EPA Method 23

Method23-DeterminationofPolychlorinatedDibenzo-p-dioxinsandPolychlorinatedDibenzofuransfromMunicipalWasteCombustors1.APPLICABILITYANDPRINCIPLE1.1Applicability.Thismethodisapplicabletothedeterminationofemissionsofpolychlorinateddibenzo-p-dioxins(PCDD's)andpolychlorinateddibenzofurans(PCDF's)fromstationarysources.1.2Principle.Asampleiswithdrawnisokineticallyfromthegasstreamandcollectedinthesampleprobe,onaglassfiberfilter,andonapackedcolumnofadsorbentmaterial.Thesamplecannotbeseparatedintoaparticleandvaporfraction.ThePCDD'sandPCDF'sareextractedfromthesample,separatedbyhighresolutiongaschromatography(HRGC),andmeasuredbyhighresolutionmassspectrometry(HRMS).2.APPARATUS2.1Sampling.AschematicofthesamplingtrainisshowninFigure23-1.Sealinggreasesmaynotbeusedinassemblingthetrain.ThetrainisidenticaltothatdescribedinSection2.1ofMethod5ofthisappendixwiththefollowingadditions:2.1.1Nozzle.Thenozzleshallbemadeofnickel,nickel-platedstainlesssteel,quartz,orborosilicateglass.2.1.2SampleTransferLines.Thesampletransferlines,ifneeded,shallbeheattraced,heavywalledTFE(½in.ODwith1/8in.wall)withconnectingfittingsthatarecapableofformingleak-free,vacuum-tightconnectionswithoutusingsealinggreases.Thelineshallbeasshortaspossibleandmustbemaintainedat120°C.2.1.1FilterSupport.TeflonorTeflon-coatedwire.2.1.2Condenser.Glass,coiltypewithcompatiblefittings.AschematicdiagramisshowninFigure23-2.2.1.3WaterBath.Thermostaticallycontrolledtomaintainthegastemperatureexitingthecondenserat20°C(68°F).2.1.4AdsorbentModule.Glasscontainertoholdthesolidadsorbent.AschematicdiagramisshowninFigure23-2.Otherphysicalconfigurationsoftheresintrap/condenserassemblyareacceptable.Theconnectingfittingsshallformleak-free,vacuumtightseals.Nosealantgreasesshallbeusedinthesamplingtrain.Acoarseglassfritisincludedtoretaintheadsorbent.2.2SampleRecovery.2.2.1FittingCaps.Groundglass,Teflontape,oraluminumfoil(Section2.2.6)tocapoffthesampleexposedsectionsofthetrainandsorbentmodule.2.2.2WashBottles.Teflon,500-mL.2.2.3ProbeLiner,ProbeNozzle,andFilterHolderBrushes.InertbristlebrusheswithprecleanedstainlesssteelorTeflonhandles.TheprobebrushshallhaveextensionsofstainlesssteelorTeflon,atleastaslongastheprobe.Thebrushesshallbeproperlysizedandshapedtobrushoutthenozzle,probeliner,andtransferline,ifused.2.2.4FilterStorageContainer.Sealedfilterholder,wide-mouthamberglassjarwithTeflon-linedcap,glasspetridish.2.2.5Balance.Triplebeam.2.2.6AluminumFoil.Heavyduty,hexane-rinsed.2.2.7MetalStorageContainer.Airtightcontainertostoresilicagel.2.2.8GraduatedCylinder.Glass,250-mLwith2-mLgraduations.2.2.9GlassSampleStorageContainers.Amberglassbottlesforsampleglasswarewashes,500-or1000-mL,withleakfreeTeflon-linedcaps.2.3Analysis.2.3.1SampleContainers.125-and250-mLflintglassbottleswithTeflon-linedcaps.2.3.2TestTubes.Glass.2.3.3SoxhletExtractionApparatus.Capableofholding43x123mmextractionthimbles.2.3.4ExtractionThimble.Glass,precleanedcellulosic,orglassfiber.2.3.5PasteurPipettes.Forpreparingliquidchromatographiccolumns.2.3.6Reacti-vials.Amberglass,2-mL,silanizedpriortouse.2.3.7RotaryEvaporator.Buchi/BrinkmanRF-121orequivalent.2.3.8NitrogenEvaporativeConcentrator.N-EvapAnalyticalEvaporatorModelIIIorequivalent.2.3.9SeparatoryFunnels.Glass,2-liter.2.3.10GasChromatograph.Consistingofthefollowingcomponents:2.3.10.1Oven.Capableofmaintainingtheseparationcolumnattheproperoperatingtemperature+10°Candperformingprogrammedincreasesintemperatureatratesofatleast40°C/min.2.3.10.2TemperatureGauges.Tomonitorcolumnoven,detector,andexhausttemperatures+1°C.2.3.10.3FlowSystems.Gasmeteringsystemtomeasuresample,fuel,combustiongas,andcarriergasflows.2.3.10.4CapillaryColumns.Afusedsilicacolumn,60x0.25mminsidediameter(ID),coatedwithDB-5andafusedsilicacolumn,30mx0.25mmIDcoatedwithDB-225.Othercolumnsystemsmaybesubstitutedprovidedthattheuserisabletodemonstrate,usingcalibrationandperformancechecks,thatthecolumnsystemisabletomeetthespecificationsofSection6.1.2.2.2.3.11MassSpectrometer.Capableofroutineoperationataresolutionof1:10000withastabilityof+5ppm.2.3.12DataSystem.Compatiblewiththemassspectrometerandcapableofmonitoringatleastfivegroupsof25ions.2.3.13AnalyticalBalance.Tomeasurewithin0.1mg.3.REAGENTS3.1Sampling.3.1.1Filters.Glassfiberfilters,withoutorganicbinder,exhibitingatleast99.95percentefficiency(0.05percentpenetration)on0.3-microndioctylphthalatesmokeparticles.ThefilterefficiencytestshallbeconductedinaccordancewithASTMStandardMethodD2986-71(Reapproved1978)(incorporatedbyreference-see§60.17).3.1.1.1Precleaning.Allfiltersshallbecleanedbeforetheirinitialuse.Placeaglassextractionthimbleand1gofsilicagelandaplugofglasswoolintoaSoxhletapparatus,chargetheapparatuswithtoluene,andrefluxforaminimumof3hours.Removethetolueneanddiscardit,butretainthesilicagel.Placenomorethan50filtersinthethimbleontothesilicagelbedandtopwiththecleanedglasswool.ChargetheSoxhletwithtolueneandrefluxfor16hours.Afterextraction,allowtheSoxhlettocool,removethefilters,anddrythemunderacleannitrogen(N2)stream.StorethefiltersinaglasspetridishsealedwithTeflontape.3.1.2Ads