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@ @ A A A& : ; < = > ? @ A A A A A @ ? > = < ; :                   &                   1 0 / . - , + * * * * * + , - . / 0 1 &* * * + , - . / 0 1 2 3 4 5 6 7 8 8 8 8 :8 ;8 <7 =6 >5 ?4 @3 A2 A1 A0 A/ A. @- ?, >+ =* <* ;* :CFIG3-2.WPG 6#   -pP p X-,XJ XXXFigure32.IntegratedGasSamplingTrain.Table_C  CRight ParRight-Aligned Paragraph NumbersI.A.1.a.(1)(a)i)a)3|d2 Ha`$"Letter GothicX&d H@7X@<6X9`(CouriericXx6X@`7X@< 9(CourierBoldXx `7X( T$  ((3$ KT!   < 9Z &Courier Regular T M'   RXXXXj%d<( 9Z &Courier RegularF<Q 9Z .Courier New Regular KT!   8*pP hX*    O7~XXdd7NXXXXMETHOD3GASANALYSISFORTHE l DETERMINATIONOFDRYMOLECULARWEIGHT  P   $ DXpP $ NOTE: Thismethoddoesnotincludeallofthe   specifications(e.g.,equipmentandsupplies)andprocedures  r (e.g.,sampling)essentialtoitsperformance.Some  6 materialisincorporatedbyreferencefromothermethodsinthispart.Therefore,toobtainreliableresults,personsusingthismethodshouldalsohaveathoroughknowledgeofMethod1.1.0ScopeandApplication. v   1.1Analytes.*q./ ddd Xdd Xdd X(#(#q,( dd ,Hdd ,8 dd +  301"  3Analyte 201!L01 2CASNo. 201!L01 2Sensitivity C9!L   01 @xCOxygen(O2)  " 7782447  " 2,000ppmv 6," x @ @x6Nitrogen(N2)  | 7727379  | N/A 6,| x @ @x6Carbondioxide(CO2)  j 124389  j 2,000ppmv =1,j  x @ Px=Carbonmonoxide(CO) 21!0!1 2630080 21!0"1 2N/A1'%0# x P  1 1 1.2Applicability.ThismethodisapplicableforthedeterminationofCO2andO2concentrationsanddrymolecular ">' weightofasamplefromaneffluentgasstreamofafossilfuelcombustionprocessorotherprocess. 1.3Othermethods,aswellasmodificationstotheproceduredescribedherein,arealsoapplicableforalloftheabovedeterminations.ExamplesofspecificmethodsandOmodificationsinclude:(1)amultipointgrabsampling B-&3 methodusinganOrsatanalyzertoanalyzetheindividualgrabsampleobtainedateachpoint;(2)amethodformeasuringeitherCO2orO2andusingstoichiometric   calculationstodeterminedrymolecularweight;and(3)assigningavalueof30.0fordrymolecularweight,inlieuofactualmeasurements,forprocessesburningnaturalgas,coal,oroil.Thesemethodsandmodificationsmaybeused,butaresubjecttotheapprovaloftheAdministrator.ThemethodmayalsobeapplicabletootherprocesseswhereithasbeendeterminedthatcompoundsotherthanCO2,O2, P carbonmonoxide(CO),andnitrogen(N2)arenotpresentin  concentrationssufficienttoaffecttheresults. 1.4DataQualityObjectives.Adherencetotherequirementsofthismethodwillenhancethequalityofthedataobtainedfromairpollutantsamplingmethods.2.0SummaryofMethod.  |  2.1Agassampleisextractedfromastackbyoneof "4  thefollowingmethods:(1)singlepoint,grabsampling;(2)singlepoint,integratedsampling;or(3)multipoint,integratedsampling.ThegassampleisanalyzedforpercentCO2andpercentO2.Fordrymolecularweightdetermination, )D#( eitheranOrsatoraFyriteanalyzermaybeusedfortheanalysis. 8-&, 3.0Definitions.[Reserved] l 4.0Interferences. 