TCLP (EPA Test Method 1311)

来源：华拓科技网

EPATestMethod1311-TCLP,

ToxicityCharacteristicLeachingProcedure

TheTCLP,orToxicityCharacteristicLeaching(notLeachate)Procedureisdesignedtodeterminethemobilityofbothorganicandinorganicanalytespresentinliquid,solid,andmultiphasicwastes.ThisisusuallyusedtodetermineifawastemaymeetthedefinitionofEPToxicity,thatis,carryingahazardouswastecodeunderRCRA(40CFRPart261)ofD004throughD052.Asitisthegenerator'sresponsibilitytomakethisdetermination,butgeneratorsoftencontractoutsidelabstoperformtheTCLPtest,thesequestionsandanswersmaybehelpfultogenerators.Forthisreasonand

sometimesincleanupactions,businessesareoftenaskedtoperformananalysisontheirwasteusingtheTCLP.TheCodeofFederalRegulations(CFR)

40CFR§261.24,outlinesthe40contaminantstheTCLPanalysistestsfor(SeeTable1—MaximumConcentrationofContaminantsforToxicityCharacteristic). If a “Solid Waste” fails the test foroneormoreofthesecompounds,thewasteisconsideredtobeacharacteristichazardouswaste–unlessthereisanexemptionthatapplies.Bearinmind,too,thatacharacteristicwastemaystillalsobea “listed” hazardous waste.Theprocedurefollowsbelow.Formoregeneralinformation,FAQsandguidances,seewww.ehso.com/

1.0SCOPEANDAPPLICATION

1.1

TheTCLPisdesignedtodeterminethemobilityofbothorganicandinorganicanalytespresentinliquid,solid,andmultiphasicwastes.

Ifatotalanalysisofthewastedemonstratesthatindividualanalytesarenotpresentinthewaste,orthattheyarepresentbutatsuchlowconcentrationsthattheappropriateregulatorylevelscouldnotpossiblybeexceeded,theTCLPneednotberun.

IfananalysisofanyoneoftheliquidfractionsoftheTCLPextractindicatesthataregulatedcompoundispresentatsuchhighconcentrationsthat,evenafteraccountingfordilutionfromtheotherfractionsoftheextract,theconcentrationwouldbeabovetheregulatorylevelforthatcompound,thenthewasteishazardousanditisnotnecessarytoanalyzetheremainingfractionsoftheextract.

Ifananalysisofextractobtainedusingabottleextractorshowsthattheconcentrationofanyregulatedvolatileanalyteexceedstheregulatorylevelforthatcompound,thenthewasteishazardousandextractionusingtheZHEisnotnecessary.However,extractfromabottleextractorcannotbeusedtodemonstratethattheconcentrationofvolatilecompoundsisbelowtheregulatorylevel.

SUMMARYOFMETHOD

2.1Forliquidwastes(i.e.,thosecontaininglessthan0.5%dry

solidmaterial),thewaste,afterfiltrationthrougha0.6to

1.2

1.3

1.4

2.0

Page1of38TCLP;Method1311-1Revision0July1992

Providedbywww.ehso.com-EnvironmentalHealth&SafetyOnlineSeeEHSOforguidanceandresourcesthatisfreeandeasytofind

EPATestMethod1311-TCLP,

ToxicityCharacteristicLeachingProcedure

0.8µmglassfiberfilter,isdefinedastheTCLPextract.

2.2Forwastescontaininggreaterthanorequalto0.5%solids,the

liquid,ifany,isseparatedfromthesolidphaseandstoredforlateranalysis;theparticlesizeofthesolidphaseisreduced,ifnecessary.Thesolidphaseisextractedwithanamountofextractionfluidequalto20timestheweightofthesolidphase.Theextractionfluidemployedisafunctionofthealkalinityofthesolidphaseofthewaste.Aspecialextractorvesselisusedwhentestingforvolatileanalytes(seeTable1foralistofvolatilecompounds).Followingextraction,theliquidextractisseparatedfromthesolidphasebyfiltrationthrougha0.6to0.8µmglassfiberfilter.2.3

Ifcompatible(i.e.,multiplephaseswillnotformoncombination),theinitialliquidphaseofthewasteisaddedtotheliquidextract,andtheseareanalyzedtogether.Ifincompatible,theliquidsareanalyzedseparatelyandtheresultsaremathematicallycombinedtoyieldavolume-weightedaverageconcentration.

3.0INTERFERENCES

3.1

Potentialinterferencesthatmaybeencounteredduringanalysisarediscussedintheindividualanalyticalmethods.

4.0APPARATUSANDMATERIALS

4.1Agitationapparatus:Theagitationapparatusmustbecapableof

rotatingtheextractionvesselinanend-over-endfashion(seeFigure1)at30+2rpm.SuitabledevicesknowntoEPAareidentifiedinTable2.4.2

ExtractionVessels

4.2.1Zero-HeadspaceExtractionVessel(ZHE).Thisdeviceis

foruseonlywhenthewasteisbeingtestedforthemobilityofvolatileanalytes(i.e.,thoselistedinTable1).TheZHE(depictedinFigure2)allowsforliquid/solidseparationwithinthedevice,andeffectivelyprecludesheadspace.Thistypeofvesselallowsforinitialliquid/solidseparation,extraction,andfinalextractfiltrationwithoutopeningthevessel(seeSection4.3.1).Thevesselsshallhaveaninternalvolumeof500-600mL,andbeequippedtoaccommodatea90-110mmfilter.ThedevicescontainVITONO-ringswhichshouldbereplacedfrequently.SuitableZHEdevicesknowntoEPAareidentifiedinTable3.

ForthetheZHEpsiorpiston,

ZHEtobeacceptableforuse,thepistonwithinshouldbeabletobemovedwithapproximately15less.IfittakesmorepressuretomovethetheO-ringsinthedeviceshouldbereplaced.If

Page2of38TCLP;Method1311-2Revision0July1992

Providedbywww.ehso.com-EnvironmentalHealth&SafetyOnlineSeeEHSOforguidanceandresourcesthatisfreeandeasytofind

EPATestMethod1311-TCLP,

ToxicityCharacteristicLeachingProcedure

thisdoesnotsolvetheproblem,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.1®VITONisatrademarkofDuPont.CD-ROM1311-2

4.2.2

BottleExtractionVessel.Whenthewasteisbeingevaluatedusingthenonvolatileextraction,ajarwithsufficientcapacitytoholdthesampleandtheextractionfluidisneeded.Headspaceisallowedinthisvessel.Theextractionbottlesmaybeconstructedfromvariousmaterials,dependingontheanalytestobeanalyzedandthenatureofthewaste(seeSection4.3.3).Itisrecommendedthatborosilicateglassbottlesbeusedinsteadofothertypesofglass,especiallywheninorganicsareofconcern.Plasticbottles,otherthanpolytetrafluoroethylene,shallnotbeusediforganicsaretobeinvestigated.Bottlesareavailablefromanumberoflaboratorysuppliers.Whenthistypeofextractionvesselisused,thefiltrationdevicediscussedinSection4.3.2isusedforinitialliquid/solidseparationandfinalextractfiltration.

4.3

FiltrationDevices:Itisrecommendedthatallfiltrationsbeperformedinahood.

4.3.1Zero-HeadspaceExtractorVessel(ZHE):Whenthewasteis

evaluatedforvolatiles,thezero-headspaceextractionvesseldescribedinSection4.2.1isusedforfiltration.Thedeviceshallbecapableofsupportingandkeepinginplacetheglassfiberfilterandbeabletowithstandthepressureneededtoaccomplishseparation(50psi).

NOTE:Whenitissuspectedthattheglassfiberfilter

Page3of38TCLP;Method1311-3Revision0July1992

Providedbywww.ehso.com-EnvironmentalHealth&SafetyOnlineSeeEHSOforguidanceandresourcesthatisfreeandeasytofind

EPATestMethod1311-TCLP,

ToxicityCharacteristicLeachingProcedure

hasbeenruptured,anin-lineglassfiberfiltermaybeusedtofilterthematerialwithintheZHE.

4.3.2FilterHolder:Whenthewasteisevaluatedforother

thanvolatileanalytes,anyfilterholdercapableofsupportingaglassfiberfilterandabletowithstandthepressureneededtoaccomplishseparationmaybeused.Suitablefilterholdersrangefromsimplevacuumunitstorelativelycomplexsystemscapableofexertingpressuresofupto50psiormore.Thetypeoffilterholderuseddependsonthepropertiesofthematerialtobefiltered(seeSection4.3.3).Thesedevicesshallhaveaminimuminternalvolumeof300mLandbeequippedtoaccommodateaminimumfiltersizeof47mm(filterholdershavinganinternalcapacityof1.5Lorgreater,andequippedtoaccommodatea142mmdiameterfilter,arerecommended).Vacuumfiltrationcanonlybeusedforwasteswithlowsolidscontent(<10%)andforhighlygranular,liquid-containingwastes.Allothertypesofwastesshouldbefilteredusingpositivepressurefiltration.SuitablefilterholdersknowntoEPAareshowninTable4.4.3.3

MaterialsofConstruction:Extractionvesselsandfiltrationdevicesshallbemadeofinertmaterialswhichwillnotleachorabsorbwastecomponents.Glass,polytetrafluoroethylene(PTFE),ortype316stainlesssteelequipmentmaybeusedwhenevaluatingthemobilityofbothorganicandinorganiccomponents.Devicesmadeofhighdensitypolyethylene(HDPE),polypropylene(PP),orpolyvinylchloride(PVC)maybeusedonlywhenevaluatingthemobilityofmetals.Borosili-categlassbottlesarerecommendedforuseoverothertypesofglassbottles,especiallywheninorganicsareanalytesofconcern.

