EPA-Method-1311-Toxicity-Characteristic-Leaching-P

CD-ROM1311-1Revision0July1992METHOD1311TOXICITYCHARACTERISTICLEACHINGPROCEDURE1.0SCOPEANDAPPLICATION1.1TheTCLPisdesignedtodeterminethemobilityofbothorganicandinorganicanalytespresentinliquid,solid,andmultiphasicwastes.1.2Ifatotalanalysisofthewastedemonstratesthatindividualanalytesarenotpresentinthewaste,orthattheyarepresentbutatsuchlowconcentrationsthattheappropriateregulatorylevelscouldnotpossiblybeexceeded,theTCLPneednotberun.1.3IfananalysisofanyoneoftheliquidfractionsoftheTCLPextractindicatesthataregulatedcompoundispresentatsuchhighconcentra-tionsthat,evenafteraccountingfordilutionfromtheotherfractionsoftheextract,theconcentrationwouldbeabovetheregulatorylevelforthatcompound,thenthewasteishazardousanditisnotnecessarytoanalyzetheremainingfractionsoftheextract.1.4Ifananalysisofextractobtainedusingabottleextractorshowsthattheconcentrationofanyregulatedvolatileanalyteexceedstheregulatorylevelforthatcompound,thenthewasteishazardousandextractionusingtheZHEisnotnecessary.However,extractfromabottleextractorcannotbeusedtodemonstratethattheconcentrationofvolatilecompoundsisbelowtheregulatorylevel.2.0SUMMARYOFMETHOD2.1Forliquidwastes(i.e.,thosecontaininglessthan0.5%drysolidmaterial),thewaste,afterfiltrationthrougha0.6to0.8µmglassfiberfilter,isdefinedastheTCLPextract.2.2Forwastescontaininggreaterthanorequalto0.5%solids,theliquid,ifany,isseparatedfromthesolidphaseandstoredforlateranalysis;theparticlesizeofthesolidphaseisreduced,ifnecessary.Thesolidphaseisextractedwithanamountofextractionfluidequalto20timestheweightofthesolidphase.Theextractionfluidemployedisafunctionofthealkalinityofthesolidphaseofthewaste.Aspecialextractorvesselisusedwhentestingforvolatileanalytes(seeTable1foralistofvolatilecompounds).Followingextraction,theliquidextractisseparatedfromthesolidphasebyfiltrationthrougha0.6to0.8µmglassfiberfilter.2.3Ifcompatible(i.e.,multiplephaseswillnotformoncombination),theinitialliquidphaseofthewasteisaddedtotheliquidextract,andtheseareanalyzedtogether.Ifincompatible,theliquidsareanalyzedseparatelyandtheresultsaremathematicallycombinedtoyieldavolume-weightedaverageconcentration.VITONisatrademarkofDuPont.1®CD-ROM1311-2Revision0July19923.0INTERFERENCES3.1Potentialinterferencesthatmaybeencounteredduringanalysisarediscussedintheindividualanalyticalmethods.4.0APPARATUSANDMATERIALS4.1Agitationapparatus:Theagitationapparatusmustbecapableofrotatingtheextractionvesselinanend-over-endfashion(seeFigure1)at30+2rpm.SuitabledevicesknowntoEPAareidentifiedinTable2.4.2ExtractionVessels4.2.1Zero-HeadspaceExtractionVessel(ZHE).Thisdeviceisforuseonlywhenthewasteisbeingtestedforthemobilityofvolatileanalytes(i.e.,thoselistedinTable1).TheZHE(depictedinFigure2)allowsforliquid/solidseparationwithinthedevice,andeffectivelyprecludesheadspace.Thistypeofvesselallowsforinitialliquid/solidseparation,extraction,andfinalextractfiltrationwithoutopeningthevessel(seeSection4.3.1).Thevesselsshallhaveaninternalvolumeof500-600mL,andbeequippedtoaccommodatea90-110mmfilter.ThedevicescontainVITONO-ringswhichshouldbereplacedfrequently.SuitableZHE®1devicesknowntoEPAareidentifiedinTable3.FortheZHEtobeacceptableforuse,thepistonwithintheZHEshouldbeabletobemovedwithapproximately15psiorless.Ifittakesmorepressuretomovethepiston,theO-ringsinthedeviceshouldbereplaced.Ifthisdoesnotsolvetheproblem,theZHEisunacceptableforTCLPanalysesandthemanufacturershouldbecontacted.TheZHEshouldbecheckedforleaksaftereveryextraction.Ifthedevicecontainsabuilt-inpressuregauge,pressurizethedeviceto50psi,allowittostandunattendedfor1hour,andrecheckthepressure.Ifthedevicedoesnothaveabuilt-inpressuregauge,pressurizethedeviceto50psi,submergeitinwater,andcheckforthepresenceofairbubblesescapingfromanyofthefittings.Ifpressureislost,checkallfittingsandinspectandreplaceO-rings,ifnecessary.Retestthedevice.Ifleakageproblemscannotbesolved,themanufacturershouldbecontacted.SomeZHEsusegaspressuretoactuatetheZHEpiston,whileothersusemechanicalpressure(seeTable3).Whereasthevolatilesprocedure(seeSection7.3)referstopoundspersquareinch(psi),forthemechanicallyactuatedpiston,thepressureappliedismeasuredintorque-inch-pounds.Refertothemanufacturer'sinstructionsastotheproperconversion.CD-ROM1311-3Revision0July19924.2.2BottleExtractionVessel.Whenthewasteisbeingevaluatedusingthenonvolatileextraction,ajarwithsufficientcapacitytoholdthesampleandtheextractionfluidisneeded.Headspaceisallowedinthisvessel.Theextractionbottlesmaybeconstructedfromvariousmaterials,dependingontheanalytestobeanalyzedandthenatureofthewaste(seeSection4.3.3).Itisrecommendedthatborosilicateglassbottlesbeusedinsteadofothertypesofglass,especiallywheninorganicsareofconcern.Plasticbottles,otherthanpolytetrafluoroethylene,shallnotbeusediforganicsaretobeinvestigated.Bottlesareavailablefromanumberoflaboratorysuppliers.Whenthistypeofextractionvesselisused,thefiltrationdevicediscussedinSection4.3.2isusedforinitialliquid/solidseparationandfinalextractfiltration.4.3FiltrationDevices:Itisrecommendedthatallfiltrationsbeperformedinahood.4.3.1Zero-HeadspaceExtrac