0  4.1Severalcompoundscaninterfere,tovaryingdegrees,withtheresultsofOrsatorFyriteanalyses.CompoundsthatinterferewithCO2concentrationmeasurement p  includeacidgases(e.g.,sulfurdioxide,hydrogen 4  chloride);compoundsthatinterferewithO2concentration   measurementincludeunsaturatedhydrocarbons(e.g.,acetone, P  acetylene),nitrousoxide,andammonia.AmmoniareactschemicallywiththeO2absorbingsolution,andwhenpresent D intheeffluentgasstreammustberemovedbeforeanalysis.5.0Safety. `  5.1Disclaimer.Thismethodmayinvolvehazardousmaterials,operations,andequipment.Thistestmethodmaynotaddressallofthesafetyproblemsassociatedwithitsuse.Itistheresponsibilityoftheuserofthistestmethodtoestablishappropriatesafetyandhealthpracticesanddeterminetheapplicabilityofregulatorylimitationspriortoperformingthistestmethod. 5.2CorrosiveReagents. 5.2.1AtypicalOrsatanalyzerrequiresfourreagents:agasconfiningsolution,CO2absorbent,O2 h+$* absorbent,andCOabsorbent.Thesereagentsmaycontain ,-&, potassiumhydroxide,sodiumhydroxide,cuprouschloride,cuproussulfate,alkalinepyrogallicacid,and/orchromouschloride.Followmanufacturer'soperatinginstructionsandobserveallwarninglabelsforreagentuse. 5.2.2AtypicalFyriteanalyzercontainszincchloride,hydrochloricacid,andeitherpotassiumhydroxideorchromouschloride.Followmanufacturer'soperatinginstructionsandobserveallwarninglabelsforreagentuse.6.0EquipmentandSupplies.    NOTE: Asanalternativetothesamplingapparatusand D systemsdescribedherein,othersamplingsystems(e.g.,   liquiddisplacement)maybeused,providedsuchsystemsarecapableofobtainingarepresentativesampleandmaintainingaconstantsamplingrate,andare,otherwise,capableofyieldingacceptableresults.UseofsuchsystemsissubjecttotheapprovaloftheAdministrator. 6.1GrabSampling(SeeFigure31). 6.1.1Probe.Stainlesssteelorborosilicateglasstubingequippedwithaninstackoroutofstackfiltertoremoveparticulatematter(aplugofglasswoolissatisfactoryforthispurpose).Anyothermaterials,resistanttotemperatureatsamplingconditionsandinerttoallcomponentsofthegasstream,maybeusedfortheprobe. <-&, Examplesofsuchmaterialsmayincludealuminum,copper,quartzglass,andTeflon. 6.1.2Pump.Aonewaysqueezebulb,orequivalent,totransportthegassampletotheanalyzer. 6.2IntegratedSampling(Figure32). 6.2.1Probe.SameasinSection6.1.1. 6.2.2Condenser.Anaircooledorwatercooledcondenser,orothercondensernogreaterthan250mlthatwillnotremoveO2,CO2,CO,andN2,toremoveexcess   moisturewhichwouldinterferewiththeoperationofthepumpandflowmeter. 6.2.3Valve.Aneedlevalve,toadjustsamplegasflowrate. 6.2.4Pump.Aleakfree,diaphragmtypepump,orequivalent,totransportsamplegastotheflexiblebag.Installasmallsurgetankbetweenthepumpandratemetertoeliminatethepulsationeffectofthediaphragmpumpontheratemeter. 