4.4

Filters:Filtersshallbemadeofborosilicateglassfiber,shallcontainnobindermaterials,andshallhaveaneffectiveporesizeof0.6to0.8µm,orequivalent.FiltersknowntoEPAwhichmeetthesespecificationsareidentifiedinTable5.Pre-filtersmustnotbeused.Whenevaluatingthemobilityofmetals,filtersshallbeacid-washedpriortousebyrinsingwith1Nnitricacidfollowedbythreeconsecutiverinseswithdeionizeddistilledwater(aminimumof1Lperrinseisrecommended).Glassfiberfiltersarefragileandshouldbehandledwithcare.

pHMeters:Themetershouldbeaccurateto+0.05unitsat25

4.5

®2

4.6

ZHEExtractCollectionDevices:TEDLARbagsorglass,stainlesssteelorPTFEgas-tightsyringesareusedtocollect

Page4of38TCLP;Method1311-4Revision0July1992

Providedbywww.ehso.com-EnvironmentalHealth&SafetyOnlineSeeEHSOforguidanceandresourcesthatisfreeandeasytofind

EPATestMethod1311-TCLP,

ToxicityCharacteristicLeachingProcedure

theinitialliquidphaseandthefinalextractofthewastewhenusingtheZHEdevice.Thedeviceslistedarerecommendedforuseunderthefollowingconditions:4.6.1

Ifawastecontainsanaqueousliquidphaseorifawastedoesnotcontainasignificantamountofnonaqueousliquid(i.e.,<1%oftotalwaste),theTEDLARbagora600mLsyringeshouldbeusedtocollectandcombinetheinitialliquidandsolidextract.

Ifawastecontainsasignificantamountof

nonaqueousliquidintheinitialliquidphase(i.e.,>1%oftotalwaste),thesyringeortheTEDLARbagmaybeusedforboththeinitialsolid/liquidseparationandthefinalextractfiltration.However,analystsshoulduseoneortheother,notboth.

Ifthewastecontainsnoinitialliquidphase(is100%solid)orhasnosignificantsolidphase(is100%liquid),eithertheTEDLARbagorthesyringemaybeused.Ifthesyringeisused,discardthefirst5mLofliquidexpressedfromthedevice.Theremainingaliquotsareusedforanalysis.

4.6.2

4.6.3

4.7ZHEExtractionFluidTransferDevices:Anydevicecapableof

transferringtheextractionfluidintotheZHEwithoutchangingthenatureoftheextractionfluidisacceptable(e.g.,apositivedisplacementorperistalticpump,agastightsyringe,pressurefiltrationunit(seeSection4.3.2),orotherZHEdevice).4.8

LaboratoryBalance:Anylaboratorybalanceaccuratetowithin+0.01gramsmaybeused(allweightmeasurementsaretobewithin+0.1grams).

BeakerorErlenmeyerflask,glass,500mL.2

4.9

TEDLARisaregisteredtrademarkofDuPont.

4.104.11

Watchglass,appropriatediametertocoverbeakerorErlenmeyerflask.

Magneticstirrer.

Reagents

5.1

Reagentgradechemicalsshallbeusedinalltests.Unlessotherwiseindicated,itisintendedthatallreagentsshallconformtothespecificationsoftheCommitteeonAnalyticalReagentsoftheAmericanChemicalSociety,wheresuchspecificationsareavailable.Othergradesmaybeused,provideditisfirstascertainedthatthereagentisof

Page5of38TCLP;Method1311-5Revision0July1992

Providedbywww.ehso.com-EnvironmentalHealth&SafetyOnlineSeeEHSOforguidanceandresourcesthatisfreeandeasytofind

EPATestMethod1311-TCLP,

ToxicityCharacteristicLeachingProcedure

sufficientlyhighpuritytopermititsusewithoutlesseningtheaccuracyofthedetermination.5.2

ReagentWater.Reagentwaterisdefinedaswaterinwhichaninterferantisnotobservedatorabovethemethod'sdetectionlimitoftheanalyte(s)ofinterest.Fornonvolatileextractions,ASTMTypeIIwaterorequivalentmeetsthedefinitionofreagentwater.Forvolatileextractions,itisrecommendedthatreagentwaterbegeneratedbyanyofthefollowingmethods.Reagentwatershouldbemonitoredperiodicallyforimpurities.

5.2.1Reagentwaterforvolatileextractionsmaybegenerated

bypassingtapwaterthroughacarbonfilterbedcontainingabout500gramsofactivatedcarbon(CalgonCorp.,Filtrasorb-300orequivalent).5.2.2

Awaterpurificationsystem(MilliporeSuper-Qorequivalent)mayalsobeusedtogeneratereagentwaterforvolatileextractions.

Reagentwaterforvolatileextractionsmayalsobepreparedbyboilingwaterfor15minutes.Subsequently,whilemaintainingthewatertemperatureat90+5degreesC,bubbleacontaminant-freeinertgas(e.g.nitrogen)throughthewaterfor1hour.Whilestillhot,transferthewatertoanarrowmouthscrew-capbottleunderzero-headspaceandsealwithaTeflon-linedseptumandcap.

5.2.3

5.35.45.55.65.7

Hydrochloricacid(1N),HCl,madefromACSreagentgrade.Nitricacid(1N),HNO

madefromACSreagentgrade.

Sodiumhydroxide(1N),NaOH,madefromACSreagentgrade.Glacialaceticacid,Extractionfluid.

5.7.1Extractionfluid#1:Add5.7mLglacialCH32CHOOHto

500mLofreagentwater(SeeSection5.2),add.3mLof1NNaOH,anddilutetoavolumeof1liter.Whencorrectlyprepared,thepHofthisfluidwillbe4.93+0.05.

5.7.2Extractionfluid#2:Dilute5.7mLglacialCH32CHOOHwith

reagentwater(SeeSection5.2)toavolumeof1liter.Whencorrectlyprepared,thepHofthisfluidwillbe2.88+0.05.NOTE:Theseextractionfluidsshouldbemonitoredfrequently

forimpurities.ThepHshouldbecheckedpriortousetoensurethatthesefluidsaremadeupaccurately.IfimpuritiesarefoundorthepHisnotwithintheabove

CH32CHOOH,ACSreagentgrade.

Page6of38TCLP;Method1311-6Revision0July1992

Providedbywww.ehso.com-EnvironmentalHealth&SafetyOnlineSeeEHSOforguidanceandresourcesthatisfreeandeasytofind

EPATestMethod1311-TCLP,

ToxicityCharacteristicLeachingProcedure

specifications,thefluidshallbediscardedandfreshextractionfluidprepared.

5.8

Analyticalstandardsshallbepreparedaccordingtotheappropriate

analyticalmethod.

6.0SAMPLECOLLECTION,PRESERVATION,ANDHANDLING

6.16.2

Allsamplesshallbecollectedusinganappropriatesamplingplan.

TheTCLPmayplacerequirementsontheminimalsizeofthefieldsample,dependinguponthephysicalstateorstatesofthewasteandtheanalytesofconcern.Analiquotisneededforpreliminaryevaluationofwhichextractionfluidistobeusedforthenonvolatileanalyteextractionprocedure.Anotheraliquotmaybeneededtoactuallyconductthenonvolatileextraction(seeSection1.4concerningtheuseofthisextractforvolatileorganics).Ifvolatileorganicsareofconcern,anotheraliquotmaybeneeded.Qualitycontrolmeasuresmayrequireadditionalaliquots.Further,itisalwayswisetocollectmoresamplejustincasesomethinggoeswrongwiththeinitialattempttoconductthetest.

Preservativesshallnotbeaddedtosamplesbeforeextraction.Samplesmayberefrigeratedunlessrefrigerationresultsinirreversiblephysicalchangetothewaste.Ifprecipitationoccurs,theentiresample(includingprecipitate)shouldbeextracted.

Whenthewasteistobeevaluatedforvolatileanalytes,careshallbetakentominimizethelossofvolatiles.Samplesshallbecollectedandstoredinamannerintendedtopreventthelossofvolatileanalytes(e.g.,samplesshouldbecollectedinTeflon-linedseptumcappedvialsandstoredat4EC.Samplesshouldbeopenedonlyimmediatelypriortoextraction).

6.36.4

6.5

6.6TCLPextractsshouldbepreparedforanalysisandanalyzedas

soonaspossiblefollowingextraction.ExtractsorportionsofextractsformetallicanalytedeterminationsmustbeacidifiedwithnitricacidtoapH<2,unlessprecipitationoccurs(seeSection7.2.14ifprecipitationoccurs).Extractsshouldbepreservedforotheranalytesaccordingtotheguidancegivenintheindividualanalysismethods.Extractsorportionsofextractsfororganicanalytedeterminationsshallnotbeallowedtocomeintocontactwiththeatmosphere(i.e.,noheadspace)topreventlosses.SeeSection8.0(QA

requirements)foracceptablesampleandextractholdingtimes.

7.0PROCEDURE

Page7of38TCLP;Method1311-7Revision0July1992

Providedbywww.ehso.com-EnvironmentalHealth&SafetyOnlineSeeEHSOforguidanceandresourcesthatisfreeandeasytofind

EPATestMethod1311-TCLP,

ToxicityCharacteristicLeachingProcedure

7.1

PreliminaryEvaluations

PerformpreliminaryTCLPevaluationsonaminimum100gramaliquotofwaste.ThisaliquotmaynotactuallyundergoTCLPextraction.Thesepreliminaryevaluationsinclude:(1)determinationofthepercentsolids(Section7.1.1);(2)determinationofwhetherthewastecontainsinsignificantsolidsandis,therefore,itsownextractafterfiltration(Section7.1.2);(3)determinationofwhetherthesolidportionofthewasterequiresparticlesizereduction(Section7.1.3);and(4)determinationofwhichofthetwoextractionfluidsaretobeusedforthenonvolatileTCLPextractionofthewaste(Section7.1.4).7.1.1

Preliminarydeterminationofpercentsolids:Percentsolidsisdefinedasthatfractionofawastesample(asapercentageofthetotalsample)fromwhichnoliquidmaybeforcedoutbyanappliedpressure,asdescribedbelow.7.1.1.1Ifthewastewillobviouslyyieldnoliquidwhen

subjectedtopressurefiltration(i.e.,is100%solids)proceedtoSection7.1.3.

7.1.1.2Ifthesampleisliquidormultiphasic,

liquid/solidseparationtomakeapreliminarydeterminationofpercentsolidsisrequired.ThisinvolvesthefiltrationdevicedescribedinSection4.3.2andisoutlinedinSections7.1.1.3through7.1.1.9.7.1.1.3Pre-weighthefilterandthecontainerthat

will

receivethefiltrate.7.1.1.4

Assemblethefilterholderandfilterfollowingthemanufacturer'sinstructions.Placethefilteronthesupportscreenandsecure.

