EPA-METHOD-3010A

METHOD3010A1.0SCOPEANDAPPLICATION1.1Thisdigestionprocedureisusedforthepreparationofaqueoussamples,EPandmobility-procedureextracts,andwastesthatcontainsuspendedsolidsforanalysis,byflameatomicabsorptionspectroscopy(FLAA)orinductivelycoupledargonplasmaspectroscopy(ICP).Theprocedureisusedtodeterminetotalmetals.1.2SamplespreparedbyMethod3010maybeanalyzedbyFLAAorICPforthefollowing:Aluminum*ArsenicBariumBerylliumCadmiumCalciumChromiumCobaltCopperIronLead*AnalysisbyICPSeeMethod7760forthedigestionandFLAAanalysisofSilver.1.3Thisdigestionprocedureisnotsuitableforsampleswhichwillbeanalyzedbygraphitefurnaceatomicabsorptionspectroscopybecausehydrochloricacidcancauseinterferencesduringfurnaceatomization.ConsultMethod3020Aforsamplesrequiringgraphitefurnaceanalysis.MagnesiumManganeseMolybdenumNickelPotassium*SeleniumSodiumThalliumVanadiumZinc2.0SUMMARYOFMETHOD2.1AmixtureofnitricacidandthematerialtobeanalyzedisrefluxedinacoveredGriffinbeaker.Thisstepisrepeatedwithadditionalportionsofnitricaciduntilthedigestateislightincolororuntilitscolorhasstabilized.Afterthedigestatehasbeenbroughttoalowvolume,itisrefluxedwithhydrochloricacidandbroughtuptovolume.Ifsampleshouldgotodryness,itmustbediscardedandthesamplereprepared.3.0INTERFERENCES3.1Interferencesarediscussedinthereferringanalyticalmethod.CD-ROM3010A-1Revision14.0APPARATUSANDMATERIALS4.14.24.34.44.5Griffinbeakers-150-mLorequivalent.Watchglasses-Ribbedandplainorequivalent.Qualitativefilterpaperorcentrifugationequipment.Graduatedcylinderorequivalent-100mL.Funnelorequivalent.4.6Hotplateorequivalentheatingsource-adjustableandcapableofmaintainingatemperatureof90-95oC.5.0REAGENTS5.1Reagentgradechemicalsshallbeusedinalltests.Unlessotherwiseindicated,itisintendedthatallreagentsshallconformtothespecificationsoftheCommitteeonAnalyticalReagentsoftheAmericanChemicalSociety,wheresuchspecificationsareavailable.Othergradesmaybeused,provideditisfirstascertainedthatthereagentisofsufficientlyhighpuritytopermititsusewithoutlesseningtheaccuracyofthedetermination.5.2ReagentWater.Reagentwaterwillbeinterferencefree.Allreferencestowaterinthemethodrefertoreagentwaterunlessotherwisespecified.RefertoChapterOneforadefinitionofreagentwater.5.3Nitricacid(concentrated),HNO3.Acidshouldbeanalyzedtodeterminelevelsofimpurities.IfmethodblankisMDL,theacidcanbeused.5.4Hydrochloricacid(1:1),HCl.Preparedfromwaterandhydrochloricacid.Hydrochloricacidshouldbeanalyzedtodeterminelevelofimpurities.IfmethodblankisMDL,theacidcanbeused.6.0SAMPLECOLLECTION,PRESERVATION,ANDHANDLING6.1AllsamplesmusthavebeencollectedusingasamplingplanthataddressestheconsiderationsdiscussedinChapterNineofthismanual.6.2Allsamplecontainersmustbeprewashedwithdetergents,acids,andwater.Plasticandglasscontainersarebothsuitable.SeeChapterThree,Step3.1.3,forfurtherinformation.6.3AqueouswastewatersmustbeacidifiedtoapHof2withHNO3.7.0PROCEDURE7.1Transfera100-mLrepresentativealiquotofthewell-mixedsampletoa150-mLGriffinbeakerandadd3mLofconcentratedHNO3.CoverthebeakerwithCD-ROM3010A-2Revision1aribbedwatchglassorequivalent.Placethebeakeronahotplateorequivalentheatingsourceandcautiouslyevaporatetoalowvolume(5mL),makingcertainthatthesampledoesnotboilandthatnoportionofthebottomofthebeakerisallowedtogodry.Coolthebeakerandaddanother3-mLportionofconcentratedHNO3.Coverthebeakerwithanonribbedwatchglassandreturntothehotplate.Increasethetemperatureofthehotplatesothatagentlerefluxactionoccurs.Ifasampleisallowedtogotodryness,lowrecoverieswillresult.Shouldthisoccur,discardthesampleandreprepare.7.2Continueheating,addingadditionalacidasnecessary,untilthedigestioniscomplete(generallyindicatedwhenthedigestateislightincolorordoesnotchangeinappearancewithcontinuedrefluxing).Again,uncoverthebeakerorusearibbedwatchglass,andevaporatetoalowvolume(3mL),notallowinganyportionofthebottomofthebeakertogodry.Coolthebeaker.Addasmallquantityof1:1HCl(10mL/100mLoffinalsolution),coverthebeaker,andrefluxforanadditional15minutestodissolveanyprecipitateorresidueresultingfromevaporation.7.3Washdownthebeakerwallsandwatchglasswithwaterand,whennecessary,filterorcentrifugethesampletoremovesilicatesandotherinsolublematerialthatcouldclogthenebulizer.Filtrationshouldbedoneonlyifthereisconcernthatinsolublematerialsmayclogthenebulizer.Thisadditionalstepcancausesamplecontaminationunlessthefilterandfilteringapparatusarethoroughlycleaned.Rinsethefilterandfilterapparatuswithdilutenitricacidanddiscardtherinsate.Filterthesampleandadjustthefinalvolumeto100mLwithreagentwaterandthefinalacidconcentrationto10%.Thesampleisnowreadyforanalysis.8.0QUALITYCONTROLAllqualitycontrolmeasuresdescribedinChapterOneshouldbe8.1followed.8.2Foreachanalyticalbatchofsamplesprocessed,blanksshouldbecarriedthroughouttheentiresample-preparationandanalyticalprocess.Theseblankswillbeusefulindeterminingifsamplesarebeingcontaminated.RefertoChapterOnefortheproperprotocolwhenanalyzingblanks.8.3Replicatesamplesshouldbeprocessedonaroutinebasis.Areplicatesampleisasamplebroughtthroughthewholesamplepreparationandanalyticalprocess.Areplicatesampleshou