriedbyanitrogenstreamintozincacetategasscrubbingbottleswhereitisprec
7、ipitatedaszincsulfide.2.2Foracid-insolublesulfidesamples,separationofsulfidefromthesamplematrixisaccomplishedbysuspendingthesampleinconcentratedhydrochloricacidbyvigorousagitation.Tin(II)chlorideispresenttopreventoxidationofsulfidetosulfurbythemetalion(asincopper(II)),byt
8、hematrix,orbydissolvedoxygeninthereagents.Thepreparedsampleisdistilledunderacidicconditionsat100