7.1.1.5Weighoutasubsampleofthewaste(100gram

minimum)andrecordtheweight.7.1.1.6Allowslurriestostandtopermitthesolid

phasetosettle.Wastesthatsettleslowlymaybecentrifugedpriortofiltration.Centrifugationistobeusedonlyasanaidtofiltration.Ifused,theliquidshouldbedecantedandfilteredfollowedbyfiltrationofthesolidportionofthewastethroughthesamefiltrationsystem.7.1.1.7Quantitativelytransferthewastesampleto

thefilterholder(liquidandsolidphases).

Page8of38TCLP;Method1311-8Revision0July1992

Providedbywww.ehso.com-EnvironmentalHealth&SafetyOnlineSeeEHSOforguidanceandresourcesthatisfreeandeasytofind

EPATestMethod1311-TCLP,

ToxicityCharacteristicLeachingProcedure

Spreadthewastesampleevenlyoverthesurfaceofthefilter.Iffiltrationofthewasteat4ECreducestheamountofexpressedliquidoverwhatwouldbeexpressedatroomtemperaturethenallowthesampletowarmuptoroomtemperatureinthedevicebeforefiltering.NOTE:

Ifwastematerial(>1%oforiginalsampleweight)hasobviouslyadheredtothecontainerusedtotransferthesampletothefiltrationapparatus,determinetheweightofthisresidueandsubtractitfromthesampleweightdeterminedinSection7.1.1.5todeterminetheweightofthewastesamplethatwillbefiltered.

Graduallyapplyvacuumorgentlepressureof1-10psi,untilairorpressurizinggasmovesthroughthefilter.Ifthispointisnotreachedunder10psi,andifnoadditionalliquidhaspassedthroughthefilterinany2minuteinterval,slowlyincreasethepressurein10psiincrementstoamaximumof50psi.Aftereachincrementalincreaseof10psi,ifthepressurizinggashasnotmovedthroughthefilter,andifnoadditionalliquidhaspassedthroughthefilterinany2minuteinterval,proceedtothenext10psiincrement.Whenthepressurizinggasbeginstomovethroughthefilter,orwhenliquidflowhasceasedat50psi(i.e.,filtrationdoesnotresultinanyadditionalfiltratewithinany2minuteperiod),stopthefiltration.

NOTE:

Instantaneousapplicationofhighpressurecandegradetheglassfiberfilterandmaycauseprematureplugging.

7.1.1.8Thematerialinthefilterholderisdefined

asthesolidphaseofthewaste,andthefiltrateisdefinedastheliquidphase.

NOTE:Somewastes,suchas

somepaintwastes,containsomematerialbealiquid.Even

oilywastesandwillobviouslythatappearstoafterapplying

Page9of38TCLP;Method1311-9Revision0July1992

Providedbywww.ehso.com-EnvironmentalHealth&SafetyOnlineSeeEHSOforguidanceandresourcesthatisfreeandeasytofind

EPATestMethod1311-TCLP,

ToxicityCharacteristicLeachingProcedure

vacuumorpressurefiltration,asoutlinedinSection7.1.1.7,thismaterialmaynotfilter.Ifthisisthecase,thematerialwithinthefiltrationdeviceisdefinedasasolid.Donotreplacetheoriginalfilterwithafreshfilterunderanycircumstances.Useonlyonefilter.

7.1.1.9Determinetheweightoftheliquidphaseby

subtractingtheweightofthefiltratecontainer(seeSection7.1.1.3)fromthetotalweightofthefiltrate-filledcontainer.Determinetheweightofthesolidphaseofthewastesamplebysubtractingtheweightoftheliquidphasefromtheweightofthetotalwastesample,asdeterminedinSection7.1.1.5or7.1.1.7.

Recordtheweightoftheliquidandsolid

phases.Calculatethepercentsolidsasfollows:

Weightofsolid(Section7.1.1.9)

Percentsolids=____________________________________________________x100

Totalweightofwaste(Section7.1.1.5or7.1.1.7)

7.1.2

IfthepercentsolidsdeterminedinSection7.1.1.9is

equaltoorgreaterthan0.5%,thenproceedeithertoSection7.1.3todeterminewhetherthesolidmaterialrequiresparticlesizereductionortoSection7.1.2.1ifitisnoticedthatasmallamountofthefiltrateisentrainedinwettingofthefilter.IfthepercentsolidsdeterminedinSection7.1.1.9islessthan0.5%,thenproceedtoSection7.2.9ifthe

nonvolatileTCLPistobeperformedandtoSection7.3withafreshportionofthewasteifthevolatileTCLPistobeperformed.7.1.2.17.1.2.2

Removethesolidphaseandfilterfromthefiltrationapparatus.

Drythefilterandsolidphaseat100+20E

Cuntiltwosuccessiveweighingyieldthesamevaluewithin+1%.Recordthefinalweight.NOTE:

Cautionshouldbetakentoensurethatthesubjectsolidwillnotflashuponheating.Itisrecommendedthatthedryingovenbe

Page10of38TCLP;Method1311-10Revision0July1992

Providedbywww.ehso.com-EnvironmentalHealth&SafetyOnlineSeeEHSOforguidanceandresourcesthatisfreeandeasytofind

EPATestMethod1311-TCLP,

ToxicityCharacteristicLeachingProcedure

ventedtoahoodappropriatedevice.

other

7.1.2.3Calculatethepercentdrysolidsasfollows:

(Wt.ofdrywaste+filter)-taredwt.offilter

Percentdrysolids=100

Initialwt.ofwaste(Section7.1.1.5or7.1.1.7)

7.1.2.4

Ifthepercentdrysolidsislessthan0.5%,thenproceedtoSection7.2.9ifthenonvolatileTCLPistobeperformed,andtoSection7.3ifthevolatileTCLPistobeperformed.Ifthepercentdrysolidsisgreaterthanorequalto0.5%,andifthenonvolatileTCLPistobeperformed,returntothebeginningofthisSection(7.1)and,withafreshportionofwaste,determinewhetherparticlesizereductionisnecessary(Section7.1.3)anddeterminetheappropriateextractionfluid(Section7.1.4).IfonlythevolatileTCLPistobeperformed,seethenoteinSection7.1.4.

7.1.3

Determinationofwhetherthewasterequiresparticlesizereduction(particlesizeisreducedduringthisstep):Usingthesolidportionofthewaste,evaluatethesolidforparticlesize.Particlesizereductionisrequired,unlessthesolidhasasurfaceareapergramofmaterialequaltoorgreaterthan3.1cm,orissmallerthan1cminitsnarrowestdimension(i.e.,iscapableofpassingthrougha9.5mm(0.375inch)standardsieve).Ifthesurfaceareaissmallerortheparticlesizelargerthandescribedabove,preparethesolidportionofthewasteforextractionbycrushing,cutting,orgrindingthewastetoasurfaceareaorparticlesizeasdescribedabove.Ifthesolidsarepreparedfororganicvolatilesextraction,specialprecautionsmustbetaken(seeSection7.3.6).

NOTE:Surfaceareacriteriaremeantforfilamentous

(e.g.,paper,cloth,andsimilar)wastematerials.Actualmeasurementofsurfaceareaisnotrequired,norisitrecommended.Formaterialsthatdonotobviouslymeetthecriteria,samplespecificmethodswouldneedtobedevelopedandemployedtomeasurethesurfacearea.Suchmethodologyiscurrentlynotavailable.

Page11of38TCLP;Method1311-11Revision0July1992

Providedbywww.ehso.com-EnvironmentalHealth&SafetyOnlineSeeEHSOforguidanceandresourcesthatisfreeandeasytofind

EPATestMethod1311-TCLP,

ToxicityCharacteristicLeachingProcedure

7.1.4

Determinationofappropriateextractionfluid:Ifthesolidcontentofthewasteisgreaterthanorequalto0.5%andifthesamplewillbeextractedfornonvolatileconstituents(Section7.2),determinetheappropriatefluid(Section5.7)forthenonvolatilesextractionasfollows:

NOTE:TCLPextractionforvolatileconstituentsusesonlyextraction7.1.4.1Weighoutasmallsubsampleofthesolidphase

ofthewaste,reducethesolid(ifnecessary)toaparticlesizeofapproximately1mmindiameterorless,andtransfer5.0gramsofthesolidphaseofthewastetoa500mLbeakerorErlenmeyerflask.7.1.4.2

Add96.5mLofreagentwatertothebeaker,coverwithawatchglass,andstirvigorouslyfor5minutesusingamagneticstirrer.MeasureandrecordthepH.IfthepHis<5.0,useextractionfluid#1.ProceedtoSection7.2.

7.1.4.3IfthepHfromSection7.1.4.2is>5.0,add3.5

mL1NHCl,slurrybriefly,coverwithawatchglass,heatto50EC,andholdat50ECfor10minutes.7.1.4.4Letthesolutioncooltoroomtemperatureand

recordthepH.IfthepHis<5.0,useextractionfluid#1.IfthepHis>5.0,useextractionfluid#2.ProceedtoSection7.2.

7.1.5Ifthealiquotofthewasteusedforthepreliminary

evaluation(Sections7.1.1-7.1.4)wasdeterminedtobe100%solidatSection7.1.1.1,thenitcanbeusedfortheSection7.2extraction(assumingatleast100gramsremain),andtheSection7.3extraction(assumingatleast25gramsremain).IfthealiquotwassubjectedtotheprocedureinSection7.1.1.7,thenanotheraliquotshallbeusedforthevolatileextractionprocedureinSection7.3.ThealiquotofthewastesubjectedtotheprocedureinSection7.1.1.7mightbeappropriateforusefortheSection7.2extractionifanadequateamountofsolid(asdeterminedbySection7.1.1.9)wasobtained.Theamountofsolidnecessaryisdependentuponwhetherasufficientamountofextractwillbeproducedtosupporttheanalyses.Ifanadequateamountofsolidremains,proceedtoSection7.2.10ofthenonvolatileTCLPextraction.