6.2.5RateMeter.Arotameter,orequivalent,capableofmeasuringflowrateto2percentoftheselectedflowrate.Aflowraterangeof500to1000ml/min issuggested. +%*  6.2.6FlexibleBag.Anyleakfreeplastic(e.g., l  Tedlar,Mylar,Teflon)orplasticcoatedaluminum(e.g., 0 aluminizedMylar)bag,orequivalent,havingacapacityconsistentwiththeselectedflowrateanddurationofthetestrun.Acapacityintherangeof55to90liters(1.9to3.2ft3)issuggested.Toleakcheckthebag,connectit @  toawatermanometer,andpressurizethebagto5to10cmH2O(2to4in.H2O).Allowtostandfor10minutes.Any \  displacementinthewatermanometerindicatesaleak.Analternativeleakcheckmethodistopressurizethebagto5to10cm(2to4in.)H2Oandallowtostandovernight.A  deflatedbagindicatesaleak. 6.2.7PressureGauge.AwaterfilledUtubemanometer,orequivalent,ofabout30cm(12in.),fortheflexiblebagleakcheck. 6.2.8VacuumGauge.Amercurymanometer,orequivalent,ofatleast760mm(30in.)Hg,forthesamplingtrainleakcheck. 6.3Analysis.AnOrsatorFyritetypecombustiongasanalyzer.7.0ReagentsandStandards. )P#(  7.1Reagents.AsspecifiedbytheOrsatorFyritetypecombustionanalyzermanufacturer. D-&,  7.2Standards.Twostandardgasmixtures,traceabletoNationalInstituteofStandardsandTechnology(NIST)standards,tobeusedinauditingtheaccuracyoftheanalyzerandtheanalyzeroperatortechnique: 7.2.1.Gascylindercontaining2to4percentO2and |  14to18percentCO2. @   7.2.2.Gascylindercontaining2to4percentCO2and   about15percentO2. \  8.0SampleCollection,Preservation,Storage,and   Transport. D  8.1SinglePoint,GrabSamplingProcedure. 8.1.1Thesamplingpointintheductshalleitherbeatthecentroidofthecrosssectionoratapointnoclosertothewallsthan1.0m(3.3ft),unlessotherwisespecifiedbytheAdministrator. 8.1.2SetuptheequipmentasshowninFigure31,makingsureallconnectionsaheadoftheanalyzeraretight.IfanOrsatanalyzerisused,itisrecommendedthattheanalyzerbeleakcheckedbyfollowingtheprocedureinSection11.5;however,theleakcheckisoptional. 8.1.3Placetheprobeinthestack,withthetipoftheprobepositionedatthesamplingpoint.Purgethesamplinglinelongenoughtoallowatleastfiveexchanges. ,-&, Drawasampleintotheanalyzer,andimmediatelyanalyzeitforpercentCO2andpercentO2accordingtoSection11.2. 0  8.2SinglePoint,IntegratedSamplingProcedure. 8.2.1ThesamplingpointintheductshallbelocatedasspecifiedinSection8.1.1. 8.2.2Leakcheck(optional)theflexiblebagasinSection6.2.6.SetuptheequipmentasshowninFigure32.Justbeforesampling,leakcheck(optional)thetrainbyplacingavacuumgaugeatthecondenserinlet,pullingavacuumofatleast250mmHg(10in.Hg),pluggingtheoutletatthequickdisconnect,andthenturningoffthepump.Thevacuumshouldremainstableforatleast0.5minute.Evacuatetheflexiblebag.Connecttheprobe,andplaceitinthestack,withthetipoftheprobepositionedatthesamplingpoint.Purgethesamplingline.Next,connectthebag,andmakesurethatallconnectionsaretight. 8.2.3SampleCollection.Sampleataconstantrate(10percent).Thesamplingrunshouldbesimultaneouswith,andforthesametotallengthoftimeas,thepollutantemissionratedetermination.Collectionofatleast28liters(1.0ft3)ofsamplegasisrecommended; +%* however,smallervolumesmaybecollected,ifdesired. D-&,  8.2.4Obtainoneintegratedfluegassampleduringeachpollutantemissionratedetermination.Within8hoursafterthesampleistaken,analyzeitforpercentCO2and   percentO2usingeitheranOrsatanalyzeroraFyritetype  L combustiongasanalyzeraccordingtoSection11.3. NOTE: WhenusinganOrsatanalyzer,periodicFyrite @  readingsmaybetakentoverify/confirmtheresultsobtainedfromtheOrsat. 