EPA Method 13A

844METHOD13A-DETERMINATIONOFTOTALFLUORIDEEMISSIONSFROMSTATIONARYSOURCES(SPADNSZIRCONIUMLAKEMETHOD)NOTE:Thismethoddoesnotincludeallofthespecifications(e.g.,equipmentandsupplies)andprocedures(e.g.,samplingandanalytical)essentialtoitsperformance.Somematerialisincorporatedbyreferencefromothermethodsinthispart.Therefore,toobtainreliableresults,personsusingthismethodshouldhaveathoroughknowledgeofatleastthefollowingadditionaltestmethods:Method1,Method2,Method3,andMethod5.1.0ScopeandApplication.1.1Analytes.AnalyteCASNo.SensitivityTotalfluoridesasFluorine7782-41-4Notdetermined1.2Applicability.Thismethodisapplicableforthedeterminationoffluoride(F-)emissionsfromsourcesasspecifiedintheregulations.Itdoesnotmeasurefluorocarbons,suchasFreons.1.3DataQualityObjectives.Adherencetotherequirementsofthismethodwillenhancethequalityofthedataobtainedfromairpollutantsamplingmethods.2.0Summary.GaseousandparticulateF-arewithdrawnisokineticallyfromthesourceandcollectedinwaterandon845afilter.ThetotalF-isthendeterminedbytheSPADNSZirconiumLakeColorimetricmethod.3.0Definitions.[Reserved]4.0Interferences.4.1Chloride.Largequantitiesofchloridewillinterferewiththeanalysis,butthisinterferencecanbepreventedbyaddingsilversulfateintothedistillationflask(seeSection11.3).Ifchlorideionispresent,itmaybeeasiertousethespecificionelectrodemethodofanalysis(Method13B).4.2Grease.Greaseonsample-exposedsurfacesmaycauselowF-resultsduetoadsorption.5.0Safety.5.1Disclaimer.Thismethodmayinvolvehazardousmaterials,operations,andequipment.Thistestmethodmaynotaddressallofthesafetyproblemsassociatedwithitsuse.Itistheresponsibilityoftheuserofthistestmethodtoestablishappropriatesafetyandhealthpracticesandtodeterminetheapplicabilityofregulatorylimitationspriortoperformingthistestmethod.5.2CorrosiveReagents.Thefollowingreagentsarehazardous.Personalprotectiveequipmentandsafeproceduresareusefulinpreventingchemicalsplashes.Ifcontactoccurs,immediatelyflushwithcopiousamountsof846wateratleast15minutes.Removeclothingundershoweranddecontaminate.Treatresidualchemicalburnasthermalburn.5.2.1HydrochloricAcid(HCl).Highlytoxic.Vaporsarehighlyirritatingtoeyes,skin,nose,andlungs,causingseveredamage.Maycausebronchitis,pneumonia,oredemaoflungs.Exposuretoconcentrationsof0.13to0.2percentcanbelethalinminutes.Willreactwithmetals,producinghydrogen.5.2.2SodiumHydroxide(NaOH).Causesseveredamagetoeyetissuesandtoskin.Inhalationcausesirritationtonose,throat,andlungs.Reactsexothermicallywithlimitedamountsofwater.5.2.3SulfuricAcid(H2SO4).Rapidlydestructivetobodytissue.Willcausethirddegreeburns.Eyedamagemayresultinblindness.Inhalationmaybefatalfromspasmofthelarynx,usuallywithin30minutes.Maycauselungtissuedamagewithedema.1mg/m3for8hourswillcauselungdamageor,inhigherconcentrations,death.Provideventilationtolimitinhalation.Reactsviolentlywithmetalsandorganics.6.0EquipmentandSupplies.6.1SampleCollection.AschematicofthesamplingtrainusedinperformingthismethodisshowninFigure84713A-1;itissimilartotheMethod5samplingtrainexceptthatthefilterpositionisinterchangeable.Thesamplingtrainconsistsofthefollowingcomponents:6.1.1ProbeNozzle,PitotTube,DifferentialPressureGauge,FilterHeatingSystem,TemperatureSensor,MeteringSystem,Barometer,andGasDensityDeterminationEquipment.SameasMethod5,Sections6.1.1.1,6.1.1.3through6.1.1.7,6.1.1.9,6.1.2,and6.1.3,respectively.Thefilterheatingsystemandtemperaturesensorareneededonlywhenmoisturecondensationisaproblem.6.1.2ProbeLiner.Borosilicateglassor316stainlesssteel.Whenthefilterislocatedimmediatelyaftertheprobe,aprobeheatingsystemmaybeusedtopreventfilterpluggingresultingfrommoisturecondensation,butthetemperatureintheprobeshallnotbeallowedtoexceed120±14EC(248±25EF).6.1.3FilterHolder.Withpositivesealagainstleakagefromtheoutsideoraroundthefilter.Ifthefilterislocatedbetweentheprobeandfirstimpinger,useborosilicateglassorstainlesssteelwitha20-meshstainlesssteelscreenfiltersupportandasiliconerubbergasket;donotuseaglassfritorasinteredmetalfiltersupport.Ifthefilterislocatedbetweenthethirdandfourthimpingers,borosilicateglasswithaglassfritfiltersupportandasiliconerubbergasketmaybeused.848Othermaterialsofconstructionmaybeused,subjecttotheapprovaloftheAdministrator.6.1.4Impingers.FourimpingersconnectedasshowninFigure13A-1withground-glass(orequivalent),vacuum-tightfittings.Forthefirst,third,andfourthimpingers,usetheGreenburg-Smithdesign,modifiedbyreplacingthetipwitha1.3-cm(1/2-in.)IDglasstubeextendingto1.3cm(1/2in.)fromthebottomoftheflask.Forthesecondimpinger,useaGreenburg-Smithimpingerwiththestandardtip.Modifications(e.g.,flexibleconnectionsbetweentheimpingersormaterialsotherthanglass)maybeused,subjecttotheapprovaloftheAdministrator.Placeatemperaturesensor,capableofmeasuringtemperaturetowithin1EC(2EF),attheoutletofthefourthimpingerformonitoringpurposes.6.2SampleRecovery.Thefollowingitemsareneededforsamplerecovery:6.2.1Probe-linerandProbe-NozzleBrushes,WashBottles,GraduatedCylinderand/orBalance,PlasticStorageContainers,FunnelandRubberPoliceman,andFunnel.SameasMethod5,Sections6.2.1,6.2.2and6.2.5to6.2.8,