7.2

ProcedureWhenVolatilesarenotInvolved

Aminimumsamplesizeof100grams(solidandliquidphases)is

Page12of38TCLP;Method1311-12Revision0July1992

Providedbywww.ehso.com-EnvironmentalHealth&SafetyOnlineSeeEHSOforguidanceandresourcesthatisfreeandeasytofind

EPATestMethod1311-TCLP,

ToxicityCharacteristicLeachingProcedure

recommended.Insomecases,alargersamplesizemaybeappropriate,dependingonthesolidscontentofthewastesample(percentsolids,SeeSection7.1.1),whethertheinitialliquidphaseofthewastewillbemisciblewiththeaqueousextractofthesolid,andwhetherinorganics,semivolatileorganics,pesticides,andherbicidesareallanalytesofconcern.EnoughsolidsshouldbegeneratedforextractionsuchthatthevolumeofTCLPextractwillbesufficienttosupportalloftheanalysesrequired.IftheamountofextractgeneratedbyasingleTCLPextractionwillnotbesufficienttoperformalloftheanalyses,morethanoneextractionmaybeperformedandtheextractsfromeachcombinedandaliquotedforanalysis.

7.2.1Ifthewastewillobviouslyyieldnoliquidwhensubjected

topressurefiltration(i.e.,is100%solid,seeSection7.1.1),weighoutasubsampleofthewaste(100gramminimum)andproceedtoSection7.2.9.7.2.2Ifthesampleisliquidormultiphasic,liquid/solid

separationisrequired.ThisinvolvesthefiltrationdevicedescribedinSection4.3.2andisoutlinedinSections7.2.3to7.2.8.7.2.3Pre-weighthecontainerthatwillreceivethefiltrate.7.2.4Assemblethefilterholderandfilterfollowingthe

manufacturer'sinstructions.Placethefilteronthesupportscreenandsecure.Acidwashthefilterifevaluatingthemobilityofmetals(seeSection4.4).

NOTE:Acidwashedfiltersmaybeusedforallnonvolatileextractions

evenwhenmetalsarenotofconcern.

7.2.5Weighoutasubsampleofthewaste(100gramminimum)and

recordtheweight.Ifthewastecontains<0.5%drysolids(Section7.1.2),theliquidportionofthewaste,afterfiltration,isdefinedastheTCLPextract.Therefore,enoughofthesampleshouldbefilteredsothattheamountoffilteredliquidwillsupportalloftheanalysesrequiredoftheTCLPextract.Forwastescontaining>0.5%drysolids(Sections7.1.1or7.1.2),usethepercentsolidsinformationobtainedinSection7.1.1todeterminetheoptimumsamplesize(100gramminimum)forfiltration.EnoughsolidsshouldbegeneratedbyfiltrationtosupporttheanalysestobeperformedontheTCLPextract.7.2.6Allowslurriestostandtopermitthesolidphaseto

settle.Wastesthatsettleslowlymaybecentrifugedpriortofiltration.Usecentrifugationonlyasanaidtofiltration.Ifthewasteiscentrifuged,theliquidshouldbedecantedandfilteredfollowedbyfiltrationofthesolidportionofthewastethroughthesamefiltrationsystem.

Page13of38TCLP;Method1311-13Revision0July1992

Providedbywww.ehso.com-EnvironmentalHealth&SafetyOnlineSeeEHSOforguidanceandresourcesthatisfreeandeasytofind

EPATestMethod1311-TCLP,

ToxicityCharacteristicLeachingProcedure

7.2.7Quantitativelytransferthewastesample(liquidandsolid

phases)tothefilterholder(seeSection4.3.2).Spreadthewastesampleevenlyoverthesurfaceofthefilter.Iffiltrationofthewasteat4ECreducestheamountofexpressedliquidoverwhatwouldbeexpressedatroomtemperature,thenallowthesampletowarmuptoroomtemperatureinthedevicebeforefiltering.

NOTE:

Ifwastematerial(>1%oftheoriginalsampleweight)hasobviouslyadheredtothecontainerusedtotransferthesampletothefiltrationapparatus,determinetheweightofthisresidueandsubtractitfromthesampleweightdeterminedinSection7.2.5,todeterminetheweightofthewastesamplethatwillbefiltered.

Graduallyapplyvacuumorgentlepressureof1-10psi,untilairorpressurizinggasmovesthroughthefilter.Ifthispointisnotreachedunder10psi,andifnoadditionalliquidhaspassedthroughthefilterinany2minuteinterval,slowlyincreasethepressurein10psiincrementstoamaximumof50psi.Aftereachincrementalincreaseof10psi,ifthepressurizinggashasnotmovedthroughthefilter,andifnoadditionalliquidhaspassedthroughthefilterinany2minuteinterval,proceedtothenext10psiincrement.Whenthepressurizinggasbeginstomovethroughthefilter,orwhentheliquidflowhasceasedat50psi(i.e.,filtrationdoesnotresultinanyadditionalfiltratewithina2minuteperiod),stopthefiltration.

NOTE:Instantaneousapplication

degradetheglassfiberprematureplugging.

ofhighpressurecanfilterandmaycause

7.2.8Thematerialinthefilterholderisdefinedasthesolid

phaseofthewaste,andthefiltrateisdefinedastheliquidphase.Weighthefiltrate.Theliquidphasemaynowbeeitheranalyzed(SeeSection7.2.12)orstoredat4ECuntiltimeofanalysis.

NOTE:Somewastes,suchasoilywastesandsomepaint

wastes,willobviouslycontainsomematerialthatappearstobealiquid.Evenafterapplyingvacuumorpressurefiltration,asoutlinedinSection7.2.7,thismaterialmaynotfilter.Ifthisisthecase,thematerialwithinthefiltrationdeviceisdefinedasasolidandiscarriedthroughtheextractionasasolid.Donotreplacetheoriginalfilterwithafreshfilterunderanycircumstances.Useonlyonefilter.

Page14of38TCLP;Method1311-14Revision0July1992

Providedbywww.ehso.com-EnvironmentalHealth&SafetyOnlineSeeEHSOforguidanceandresourcesthatisfreeandeasytofind

EPATestMethod1311-TCLP,

ToxicityCharacteristicLeachingProcedure

7.2.9

Ifthewastecontains<0.5%drysolids(seeSection7.1.2),proceedtoSection7.2.13.Ifthewastecontains>0.5%drysolids(seeSection7.1.1or7.1.2),andifparticlesizereductionofthesolidwasneededinSection7.1.3,proceedtoSection7.2.10.Ifthewasteasreceivedpassesa9.5mmsieve,quantitativelytransferthesolidmaterialintotheextractorbottlealongwiththefilterusedtoseparatetheinitialliquidfromthesolidphase,andproceedtoSection7.2.11.

Preparethesolidportionofthewasteforextractionbycrushing,cutting,orgrindingthewastetoasurfaceareaorparticlesizeasdescribedinSection7.1.3.Whenthesurfaceareaorparticlesizehasbeenappropriatelyaltered,quantitativelytransferthesolidmaterialintoanextractorbottle.Includethefilterusedtoseparatetheinitialliquidfromthesolidphase.

NOTE:Sievingofthewasteisnotnormallyrequired.

Surfacearearequirementsaremeantforfilamentous(e.g.,paper,cloth)andsimilarwastematerials.Actualmeasurementofsurfaceareaisnotrecommended.Ifsievingisnecessary,aTefloncoatedsieveshouldbeusedtoavoidcontaminationofthesample.

7.2.11

Determinetheamountofextractionfluidtoaddtothe

extractorvesselasfollows:

20xpercentsolids(Section7.1.1)xweightof

wastefiltered(Section7.2.5or7.2.7)

Weightof

extractionfluid

100

Slowlyaddthisamountofappropriateextractionfluid(seeSection7.1.4)totheextractorvessel.Closetheextractorbottletightly(itisrecommendedthatTeflontapebeusedtoensureatightseal),secureinrotaryagitationdevice,androtateat30+2rpmfor18+2hours.Ambienttemperature(i.e.,temperatureofroominwhichextractiontakesplace)shallbemaintainedat23+2ECduringtheextractionperiod.

NOTE:Asagitationcontinues,pressuremay

withintheextractorbottleforsomewastes(e.g.,limedorcalciumcontainingwastemayevolvegases

builduptypesofcarbonatesuchas

7.2.10

Page15of38TCLP;Method1311-15Revision0July1992

Providedbywww.ehso.com-EnvironmentalHealth&SafetyOnlineSeeEHSOforguidanceandresourcesthatisfreeandeasytofind

EPATestMethod1311-TCLP,

ToxicityCharacteristicLeachingProcedure

carbondioxide).Torelieveexcesspressure,theextractorbottlemaybeperiodicallyopened(e.g.,after15minutes,30minutes,and1hour)andventedintoahood.

7.2.12

Followingthe18+2hourextraction,separatethematerialintheextractorvesselintoitscomponentliquidandsolidphasesbyfilteringthroughanewglassfiberfilter,asoutlinedinSection7.2.7.ForfinalfiltrationoftheTCLPextract,theglassfiberfiltermaybechanged,ifnecessary,tofacilitatefiltration.Filter(s)shallbeacid-washed(seeSection4.4)ifevaluatingthemobilityofmetals.PreparetheTCLPextractasfollows:7.2.13.1

Ifthewastecontainednoinitialliquidphase,thefilteredliquidmaterialobtainedfromSection7.2.12isdefinedastheTCLPextract.ProceedtoSection7.2.14.

Ifcompatible(e.g.,multiplephaseswillnotresultoncombination),combinethefilteredliquidresultingfromSection7.2.12withtheinitialliquidphaseofthewasteobtainedinSection7.2.7.ThiscombinedliquidisdefinedastheTCLPextract.ProceedtoSection7.2.14.

7.2.13

7.2.13.2

7.2.13.3Iftheinitialliquidphaseofthewaste,as

obtainedfromSection7.2.7,isnotormaynotbecompatiblewiththefilteredliquidresultingfromSection7.2.12,donotcombinetheseliquids.Analyzetheseliquids,collectivelydefinedastheTCLPextract,andcombinetheresultsmathematically,asdescribedinSection7.2.14.