8.3MultiPoint,IntegratedSamplingProcedure. 8.3.1Unlessotherwisespecifiedinanapplicableregulation,orbytheAdministrator,aminimumofeighttraversepointsshallbeusedforcircularstackshavingdiameterslessthan0.61m(24in.),aminimumofnineshallbeusedforrectangularstackshavingequivalentdiameterslessthan0.61m(24in.),andaminimumof12traversepointsshallbeusedforallothercases.ThetraversepointsshallbelocatedaccordingtoMethod1. 8.3.2FollowtheproceduresoutlinedinSections8.2.2through8.2.4,exceptforthefollowing:Traverseallsamplingpoints,andsampleateachpointforanequallengthoftime.RecordsamplingdataasshowninFigure33.  H-&, 9.0QualityControl. l *q23 dd( dd Hdd 8 dd ./(#(#q,dd ,@ dd ,@ dd +  301" * H3Section ;01* H01 ;QualityControlMeasure ;01* H01 ;Effect LB* H  H 01 xL8.2     UseofFyritetoconfirmOrsatresults.     EnsurestheaccuratemeasurementofCO2and    O2. 6, v x  x610.1  < Periodicauditofanalyzerandoperatortechnique.    Ensuresthattheanalyzerisoperatingproperlyandthattheoperatorperformsthesamplingprocedurecorrectlyandaccurately. 90(  x  8x911.3 20!v0 2Replicableanalysesofintegratedsamples. 20!X0 2Minimizesexperimentalerror.1'%X x0 8  0 110.0CalibrationandStandardization. F  10.1Analyzer.Theanalyzerandanalyzeroperator'stechniqueshouldbeauditedperiodicallyasfollows:takeasamplefromamanifoldcontainingaknownmixtureofCO2and % O2,andanalyzeaccordingtotheprocedureinSection11.3. J' Repeatthisprocedureuntilthemeasuredconcentrationofthreeconsecutivesamplesagreeswiththestatedvalue0.5percent.Ifnecessary,takecorrectiveaction,asspecifiedintheanalyzerusersmanual. 10.2Rotameter.Therotameterneednotbecalibrated,butshouldbecleanedandmaintainedaccordingtothemanufacturer'sinstruction.11.0AnalyticalProcedure. ,j&7  11.1Maintenance.TheOrsatorFyritetypeanalyzershouldbemaintainedandoperatedaccordingtothemanufacturersspecifications. 11.2GrabSampleAnalysis.UseeitheranOrsatanalyzeroraFyritetypecombustiongasanalyzertomeasureO2andCO2concentrationfordrymolecularweight @  determination,usingproceduresasspecifiedintheanalyzeruser'smanual.IfanOrsatanalyzerisused,itisrecommendedthattheOrsatleakcheck,describedinSection11.5,beperformedbeforethisdetermination;however,thecheckisoptional.CalculatethedrymolecularweightasindicatedinSection12.0.Repeatthesampling,analysis,andcalculationproceduresuntilthedrymolecularweightsofanythreegrabsamplesdifferfromtheirmeanbynomorethan0.3g/gmole(0.3lb/lbmole).Averagethesethreemolecularweights,andreporttheresultstothenearest0.1g/gmole(0.1lb/lbmole). 11.3IntegratedSampleAnalysis.UseeitheranOrsatanalyzeroraFyritetypecombustiongasanalyzertomeasureO2andCO2concentrationfordrymolecularweight '!