EPA Method 308

3.AppendixAofpart63isamendedbyaddingMethod308innumericalordertoreadasfollows:AppendixAtoPart63--TestMethods*****Method308--ProcedureforDeterminationofMethanolEmissionfromStationarySources1.0ScopeandApplication.1.1Analyte.Methanol.ChemicalAbstractService(CAS)No.67-56-1.1.2Applicability.Thismethodappliestothemeasurementofmethanolemissionsfromspecifiedstationarysources.2.0SummaryofMethod.Agassampleisextractedfromthesamplingpointinthestack.Themethanoliscollectedindeionizeddistilledwaterandadsorbedonsilicagel.Thesampleisreturnedtothelaboratorywherethemethanolinthewaterfractionisseparatedfromotherorganiccompoundswithagaschromatograph(GC)andisthenmeasuredbyaflameionizationdetector(FID).Thefractionadsorbedonsilicagelisextractedwithanaqueoussolutionofn-propanolandisthenseparatedandmeasuredbyGC/FID.3.0Definitions.[Reserved]4.0Interferences.[Reserved]5.0Safety.5.1Disclaimer.Thismethodmayinvolvehazardousmaterials,operations,andequipment.Thistestmethoddoesnotpurporttoaddressallofthesafetyproblemsassociatedwithitsuse.Itistheresponsibilityoftheuserofthistestmethodtoestablishappropriatesafetyandhealthpracticesandtodeterminetheapplicabilityofregulatorylimitationsbeforeperformingthistestmethod.5.2MethanolCharacteristics.Methanolisflammableandadangerousfireandexplosionrisk.Itismoderatelytoxicbyingestionandinhalation.6.0EquipmentandSupplies.6.1SampleCollection.Thefollowingitemsarerequiredforsamplecollection:6.1.1SamplingTrain.ThesamplingtrainisshowninFigure308-1andcomponentpartsarediscussedbelow.6.1.1.1Probe.Teflon®,approximately6-millimeter(mm)(0.24inch)outsidediameter.6.1.1.2Impinger.A30-milliliter(ml)midgetimpinger.Theimpingermustbeconnectedwithleak-freeglassconnectors.Siliconegreasemaynotbeusedtolubricatetheconnectors.6.1.1.3AdsorbentTube.Glasstubespackedwiththerequiredamountofthespecifiedadsorbent.6.1.1.4Valve.Needlevalve,toregulatesamplegasflowrate.6.1.1.5Pump.Leak-freediaphragmpump,orequivalent,topullgasthroughthesamplingtrain.Installasmallsurgetankbetweenthepumpandratemetertoeliminatethepulsationeffectofthediaphragmpumpontherotameter.6.1.1.6RateMeter.Rotameter,orequivalent,capableofmeasuringflowratetowithin2percentoftheselectedflowrateofupto1000milliliterperminute(ml/min).Alternatively,thetestermayuseacriticalorificetosettheflowrate.6.1.1.7VolumeMeter.Drygasmeter(DGM),sufficientlyaccuratetomeasurethesamplevolumetowithin2percent,calibratedattheselectedflowrateandconditionsactuallyencounteredduringsampling,andequippedwithatemperaturesensor(dialthermometer,orequivalent)capableofmeasuringtemperatureaccuratelytowithin3oC(5.4oF).6.1.1.8Barometer.Mercury(Hg),aneroid,orotherbarometercapableofmeasuringatmosphericpressuretowithin2.5mm(0.1inch)Hg.SeetheNOTEinMethod5(40CFRpart60,appendixA),section6.1.2.6.1.1.9VacuumGaugeandRotameter.Atleast760-mm(30-inch)Hggaugeand0-to40-ml/minrotameter,tobeusedforleak-checkofthesamplingtrain.6.2SampleRecovery.Thefollowingitemsarerequiredforsamplerecovery:6.2.1WashBottles.Polyethyleneorglass,500-ml,two.6.2.2SampleVials.Glass,40-ml,withTeflon®-linedsepta,tostoreimpingersamples(onepersample).6.2.3GraduatedCylinder.100-mlsize.6.3Analysis.Thefollowingarerequiredforanalysis:6.3.1GasChromatograph.GCwithanFID,programmabletemperaturecontrol,andheatedliquidinjectionport.6.3.2Pump.Capableofpumping100ml/min.Forflushingsampleloop.6.3.3FlowMeter.Tomonitoraccuratelysampleloopflowrateof100ml/min.6.3.4Regulators.Two-stageregulatorsusedongascylindersforGCandforcylinderstandards.6.3.5Recorder.Torecord,integrate,andstorechromatograms.6.3.6Syringes.1.0-and10-microliter(l)size,calibrated,forinjectingsamples.6.3.7TubingFittings.Stainlesssteel,toplumbGCandgascylinders.6.3.8Vials.Two5.0-mlglassvialswithscrewcapsfittedwithTeflon®-linedseptaforeachsample.6.3.9Pipettes.Volumetrictype,assortedsizesforpreparingcalibrationstandards.6.3.10VolumetricFlasks.Assortedsizesforpreparingcalibrationstandards.6.3.11Vials.Glass40-mlwithTeflon®-linedsepta,tostorecalibrationstandards(oneperstandard).7.0ReagentsandStandards.NOTE:Unlessotherwiseindicated,allreagentsmustconformtothespecificationsestablishedbytheCommitteeonAnalyticalReagentsoftheAmericanChemicalSociety.Wheresuchspecificationsarenotavailable,usethebestavailablegrade.7.1Sampling.Thefollowingarerequiredforsampling:7.1.1Water.DeionizeddistilledtoconformtotheAmericanSocietyforTestingandMaterials(ASTM)SpecificationD1193-77,Type3.Attheoptionoftheanalyst,thepotassiumpermanganate(KMnO4)testforoxidizableorganicmattermaybeomittedwhenhighconcentrationsoforganicmatterarenotexpectedtobepresent.7.1.2SilicaGel.Deactivatedchromatographicgrade20/40meshsilicagelpackedinglassadsorbenttubes.Thesilicagelispackedintwosections.Thefrontsectioncontains520milligrams(mg)ofsilicagel,andthebacksectioncontains260mg.7.2Analysis.Thefollowingarerequiredforanalysis:7.2.1Water.Sameasspecifiedinsection7.1.1.7.2.2n-Propanol,3Percent.Mix3mlofn-propanolwith97mlofwater.7.2.3MethanolStockStandard.Prepareamethanolstockstandardbyweighing1gramofmethanolintoa100-mlvolumetricflask.Diluteto100mlwithwater.7.2.3.1MethanolWork