7.2.14

FollowingcollectionoftheTCLPextract,thepHoftheextractshouldberecorded.Immediatelyaliquotandpreservetheextractforanalysis.MetalsaliquotsmustbeacidifiedwithnitricacidtopH<2.Ifprecipitationisobserveduponadditionofnitricacidtoasmallaliquotoftheextract,thentheremainingportionoftheextractformetalsanalysesshallnotbeacidifiedandtheextractshallbeanalyzedassoonaspossible.Allotheraliquotsmustbestoredunderrefrigeration(4EC)untilanalyzed.TheTCLPextractshallbepreparedandanalyzedaccordingtoappropriateanalyticalmethods.TCLPextractstobeanalyzedformetalsshallbeaciddigestedexceptinthoseinstanceswheredigestioncauseslossofmetallic

Page16of38TCLP;Method1311-16Revision0July1992

Providedbywww.ehso.com-EnvironmentalHealth&SafetyOnlineSeeEHSOforguidanceandresourcesthatisfreeandeasytofind

EPATestMethod1311-TCLP,

ToxicityCharacteristicLeachingProcedure

analytes.Ifananalysisoftheundigestedextractshowsthattheconcentrationofanyregulatedmetallicanalyteexceedstheregulatorylevel,thenthewasteishazardousanddigestionoftheextractisnotnecessary.However,dataonundigestedextractsalonecannotbeusedtodemonstratethatthewasteisnothazardous.Iftheindividualphasesaretobeanalyzedseparately,determinethevolumeoftheindividualphases(to+0.5%),conducttheappropriateanalyses,andcombinetheresultsmathematicallybyusingasimplevolume-weightedaverage:

(V1)(C1)+(V2

FinalAnalyteConcentration=

where:

V1=Thevolumeofthefirstphase(L).

C1=Theconcentrationoftheanalyteofconcerninthefirstphase(mg/L).

V2=Thevolumeofthesecondphase(L).

C2=Theconcentrationoftheanalyteofconcerninthesecond

phase(mg/L).

(C)

7.2.15

ComparetheanalyteconcentrationsintheTCLPextractwiththelevelsidentifiedintheappropriateregulations.RefertoSection8.0forqualityassurancerequirements.

7.3ProcedureWhenVolatilesareInvolved

UsetheZHEdevicetoobtainTCLPextractforanalysisofvolatilecompoundsonly.ExtractresultingfromtheuseoftheZHEshallnotbeusedtoevaluatethemobilityofnonvolatileanalytes(e.g.,metals,pesticides,etc.).

TheZHEdevicehasapproximatelya500mLinternalcapacity.TheZHEcanthusaccommodateamaximumof25gramsofsolid(definedasthatfractionofasamplefromwhichnoadditionalliquidmaybeforcedoutbyanappliedpressureof50psi),duetotheneedtoaddanamountofextractionfluidequalto20timestheweightofthesolidphase.

ChargetheZHEwithsampleonlyonceanddonotopenthedeviceuntilthefinalextract(ofthesolid)hasbeencollected.RepeatedfillingoftheZHEtoobtain25gramsofsolidisnotpermitted.

Donotallowthewaste,theinitialliquidphase,ortheextracttobeexposedtotheatmosphereforanymoretimethan

Page17of38TCLP;Method1311-17Revision0July1992

Providedbywww.ehso.com-EnvironmentalHealth&SafetyOnlineSeeEHSOforguidanceandresourcesthatisfreeandeasytofind

EPATestMethod1311-TCLP,

ToxicityCharacteristicLeachingProcedure

isabsolutelynecessary.Anymanipulationofthesematerialsshouldbedonewhencold(4EC)tominimizelossofvolatiles.7.3.1

Pre-weighthe(evacuated)filtratecollectioncontainer(SeeSection4.6)andsetaside.IfusingaTEDLARbag,expressallliquidfromtheZHEdeviceintothebag,whetherfortheinitialorfinalliquid/solidseparation,andtakeanaliquotfromtheliquidinthebagforanalysis.ThecontainerslistedinSection4.6arerecommendedforuseundertheconditionsstatedinSections4.6.1-4.6.3.

PlacetheZHEpistonwithinthebodyoftheZHE(itmaybehelpfulfirsttomoistenthepistonO-ringsslightlywithextractionfluid).AdjustthepistonwithintheZHEbodytoaheightthatwillminimizethedistancethepistonwillhavetomoveoncetheZHEischargedwithsample(baseduponsamplesizerequirementsdeterminedfromSection7.3,Section7.1.1and/or7.1.2).Securethegasinlet/outletflange(bottomflange)ontotheZHEbodyinaccordancewiththemanufacturer'sinstructions.Securetheglassfiberfilterbetweenthesupportscreensandsetaside.Setliquidinlet/outletflange(topflange)aside.

Ifthewasteis100%solid(seeSection7.1.1),weighoutasubsample(25grammaximum)ofthewaste,recordweight,andproceedtoSection7.3.5.

Ifthewastecontains<0.5%drysolids(Section7.1.2),theliquidportionofwaste,afterfiltration,isdefinedastheTCLPextract.Filterenoughofthesamplesothattheamountoffilteredliquidwillsupportallofthevolatileanalysesrequired.Forwastescontaining>0.5%drysolids(Sections7.1.1and/or7.1.2),usethepercentsolidsinformationobtainedinSection7.1.1todeterminetheoptimumsamplesizetochargeintotheZHE.Therecommendedsamplesizeisasfollows:7.3.4.1

Forwastescontaining<5%solids(seeSection7.1.1),weighouta500gramsubsampleofwasteandrecordtheweight.Forwastescontaining>5%solids(seeSection7.1.1),determinetheamountofwastetochargeintotheZHEasfollows:

7.3.2

7.3.3

7.3.4

7.3.4.2

WeightofwastetochargeZHE=______________________________________x

100percentsolids(Section7.1.1)

Page18of38TCLP;Method1311-18Revision0July1992

Providedbywww.ehso.com-EnvironmentalHealth&SafetyOnlineSeeEHSOforguidanceandresourcesthatisfreeandeasytofind

EPATestMethod1311-TCLP,

ToxicityCharacteristicLeachingProcedure

Weighoutasubsampleofthewasteoftheappropriatesizeandrecordtheweight.7.3.5

IfparticlesizereductionofthesolidportionofthewastewasrequiredinSection7.1.3,proceedtoSection7.3.6.IfparticlesizereductionwasnotrequiredinSection7.1.3,proceedtoSection7.3.7.

Preparethewasteforextractionbycrushing,cutting,orgrindingthesolidportionofthewastetoasurfaceareaorparticlesizeasdescribedinSection7.1.3.Wastesandappropriatereductionequipmentshouldberefrigerated,ifpossible,to4ECpriortoparticlesizereduction.Themeansusedtoeffectparticlesizereductionmustnotgenerateheatinandofitself.Ifreductionofthesolidphaseofthewasteisnecessary,exposureofthewastetotheatmosphereshouldbeavoidedtotheextentpossible.NOTE:

Sievingofthewasteisnotrecommendedduetothepossibilitythatvolatilesmaybelost.Theuseofanappropriatelygraduatedrulerisrecommendedasanacceptablealternative.Surfacearearequirementsaremeantfor

filamentous(e.g.,paper,cloth)andsimilarwastematerials.Actualmeasurementofsurfaceareaisnotrecommended.

Whenthesurfaceareaorparticlesizehas

beenappropriatelyaltered,proceedtoSection7.3.7.

7.3.7

Wasteslurriesneednotbeallowedtostandtopermitthe

solidphasetosettle.Donotcentrifugewastespriortofiltration.

Quantitativelytransfertheentiresample(liquidandsolidphases)quicklytotheZHE.SecurethefilterandsupportscreensontothetopflangeofthedeviceandsecurethetopflangetotheZHEbodyinaccordancewiththemanufacturer'sinstructions.TightenallZHEfittingsandplacethedeviceintheverticalposition(gasinlet/outletflangeonthebottom).Donotattachtheextractcollectiondevicetothetopplate.NOTE:

Ifwastematerial(>1%oforiginalsampleweight)hasobviouslyadheredtothecontainerusedtotransferthesampletotheZHE,determinetheweightofthisresidueandsubtractitfromthesampleweightdeterminedinSection7.3.4to

7.3.6

7.3.8

Page19of38TCLP;Method1311-19Revision0July1992

Providedbywww.ehso.com-EnvironmentalHealth&SafetyOnlineSeeEHSOforguidanceandresourcesthatisfreeandeasytofind

EPATestMethod1311-TCLP,

ToxicityCharacteristicLeachingProcedure

determinetheweightofthewastesamplethatwillbefiltered.Attachagaslinetothegasinlet/outletvalve(bottomflange)and,withtheliquidinlet/outletvalve(topflange)open,beginapplyinggentlepressureof1-10psi(ormoreifnecessary)toforceallheadspaceslowlyoutoftheZHEdeviceintoahood.Atthefirstappearanceofliquidfromtheliquidinlet/outletvalve,quicklyclosethevalveanddiscontinuepressure.Iffiltrationofthewasteat4ECreducestheamountofexpressedliquidoverwhatwouldbeexpressedatroomtemperature,thenallowthesampletowarmuptoroomtemperatureinthedevicebeforefiltering.Ifthewasteis100%solid(seeSection7.1.1),slowlyincreasethepressuretoamaximumof50psitoforcemostoftheheadspaceoutofthedeviceandproceedtoSection7.3.12.

7.3.9

Attachtheevacuatedpre-weighedfiltratecollectioncontainertotheliquidinlet/outletvalveandopenthevalve.Beginapplyinggentlepressureof1-10psitoforcetheliquidphaseofthesampleintothefiltratecollectioncontainer.Ifnoadditionalliquidhaspassedthroughthefilterinany2minuteinterval,slowlyincreasethepressurein10psiincrementstoamaximumof50psi.Aftereachincrementalincreaseof10psi,ifnoadditionalliquidhaspassedthroughthefilterinany2minuteinterval,proceedtothenext10psiincrement.Whenliquidflowhasceasedsuchthatcontinuedpressurefiltrationat50psidoesnotresultinanyadditionalfiltratewithina2minuteperiod,stopthefiltration.Closetheliquidinlet/outletvalve,discontinuepressuretothepiston,anddisconnectandweighthefiltratecollectioncontainer.NOTE:

Instantaneousapplicationofhighpressurecandegradetheglassfiberfilterandmaycauseprematureplugging.

7.3.10ThematerialintheZHEisdefinedasthesolidphaseof

thewasteandthefiltrateisdefinedastheliquidphase.

