EPA Method 13B

874METHOD13B-DETERMINATIONOFTOTALFLUORIDEEMISSIONSFROMSTATIONARYSOURCES(SPECIFICIONELECTRODEMETHOD)NOTE:Thismethoddoesnotincludeallofthespecifications(e.g.,equipmentandsupplies)andprocedures(e.g.,samplingandanalytical)essentialtoitsperformance.Somematerialisincorporatedbyreferencefromothermethodsinthispart.Therefore,toobtainreliableresults,personsusingthismethodshouldhaveathoroughknowledgeofatleastthefollowingadditionaltestmethods:Method1,Method2,Method3,Method5,andMethod13A.1.0ScopeandApplication.1.1Analytes.AnalyteCASNo.SensitivityTotalfluoridesasFluorine7782-41-4Notdetermined1.2Applicability.Thismethodisapplicableforthedeterminationoffluoride(F-)emissionsfromsourcesasspecifiedintheregulations.Itdoesnotmeasurefluorocarbons,suchasFreons.1.3DataQualityObjectives.Adherencetotherequirementsofthismethodwillenhancethequalityofthedataobtainedfromairpollutantsamplingmethods.8752.0Summary.GaseousandparticulateF-arewithdrawnisokineticallyfromthesourceandcollectedinwaterandonafilter.ThetotalF-isthendeterminedbythespecificionelectrodemethod.3.0Definitions.[Reserved]4.0Interferences.Greaseonsample-exposedsurfacesmaycauselowF-resultsbecauseofadsorption.5.0Safety.5.1Disclaimer.Thismethodmayinvolvehazardousmaterials,operations,andequipment.Thistestmethoddoesnotpurporttoaddressallofthesafetyproblemsassociatedwithitsuse.Itistheresponsibilityoftheuserofthistestmethodtoestablishappropriatesafetyandhealthpracticesandtodeterminetheapplicabilityofregulatorylimitationspriortoperformingthistestmethod.5.2CorrosiveReagents.Thefollowingreagentsarehazardous.Personalprotectiveequipmentandsafeproceduresareusefulinpreventingchemicalsplashes.Ifcontactoccurs,immediatelyflushwithcopiousamountsofwateratleast15minutes.Removeclothingundershoweranddecontaminate.Treatresidualchemicalburnasthermalburn.8765.2.1SodiumHydroxide(NaOH).Causesseveredamagetoeyetissuesandtoskin.Inhalationcausesirritationtonose,throat,andlungs.Reactsexothermicallywithlimitedamountsofwater.5.2.2SulfuricAcid(H2SO4).Rapidlydestructivetobodytissue.Willcausethirddegreeburns.Eyedamagemayresultinblindness.Inhalationmaybefatalfromspasmofthelarynx,usuallywithin30minutes.Maycauselungtissuedamagewithedema.1mg/m3for8hourswillcauselungdamageor,inhigherconcentrations,death.Provideventilationtolimitinhalation.Reactsviolentlywithmetalsandorganics.6.0EquipmentandSupplies.6.1SampleCollectionandSampleRecovery.SameasMethod13A,Sections6.1and6.2,respectively.6.2SamplePreparationandAnalysis.Thefollowingitemsarerequiredforsamplepreparationandanalysis:6.2.1DistillationApparatus,BunsenBurner,ElectricMuffleFurnace,Crucibles,Beakers,VolumetricFlasks,ErlenmeyerFlasksorPlasticBottles,ConstantTemperatureBath,andBalance.SameasMethod13A,Sections6.3.1to6.3.9,respectively.6.2.2FluorideIonActivitySensingElectrode.8776.2.3ReferenceElectrode.Singlejunction,sleevetype.6.2.4Electrometer.ApHmeterwithmillivolt-scalecapableof±0.1-mvresolution,oraspecificionmetermadespecificallyforspecificionelectrodeuse.6.2.5MagneticStirrerandTetrafluoroethylene(TFE)Fluorocarbon-CoatedStirringBars.6.2.6Beakers.Polyethylene,100-ml.7.0ReagentsandStandards.Unlessotherwiseindicated,allreagentsaretoconformtothespecificationsestablishedbytheCommitteeonAnalyticalReagentsoftheAmericanChemicalSociety,wheresuchspecificationsareavailable.Otherwise,usethebestavailablegrade.7.1SampleCollectionandSampleRecovery.SameasMethod13A,Sections7.1and7.2,respectively.7.2SamplePreparationandAnalysis.Thefollowingreagentsandstandardsarerequiredforsampleanalysis:7.2.1CalciumOxide(CaO).Certifiedgradecontaining0.005percentF-orless.7.2.2PhenolphthaleinIndicator.Dissolve0.1gphenolphthaleininamixtureof50mlof90percentethanoland50mlwater.7.2.3SodiumHydroxide(NaOH),Pellets.8787.2.4SulfuricAcid(H2SO4),Concentrated.7.2.5Filters.WhatmanNo.541,orequivalent.7.2.6Water.SameasSection7.1.2ofMethod13A.7.2.7SodiumHydroxide,5M.Dissolve20gofNaOHin100mlofwater.7.2.8SulfuricAcid,25Percent(v/v).Mix1partofconcentratedH2SO4with3partsofwater.7.2.9TotalIonicStrengthAdjustmentBuffer(TISAB).Placeapproximately500mlofwaterina1-literbeaker.Add57mlofglacialaceticacid,58gofsodiumchloride,and4gofcyclohexylenedinitrilotetraaceticacid.Stirtodissolve.Placethebeakerinawaterbathandcoolto20EC(68EF).Slowlyadd5MNaOHtothesolution,measuringthepHcontinuouslywithacalibratedpH/referenceelectrodepair,untilthepHis5.3.Pourintoa1-litervolumetricflask,anddilutetovolumewithdeionized,distilledwater.CommerciallypreparedTISABmaybesubstitutedfortheabove.7.2.10FluorideStandardSolution,0.1M.Ovendryapproximately10gofsodiumfluoride(NaF)foraminimumof2hoursat110EC(230EF),andstoreinadesiccator.Thenadd4.2gofNaFtoa1-litervolumetricflask,andaddenoughwatertodissolve.Dilutetovolumewithwater.8798.0SampleCollection,Preservation,Storage,andTransport.SameasMethod13A,Section8.0.9.0QualityControl.9.1MiscellaneousQualityControlMeasures.SectionQualityControlMeasureEffect8.0,10.1Samplingequipmentleak-checkandcalibrationEnsureaccuratemeasurementofstackgasflowrateandsamplevolume10.2FluorideelectrodeEvaluateanalyticaltechnique,preparatio