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1、METHOD3015MICROWAVEASSISTEDACIDDIGESTIONOFAQUEOUSSAMPLESANDEXTRACTS1.0SCOPEANDAPPLICATION1.1Thisdigestionprocedureisusedforthepreparationofaqueoussamples,mobility-procedureextracts,andwastesthatcontainsuspendedsolidsforanalysis,byflameatomicabsorptionspectroscopy(FLAA),gr
2、aphitefurnaceabsorptionspectroscopy(GFAA),inductivelycoupledargonplasmaspectroscopy(ICP),orinductivelycoupledargonplasmamassspectrometry(ICP-MS).Theprocedureisahotacidleachfordeterminingavailablemetals.Duetotherapidadvancesinmicrowavetechnology,consultyourmanufacturer'sre
3、commendedinstructionsforguidanceontheirmicrowavedigestionsystemandrefertotheSW-846"DISCLAIMER"whenconductinganalysesusingMethod3015.1.2SamplespreparedbyMethod3015usingnitricaciddigestionmaybeanalyzedbyFLAA,GFAA,ICP-AES,orICP-MSforthefollowing:AluminumLeadAntimonyMagnesium
4、Arsenic*ManganeseBariumMolybdenumBerylliumNickelCadmiumPotassiumCalciumSelenium*ChromiumSilverCobaltSodiumCopperThalliumIronVanadiumZinc*CannotbeanalyzedbyFLAA2.0SUMMARYOFMETHOD2.1Arepresentative45mLaqueoussampleisdigestedin5mLofconcentratednitricacidinafluorocarbon(PFAor
5、TFM)digestionvesselfor20minutesusingmicrowaveheating.Afterthedigestionprocess,thesampleiscooled,andthenfiltered,centrifuged,orallowedtosettleinacleansamplebottlepriortoanalysis.3.0INTERFERENCES3.1Manysamplesthatcontainorganics,suchasTCLPextracts,willresultinhighervesselpr
6、essureswhichhavethepotentialtocauseventingofthevessels.Ventingcanresultineitherlossofanalytesand/orsample,whichCD-ROM3015-1Revision0September1994mustbeavoided.Asmallersamplesizecanbeusedbutthefinalwatervolumepriortonitricacidadditionmustremainat45mL.Thisisrequiredtoretain
7、theheatcharacteristicsofthecalibrationprocedure.Limitsofquantitationwillchangewithsamplequantity(dilution)aswithinstrumentation."4.0APPARATUSANDMATERIALS4.1Microwaveapparatusrequirements4.1.1Themicrowaveunitprovidesprogrammablepowerwithaminimumof574W,whichcanbeprogrammedt
8、owithin+10Woftherequiredpower.Typicalunitsprovideanominal600Wto1200Wofpower.Temperaturemonitorin