NOTE:

Somewastes,suchasoilywastesandsomepaintwastes,willobviouslycontainsomematerialthatappearstobealiquid.Evenafterapplyingpressurefiltration,thismaterialwillnotfilter.Ifthisisthecase,thematerialwithinthefiltrationdeviceisdefinedasasolidandiscarriedthroughtheTCLPextractionasa

Page20of38TCLP;Method1311-20Revision0July1992

Providedbywww.ehso.com-EnvironmentalHealth&SafetyOnlineSeeEHSOforguidanceandresourcesthatisfreeandeasytofind

EPATestMethod1311-TCLP,

ToxicityCharacteristicLeachingProcedure

solid.

Iftheoriginalwastecontained<0.5%drysolids(seeSection7.1.2),thisfiltrateisdefinedastheTCLPextractandisanalyzeddirectly.ProceedtoSection7.3.15.

7.3.11Theliquidphasemaynowbeeitheranalyzedimmediately

(SeeSections7.3.13through7.3.15)orstoredat4ECunderminimalheadspaceconditionsuntiltimeofanalysis.Determinetheweightofextractionfluid#1toaddtotheZHEasfollows:

20xpercentsolids(Section7.1.1)xweightofwastefiltered(Section7.3.4or7.3.8)

Weightofextraction

fluid=

100

7.3.12

ThefollowingSectionsdetailhowtoaddthe

appropriateamountofextractionfluidtothesolidmaterialwithintheZHEandagitationoftheZHEvessel.Extractionfluid#1isusedinallcases(SeeSection5.7).7.3.12.1

WiththeZHEintheverticalposition,attachalinefromtheextractionfluidreservoirtotheliquidinlet/outletvalve.Thelineusedshallcontainfreshextractionfluidandshouldbepreflushedwithfluidtoeliminateanyairpocketsintheline.ReleasegaspressureontheZHEpiston(fromthegasinlet/outletvalve),opentheliquidinlet/outletvalve,andbegintransferringextractionfluid(bypumpingorsimilarmeans)intotheZHE.ContinuepumpingextractionfluidintotheZHEuntiltheappropriateamountoffluidhasbeenintroducedintothedevice.

Aftertheextractionfluidhasbeenadded,immediatelyclosetheliquidinlet/outletvalveanddisconnecttheextractionfluidline.ChecktheZHEtoensurethatallvalvesareintheirclosedpositions.Manuallyrotatethedeviceinanend-over-endfashion2or3times.RepositiontheZHEintheverticalpositionwiththeliquidinlet/outletvalveontop.PressurizetheZHEto5-10psi(ifnecessary)andslowlyopentheliquid

7.3.12.2

Page21of38TCLP;Method1311-21Revision0July1992

Providedbywww.ehso.com-EnvironmentalHealth&SafetyOnlineSeeEHSOforguidanceandresourcesthatisfreeandeasytofind

EPATestMethod1311-TCLP,

ToxicityCharacteristicLeachingProcedure

inlet/outletvalvetobleedoutanyheadspace(intoahood)thatmayhavebeenintroducedduetotheadditionofextractionfluid.Thisbleedingshallbedonequicklyandshallbestoppedatthefirstappearanceofliquidfromthevalve.Re-pressurizetheZHEwith5-10psiandcheckallZHEfittingstoensurethattheyareclosed.

7.3.12.3

PlacetheZHEintherotaryagitationapparatus(ifitisnotalreadythere)androtateat30+2rpmfor18+2hours.Ambienttemperature(i.e.,temperatureofroominwhichextractionoccurs)shallbemaintainedat23+2ECduringagitation.

7.3.13Followingthe18+2houragitationperiod,checkthe

pressurebehindtheZHEpistonbyquicklyopeningandclosingthegasinlet/outletvalveandnotingtheescapeofgas.Ifthepressurehasnotbeenmaintained(i.e.,nogasreleaseobserved),thedeviceisleaking.ChecktheZHEforleakingasspecifiedinSection4.2.1,andperformtheextractionagainwithanewsampleofwaste.Ifthepressurewithinthedevicehasbeenmaintained,thematerialintheextractorvesselisonceagainseparatedintoitscomponentliquidandsolidphases.Ifthewastecontainedaninitialliquidphase,theliquidmaybefiltereddirectlyintothesamefiltratecollectioncontainer(i.e.,TEDLARbag)holdingtheinitialliquidphaseofthewaste.Aseparatefiltratecollectioncontainermustbeusedifcombiningwouldcreatemultiplephases,orthereisnotenoughvolumeleftwithinthefiltratecollectioncontainer.Filterthroughtheglassfiberfilter,usingtheZHEdeviceasdiscussedinSection7.3.9.AllextractshallbefilteredandcollectediftheTEDLARbagisused,iftheextractismultiphasic,orifthewastecontainedaninitialliquidphase(seeSections4.6and7.3.1).

NOTE:Anin-lineglassfiberfiltermaybeusedto

filterthematerialwithintheZHEifitissuspectedthattheglassfiberfilterhasbeenruptured.

7.3.14

Iftheoriginalwastecontainednoinitialliquidphase,thefilteredliquidmaterialobtainedfromSection7.3.13isdefinedastheTCLPextract.Ifthewastecontainedaninitialliquidphase,thefilteredliquidmaterialobtainedfromSection7.3.13andtheinitialliquidphase(Section7.3.9)arecollectivelydefinedastheTCLPextract.

Page22of38TCLP;Method1311-22Revision0July1992

Providedbywww.ehso.com-EnvironmentalHealth&SafetyOnlineSeeEHSOforguidanceandresourcesthatisfreeandeasytofind

EPATestMethod1311-TCLP,

ToxicityCharacteristicLeachingProcedure

7.3.15FollowingcollectionoftheTCLPextract,immediately

preparetheextractforanalysisandstorewithminimalheadspaceat4ECuntilanalyzed.AnalyzetheTCLPextractaccordingtotheappropriateanalyticalmethods.Iftheindividualphasesaretobeanalyzedseparately(i.e.,arenotmiscible),determinethevolumeoftheindividualphases(to0.5%),conducttheappropriateanalyses,andcombinetheresultsmathematicallybyusingasimplevolume-weightedaverage:

(V1)(C1)+(V2)(C2)

FinalAnalyte=Concentrationwhere:VC

=Thevolumeofthefirstphases(L).

1=Theconcentrationoftheanalyteofconcerninthe

firstphase(mg/L).

V2=Thevolumeofthesecondphase(L).

C2=Theconcentrationoftheanalyteofconcerninthe

secondphase(mg/L).

7.3.16ComparetheanalyteconcentrationsintheTCLPextract

withthelevelsidentifiedintheappropriateregulations.RefertoSection8.0forqualityassurancerequirements.

8.0QUALITYASSURANCE

8.1

Aminimumofoneblank(usingthesameextractionfluidasusedforthesamples)mustbeanalyzedforevery20extractionsthathavebeenconductedinanextractionvessel.

8.2Amatrixspikeshallbeperformedforeachwastetype(e.g.,

wastewatertreatmentsludge,contaminatedsoil,etc.)unlesstheresultexceedstheregulatorylevelandthedataarebeingusedsolelytodemonstratethatthewastepropertyexceedstheregulatorylevel.Aminimumofonematrixspikemustbeanalyzedforeachanalyticalbatch.Asaminimum,followthematrixspikeadditionguidanceprovidedineachanalyticalmethod.

8.2.1MatrixspikesaretobeaddedafterfiltrationoftheTCLP

extractandbeforepreservation.MatrixspikesshouldnotbeaddedpriortoTCLPextractionofthesample.8.2.2Inmostcases,matrixspikesshouldbeaddedata

concentrationequivalenttothecorrespondingregulatorylevel.Iftheanalyteconcentrationislessthanonehalftheregulatorylevel,thespikeconcentrationmaybeas

Page23of38TCLP;Method1311-23Revision0July1992

Providedbywww.ehso.com-EnvironmentalHealth&SafetyOnlineSeeEHSOforguidanceandresourcesthatisfreeandeasytofind

EPATestMethod1311-TCLP,

ToxicityCharacteristicLeachingProcedure

lowasonehalfoftheanalyteconcentration,butmaynotbenotlessthanfivetimesthemethoddetectionlimit.Inordertoavoiddifferencesinmatrixeffects,thematrixspikesmustbeaddedtothesamenominalvolumeofTCLPextractasthatwhichwasanalyzedfortheunspikedsample.

8.2.3Thepurposeofthematrixspikeistomonitorthe

performanceoftheanalyticalmethodsused,andtodeterminewhethermatrixinterferencesexist.Useofotherinternalcalibrationmethods,modificationoftheanalyticalmethods,oruseofalternateanalyticalmethodsmaybeneededtoaccuratelymeasuretheanalyteconcentrationintheTCLPextractwhentherecoveryofthematrixspikeisbelowtheexpectedanalyticalmethodperformance.8.2.4Matrixspikerecoveriesarecalculatedbythefollowing

formula:

%R(%Recovery)=100(Xsu-X)/K

where:

Xs=measuredvalueforthespikedsample,Xu=measuredvalueforthe

unspikedsample,and

K=knownvalueofthespikein

thesample.

8.3

Allqualitycontrolmeasuresdescribedintheappropriateanalytical

methodsshallbefollowed.

Theuseofinternalcalibrationquantitationmethodsshallbeemployedforametalliccontaminantif:(1)RecoveryofthecontaminantfromtheTCLPextractisnotatleast50%andtheconcentrationdoesnotexceedtheregulatorylevel,and(2)Theconcentrationofthecontaminantmeasuredintheextractiswithin20%oftheappropriateregulatorylevel.

8.4.1.Themethodofstandardadditionsshallbeemployedasthe

internalcalibrationquantitationmethodforeachmetalliccontaminant.8.4.2Themethodofstandardadditionsrequirespreparing

calibrationstandardsinthesamplematrixratherthanreagentwaterorblanksolution.Itrequirestakingfouridenticalaliquotsofthesolutionandaddingknown

amountsofstandardtothreeofthesealiquots.Theforthaliquotistheunknown.Preferably,thefirstadditionshouldbepreparedsothattheresultingconcentrationisapproximately50%oftheexpectedconcentrationofthesample.Thesecondandthirdadditionsshouldbeprepared

8.4

Page24of38TCLP;Method1311-24Revision0July1992

Providedbywww.ehso.com-EnvironmentalHealth&SafetyOnlineSeeEHSOforguidanceandresourcesthatisfreeandeasytofind

EPATestMethod1311-TCLP,

ToxicityCharacteristicLeachingProcedure

sothattheconcentrationsareapproximately100%and150%oftheexpectedconcentrationofthesample.Allfour

aliquotsaremaintainedatthesamefinalvolumebyaddingreagentwaterorablanksolution,andmayneeddilutionadjustmenttomaintainthesignalsinthelinearrangeoftheinstrumenttechnique.Allfouraliquotsareanalyzed.

