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1、METHOD3050BACIDDIGESTIONOFSEDIMENTS,SLUDGES,ANDSOILS1.0SCOPEANDAPPLICATION1.1Thismethodhasbeenwrittentoprovidetwoseparatedigestionprocedures,oneforthepreparationofsediments,sludges,andsoilsamplesforanalysisbyflameatomicabsorptionspectrometry(FLAA)orinductivelycoupledplasma
2、atomicemissionspectrometry(ICP-AES)andoneforthepreparationofsediments,sludges,andsoilsamplesforanalysisofsamplesbyGraphiteFurnaceAA(GFAA)orinductivelycoupledplasmamassspectrometry(ICP-MS).Theextractsfromthesetwoproceduresarenotinterchangeableandshouldonlybeusedwiththeanaly
3、ticaldeterminationsoutlinedinthissection.SamplespreparedbythismethodmaybeanalyzedbyICP-AESorGFAAforallthelistedmetalsaslongasthedetecionlimitsareadequatefortherequiredend-useofthedata.AlternativedeterminativetechniquesmaybeusediftheyarescientificallyvalidandtheQCcriteriaof
4、themethod,includingthosedealingwithinterferences,canbeachieved.Otherelementsandmatricesmaybeanalyzedbythismethodifperformanceisdemonstratedfortheanalytesofinterest,inthematricesofinterest,attheconcentrationlevelsofinterest(SeeSection8.0).Therecommendeddeterminativetechniqu
5、esforeachelementarelistedbelow:FLAA/ICP-AESGFAA/ICP-MSAluminumMagnesiumArsenicAntimonyManganeseBerylliumBariumMolybdenumCadmiumBerylliumNickelChromiumCadmiumPotassiumCobaltCalciumSilverIronChromiumSodiumLeadCobaltThalliumMolybdenumCopperVanadiumSeleniumIronZincThalliumLead
6、Vanadium1.2Thismethodisnotatotaldigestiontechniqueformostsamples.Itisaverystrongaciddigestionthatwilldissolvealmostallelementsthatcouldbecomeenvironmentallyavailable.Bydesign,elementsboundinsilicatestructuresarenotnormallydissolvedbythisprocedureastheyarenotusuallymobilein
7、theenvironment.IfabsolutetotaldigestionisrequireduseMethod3052.2.0SUMMARYOFMETHOD2.1Forthedigestionofsamples,arepresentative1-2gram(wetweight)or1gram(dryweight)sampleisdigestedwithrepeatedadditionsofnitricacid(HNO3)andhydrogenperoxide(H2O2).2.2ForGFAAorICP-MSanalysis,there
8、sultantdigestateisreducedinvolumewhileheatingandthendilutedtoafinalvolumeof100mL.2.3ForIC