8.4.3Prepareaplot,orsubjectdatatolinearregression,of

instrumentsignalsorexternal-calibration-derivedconcentrationsasthedependantvariable(y-axis)versusconcentrationsoftheadditionsofstandardastheindependentvariable(x-axis).Solvefortheinterceptoftheabscissa(theindependentvariable,x-axis)whichistheconcentrationintheunknown.8.4.4Alternately,subtracttheinstrumentalsignalorexternal-calibration-derivedconcentrationoftheunknown(unspiked)samplefromtheinstrumentalsignalsorexternal-calibration-derivedconcentrationsofthestandardadditions.Plotorsubjecttolinearregressionofthecorrectedinstrumentsignalsorexternal-calibration-derivedconcentrationsasthedependantvariableversustheindependentvariable.Deriveconcentrationsforunknownsusingtheinternalcalibrationcurveasifitwereanexternalcalibrationcurve.

SamplesmustundergoTCLPextractionwithinthefollowingtimeperiods:

SAMPLEMAXIMUMHOLDINGTIMES[DAYS]From:Field

collectionTo:TCLP

extraction

From:TCLP

extractionTo:

Preparativeextraction

From:

PreparativeextractionTo:

Determinativeanalysis

Totalelapsedtime144028180

286156360

8.5

Volatiles

Semi-volatilesMercury

Metals,exceptmercury

NA=Notapplicable

141428180NA7NANA

Ifsampleholdingtimesareexceeded,thevaluesobtainedwillbeconsideredminimalconcentrations.Exceedingtheholdingtimeisnotacceptableinestablishingthatawastedoesnotexceedtheregulatorylevel.Exceedingtheholdingtimewillnotinvalidatecharacterizationifthewasteexceedstheregulatory

Page25of38TCLP;Method1311-25Revision0July1992

Providedbywww.ehso.com-EnvironmentalHealth&SafetyOnlineSeeEHSOforguidanceandresourcesthatisfreeandeasytofind

EPATestMethod1311-TCLP,

ToxicityCharacteristicLeachingProcedure

level.

Noneoftheparametershadasignificanteffectontheresultsoftheruggednesstest.

9.0

METHODPERFORMANCE9.1

Ruggedness.Tworuggednessstudieshavebeenperformedtodeterminetheeffectofvariousperturbationsonspecific

elementsoftheTCLPprotocol.Ruggednesstestingdeterminesthesensitivityofsmallproceduralvariationswhichmightbeexpectedtooccurduringroutinelaboratoryapplication.

9.1.1Metals-Thefollowingconditionswereusedwhenleaching

awasteformetalsanalysis:

VaryingConditionsLiquid/Solidratio19:1vs.21:1Extractiontime16hoursvs.18hoursHeadspace20%vs.60%Buffer#2acidity190meqvs.210meqAcid-washedfiltersyesvs.noFiltertype0.7µmglassfibervs.0.45µmvs.polycarbonate

Bottletypeborosilicatevs.flintglass

Ofthesevenmethodvariationsexamined,acidityoftheextractionfluidhadthegreatestimpactontheresults.Fourof13metalsfromanAPIseparatorsludge/

electroplatingwaste(API/EW)mixtureandtwoofthreemetalsfromanammonialimestillbottomwastewereextractedathigherlevelsbythemoreacidicbuffer.BecauseofthesensitivitytopHchanges,themethodrequiresthattheextractionfluidsbepreparedsothatthefinalpHiswithin+0.05unitsasspecified.

9.1.2VolatileOrganicCompounds-Thefollowingconditionswere

usedwhenleachingawasteforVOCanalysis:

VaryingConditionsLiquid/Solidratio19:1vs.21:1Headspace0%vs.5%Buffer#1acidity60meqvs.80meqMethodofstoringextractSyringevs.Tedlarbag®Aliquottingyesvs.noPressurebehindpiston0psivs.20psi9.2

Precision.ManyTCLPprecision(reproducibility)studieshave

beenperformed,andhaveshownthat,ingeneral,theprecisionoftheTCLPiscomparabletoorexceedsthatoftheEPtoxicitytestandthatmethodprecisionisadequate.Oneofthemoresignificantcontributionstopoorprecisionappearstoberelatedtosamplehomogeneityandinter-laboratoryvariation(duetothe

Page26of38TCLP;Method1311-26Revision0July1992

Providedbywww.ehso.com-EnvironmentalHealth&SafetyOnlineSeeEHSOforguidanceandresourcesthatisfreeandeasytofind

EPATestMethod1311-TCLP,

ToxicityCharacteristicLeachingProcedure

natureofwastematerials).

9.2.1Metals-Theresultsofamulti-laboratorystudyareshown

inTable6,andindicatethatasingleanalysisofawastemaynotbeadequateforwastecharacterizationandidentificationrequirements.9.2.2Semi-VolatileOrganicCompounds-Theresultsoftwo

studiesareshowninTables7and8.Singlelaboratoryprecisionwasexcellentwithgreaterthan90percentoftheresultsexhibitinganRSDlessthan25percent.Over85percentofallindividualcompoundsinthemulti-laboratorystudyfellintheRSDrangeof20-120percent.BothstudiesconcludedthattheTCLPprovidesadequateprecision.Itwasalsodeterminedthatthehighacetatecontentoftheextractionfluiddidnotpresentproblems(i.e.,columndegradationofthegaschromatograph)fortheanalyticalconditionsused.9.2.3VolatileOrganicCompounds-Elevenlaboratories

participatedinacollaborativestudyoftheuseoftheZHEwithtwowastetypeswhichwerefortifiedwithamixtureofVOCs.TheresultsofthecollaborativestudyareshowninTable9.PrecisionresultsforVOCstendtooccuroveraconsiderablerange.However,therangeandmeanRSDcomparedverycloselytothesamecollaborativestudymetalsresultsinTable6.BlackburnandShowconcludedthatatthe95%levelofsignificance:1)recoveriesamonglaboratorieswerestatisticallysimilar,2)recoveriesdidnotvarysignificantlybetweenthetwosampletypes,and3)eachlaboratoryshowedthesamepatternofrecoveryforeachofthetwosamples.

10.0REFERENCES

Blackburn,W.B.andShow,I.\"CollaborativeStudyoftheToxicityCharacteristicsLeachingProcedure(TCLP).\"DraftFinalReport,ContractNo.68-03-1958,S-Cubed,November1986.

Newcomer,L.R.,Blackburn,W.B.,Kimmell,T.A.\"PerformanceoftheToxicityCharacteristicLeachingProcedure.\"WilsonLaboratories,S-Cubed,U.S.EPA,December1986.

Williams,L.R.,Francis,C.W.;Maskarinec,M.P.,TaylorD.R.,andRothman,N.\"Single-LaboratoryEvaluationofMobilityProcedureforSolidWaste.\"EMSL,ORNL,S-Cubed,ENSECO.

Page27of38TCLP;Method1311-27Revision0July1992

Providedbywww.ehso.com-EnvironmentalHealth&SafetyOnlineSeeEHSOforguidanceandresourcesthatisfreeandeasytofind

EPATestMethod1311-TCLP,

ToxicityCharacteristicLeachingProcedure

Table1.

VolatileAnalytes1,2CompoundCASNo.

AcetoneBenzene

n-ButylalcoholCarbondisulfide

CarbontetrachlorideChlorobenzeneChloroform

1,2-Dichloroethane1,1-DichloroethyleneEthylacetateEthylbenzeneEthyletherIsobutanolMethanol

MethylenechlorideMethylethylketoneMethylisobutylketoneTetrachloroethyleneToluene

1,1,1,-TrichloroethaneTrichloroethylene

Trichlorofluoromethane

1,1,2-Trichloro-1,2,2-trifluoroethaneVinylchlorideXylene67--171-43-271-36-375-15-056-23-5108-90-767-66-3107-06-275-35-4141-78-6100-41-460-29-778-83-167-56-175-09-278-93-3108-10-1127-18-4108-88-371-55-679-01-675-69-476-13-175-01-41330-20-7

Whentestingforanyoralloftheseanalytes,thezero-headspaceextractorvesselshallbeusedinsteadofthebottleextractor.

Benzene,carbontetrachloride,chlorobenzene,chloroform,1,2-dichloroethane,1,1-dichloroethylene,methylethylketone,

tetrachloroethylene,andvinylchloridearetoxicitycharacteristicconstituents.

Page28of38TCLP;Method1311-28Revision0July1992

Providedbywww.ehso.com-EnvironmentalHealth&SafetyOnlineSeeEHSOforguidanceandresourcesthatisfreeandeasytofind

EPATestMethod1311-TCLP,

ToxicityCharacteristicLeachingProcedure

Table2.

SuitableRotaryAgitationApparatus1CompanyLocationModelNo.

AnalyticalTestingandConsultingServices,Inc.

Warrington,PA(215)343-4490

4-vessel8-vessel12-vessel24-vessel2-vessel4-vessel6-vessel8-vessel12-vessel24-vessel

extractorextractorextractorextractor(DC20S)(DC20)(DC20B)(DC24C)

AssociatedDesignandManufacturingCompanyAlexandria,VA(703)549-5999

(3740-2-BRE)(3740-4-BRE)(3740-6-BRE)(3740-8-BRE)(3740-12-BRE)(3740-24-BRE)

EnvironmentalMachineandDesign,Inc.IRAMachineShopandLaboratory

LarsLandeManufacturing

Lynchburg,VA(804)845-24Santurce,PR(809)752-4004WhitmoreLake,MI(313)449-4116

8-vessel(08-00-00)4-vessel(04-00-00)8-vessel(011001)

10-vessel(10VRE)5-vessel(5VRE)6-vessel(6VRE)

4-ZHEor

42-literbottleextractor

(YT31ORAHW)

MilliporeCorp.

Bedford,MA(800)225-3384

Anydevicethatrotatestheextractionvesselinanend-over-endfashionat30+2rpmisacceptable.

Page29of38TCLP;Method1311-29Revision0July1992

Providedbywww.ehso.com-EnvironmentalHealth&SafetyOnlineSeeEHSOforguidanceandresourcesthatisfreeandeasytofind

EPATestMethod1311-TCLP,

ToxicityCharacteristicLeachingProcedure

Table3.

SuitableZero-HeadspaceExtractorVessels1CompanyLocationModelNo.

AnalyticalTesting&

ConsultingServices,Inc.AssociatedDesignandManufacturingCompany

Warrington,PA(215)343-4490Alexandria,VA(703)549-5999WhitmoreLake,MI(313)449-4116

C1O2,MechanicalPressureDevice3745-ZHE,GasPressureDeviceZHE-11,GasPressureDeviceYT30O9OHW,GasPressureDeviceVOLA-TOX1,GasPressureDevice15400GasPressureDevice

LarsLandeManufacturing

MilliporeCorporation

Bedford,MA(800)225-3384Lynchburg,VA(804)845-24AnnArbor,MI(800)521-1520

EnvironmentalMachineandDesign,Inc.GelmanScience

AnydevicethatmeetsthespecificationslistedinSection4.2.1ofthemethodissuitable.

Thisdeviceusesa110mmfilter.

Page30of38TCLP;Method1311-30Revision0July1992

Providedbywww.ehso.com-EnvironmentalHealth&SafetyOnlineSeeEHSOforguidanceandresourcesthatisfreeandeasytofind

EPATestMethod1311-TCLP,

ToxicityCharacteristicLeachingProcedure

Table4.

SuitableFilterHolders1Company

NucleoporeCorporationMicroFiltrationSystems

MilliporeCorporation

LocationPleasanton,CA(800)882-7711Dublin,CA

(800)334-7132

828-6010Bedford,MA(800)225-3384

Model/

CatalogueNo.425910410400302400311400YT30142HWXX1004700

Size142mm47mm

142mm

47mm(415)142mm47mm

Anydevicecapableofseparatingtheliquidfromthesolidphaseofthewasteissuitable,providingthatitischemicallycompatiblewiththewasteandtheconstituentstobeanalyzed.Plasticdevices(notlistedabove)maybeusedwhenonlyinorganicanalytesareofconcern.The142mmsizefilterholderisrecommended.

Table5.SuitableFilterMedia1PoreSize

Company

Location

Model

(µm)

MilliporeCorporationNucleoporeCorporation

Bedford,MA(800)225-3384Pleasanton,CA(415)463-2530Clifton,NJ(201)773-5800Dublin,CA

(800)334-7132(415)828-6010AnnArbor,MI(800)521-1520

AP40211625

0.70.7

WhatmanLaboratoryProducts,Inc.MicroFiltrationSystems

GFF0.7

GF750.7

GelmanScience

66256(90mm)66257(142mm)

0.7

AnyfilterthatmeetsthespecificationsinSection4.4oftheMethodissuitable.

Page31of38TCLP;Method1311-31Revision0July1992

Providedbywww.ehso.com-EnvironmentalHealth&SafetyOnlineSeeEHSOforguidanceandresourcesthatisfreeandeasytofind

EPATestMethod1311-TCLP,

ToxicityCharacteristicLeachingProcedure

Table6.Multi-LaboratoryTCLPMetals,Precision

ExtractionFluid

#1#2#1#2#1#2#1#2#1#2#1#2#1#2#1#2#1#2

WasteAmmonia

LimeStillBottoms

MetalCadmiumChromiumLead

X0.0530.0230.0150.00320.00300.00320.00460.00050.05610.1050.00310.01240.0800.0930.0170.0700.00870.0457

S0.0310.0170.00140.00370.00270.00280.00280.00040.02270.0180.00310.01360.0690.0670.0140.0400.00740.0083

%RSD6076931108761774017100110867285578518

API/EWMixture

CadmiumChromiumLead

FossilFuelFlyAsh

CadmiumChromiumLead

%RSDRange=17-118Mean%RSD=74

NOTE:X=Meanresultsfrom6-12differentlaboratories

Units=mg/L

ExtractionFluid#1=pH4.9#2

=pH2.9

Page32of38TCLP;Method1311-32Revision0July1992

Providedbywww.ehso.com-EnvironmentalHealth&SafetyOnlineSeeEHSOforguidanceandresourcesthatisfreeandeasytofind

EPATestMethod1311-TCLP,

ToxicityCharacteristicLeachingProcedure

Table7.Single-LaboratorySemi-Volatiles,Precision

ExtractionFluid

#1#2#1#2#1#2#1#2#1#2#1#2#1#2#1#2#1#2#1#2#1#2#1#2#1#2#1#2#1#2#1#2

WasteAmmonia

LimeStillBottoms

CompoundPhenol

2-Methylphenol4-Methylphenol2,4-DimethylphenolNaphthalene

2-MethylnaphthaleneDibenzofuranAcenaphthyleneFluorenePhenanthreneAnthraceneFluoranthrene

X190001940020001860794074903213073920382729027318718770366315115624124333.234.625.326.040.719.033.043.3185165265200

S223092929752.9138020046.845.8413174.819.322.77.2.220.117.62.122.77.96.191.551.81.813.51.769.358.6129.424.861.218.9

%RSD11..814.92.817.42.714.614.910.54.615.57.112.13.912.73.011.71.39.43.318..57.17.133.09.328.319.915.815.023.19.5

API/EWMixture

Phenol

2,4-DimethylphenolNaphthalene

2-Methylnaphthalene

%RSDRange=1-33Mean%RSD=12

NOTE:Units=µg/L

Extractionswereperformedintriplicate

Allresultswereatleast2xthedetectionlimitExtractionFluid#1=pH4.9

#2=pH2.9

Page33of38TCLP;Method1311-33Revision0July1992

Providedbywww.ehso.com-EnvironmentalHealth&SafetyOnlineSeeEHSOforguidanceandresourcesthatisfreeandeasytofind

EPATestMethod1311-TCLP,

ToxicityCharacteristicLeachingProcedure

Table8.Multi-LaboratorySemi-Volatiles,Precision

Waste

AmmoniaLime

StillBottoms(A)API/EW

Mixture(B)FossilFuelFlyAsh(C)

CompoundBNAsBNAsBNAs

ExtractionFluid

#1#2#1#2#1#2

X100431037616242074750739

S768065526751463175342

%RSD76.563.141.670.523.446.3

Mean%RSD=54

NOTE:Units=µg/L

X=Meanresultsfrom3-10labsExtractionFluid#1=pH4.9

#2=pH2.9

%RSDRangeforIndividualCompounds

A,#10-113A,#228-108B,#120-156B,#249-128C,#136-143C,#261-1

Page34of38TCLP;Method1311-34Revision0July1992

Providedbywww.ehso.com-EnvironmentalHealth&SafetyOnlineSeeEHSOforguidanceandresourcesthatisfreeandeasytofind

EPATestMethod1311-TCLP,

ToxicityCharacteristicLeachingProcedure

Table9.Multi-Laboratory(11Labs)VOCs,Precision

WasteMine

Tailings

Compound

Vinylchloride

MethylenechlorideCarbondisulfide1,1-Dichloroethene1,1-DichloroethaneChloroform

1,2-Dichloroethane2-Butanone

1,1,1-TrichloroethaneCarbontetrachlorideTrichloroethene

1,1,2-TrichloroetheneBenzene

1,1,2,2-TetrachloroethaneToluene

ChlorobenzeneEthylbenzene

TrichlorofluoromethaneAcrylonitrile

Vinylchloride

MethylenechlorideCarbondisulfide1,1-Dichloroethene1,1-DichloroethaneChloroform

1,2-Dichloroethane2-Butanone

1,1,1-TrichloroethaneCarbontetrachlorideTrichloroethene

1,1,2-TrichloroetheneBenzene

1,1,2,2-TetrachloroethaneToluene

ChlorobenzeneEthylbenzene

TrichlorofluoromethaneAcrylonitrile

X6.3612.15.5721.931.446.7.843.520.912.024.719.637.934.929.335..273.8276.75.0014.33.3752.152.8.743.159.053.67.1057.36.761.33.1669.071.83.704.0529.4

S6.3611.82.8327.725.429.233.636.920.98.221.210.928.725.611.219.32.804.40110.84.7113.12.0738.825.628.431.539.0.96.134.24.726.82.118.512.02.24.834.8

%RSD10098511278163708510068865676733854661151449492617549447367768660704466271758119118

AmmoniaLimeStillBottoms

%RSDRange=17-144Mean%RSD=75

NOTE:Units=µg/L

Page35of38TCLP;Method1311-35Revision0July1992

Providedbywww.ehso.com-EnvironmentalHealth&SafetyOnlineSeeEHSOforguidanceandresourcesthatisfreeandeasytofind

EPATestMethod1311-TCLP,

ToxicityCharacteristicLeachingProcedure

Figure1.RotaryAgitationApparatus

Figure2.Zero-HeadspaceExtractor(ZHE)

Page36of38TCLP;Method1311-36Revision0July1992

Providedbywww.ehso.com-EnvironmentalHealth&SafetyOnlineSeeEHSOforguidanceandresourcesthatisfreeandeasytofind

EPATestMethod1311-TCLP,

ToxicityCharacteristicLeachingProcedure

METHOD1311-TOXICITYCHARACTERISTICLEACHATEPROCEDURE

Page37of38TCLP;Method1311-37Revision0July1992

Providedbywww.ehso.com-EnvironmentalHealth&SafetyOnlineSeeEHSOforguidanceandresourcesthatisfreeandeasytofind

EPATestMethod1311-TCLP,

ToxicityCharacteristicLeachingProcedure

METHOD1311(CONTINUED)

TOXICITYCHARACTERISTICLEACHATEPROCEDURE

Page38of38TCLP;Method1311-38Revision0July1992

Providedbywww.ehso.com-EnvironmentalHealth&SafetyOnlineSeeEHSOforguidanceandresourcesthatisfreeandeasytofind

因篇幅问题不能全部显示，请点此查看更多更全内容

查看全文