& determination,usingproceduresasspecifiedintheanalyzeruser'smanual.IfanOrsatanalyzerisused,itisrecommendedthattheOrsatleakcheck,describedin D-&, Section11.5,beperformedbeforethisdetermination;however,thecheckisoptional.CalculatethedrymolecularweightasindicatedinSection12.0.Repeattheanalysisandcalculationproceduresuntiltheindividualdrymolecularweightsforanythreeanalysesdifferfromtheirmeanbynomorethan0.3g/gmole(0.3lb/lbmole).Averagethesethreemolecularweights,andreporttheresultstothenearest0.1g/gmole(0.1lb/lbmole). 11.4Standardization.AperiodiccheckofthereagentsandofoperatortechniqueshouldbeconductedatleastonceeverythreeseriesoftestrunsasoutlinedinSection10.1. 11.5LeakCheckProcedureforOrsatAnalyzer.MovinganOrsatanalyzerfrequentlycausesittoleak.Therefore,anOrsatanalyzershouldbethoroughlyleakcheckedonsitebeforethefluegassampleisintroducedintoit.TheprocedureforleakcheckinganOrsatanalyzerisasfollows: 11.5.1Bringtheliquidlevelineachpipetteuptothereferencemarkonthecapillarytubing,andthenclosethepipettestopcock. 11.5.2Raisethelevelingbulbsufficientlytobringtheconfiningliquidmeniscusontothegraduatedportionoftheburette,andthenclosethemanifoldstopcock. D-&,  11.5.3Recordthemeniscusposition. 11.5.4Observethemeniscusintheburetteandtheliquidlevelinthepipetteformovementoverthenext4minutes. 11.5.5FortheOrsatanalyzertopasstheleakcheck,twoconditionsmustbemet: 11.5.5.1Theliquidlevelineachpipettemustnotfallbelowthebottomofthecapillarytubingduringthis4minuteinterval. 11.5.5.2Themeniscusintheburettemustnotchangebymorethan0.2mlduringthis4minuteinterval. 11.5.6Iftheanalyzerfailstheleakcheckprocedure,checkallrubberconnectionsandstopcockstodeterminewhethertheymightbethecauseoftheleak.Disassemble,clean,andregreaseanyleakingstopcocks.Replaceleakingrubberconnections.Aftertheanalyzerisreassembled,repeattheleakcheckprocedure.12.0CalculationsandDataAnalysis. p$"  12.1Nomenclature. Md0  L =Drymolecularweight,g/gmole'!& (# (#    L (lb/lbmole). %CO20 L =PercentCO2byvolume,drybasis.t+%*L(#L(#  %O2 0 L =PercentO2byvolume,drybasis.8-&,L(#L(#  %CO 0 L =PercentCObyvolume,drybasis.lL(#L(#  %N2 0 L =PercentN2byvolume,drybasis.0L(#L(#  0.2800 L =MolecularweightofN2orCO,dividedby   Ѐ100. L(#L(#  0.3200 L =MolecularweightofO2dividedby100.| L(#L(#  0.4400 L =MolecularweightofCO2dividedby100.@ L(#L(#  12.2Nitrogen,CarbonMonoxideConcentration.DeterminethepercentageofthegasthatisN2andCOby \  subtractingthesumofthepercentCO2andpercentO2from   100percent. 12.3DryMolecularWeight.UseEquation31tocalculatethedrymolecularweightofthestackgas.8*W9;ZJFz (  p%!@Xdddddddd@Edd w|5   (#(#      (#(#    NOTE :TheaboveEquation31doesnotconsiderthe $ effectoncalculateddrymolecularweightofargonintheeffluentgas.Theconcentrationofargon,withamolecularweightof39.9,inambientairisabout0.9percent.Anegativeerrorofapproximately0.4percentisintroduced.ThetestermaychoosetoincludeargonintheanalysisusingproceduressubjecttoapprovaloftheAdministrator.13.0MethodPerformance.󀀀[Reserved] +%* 14.0PollutionPrevention.[Reserved] H-&, 15.0WasteManagement.[Reserved] l 16.0References. 0  1.Altshuller,A.P.StorageofGasesandVaporsinPlasticBags.InternationalJournalofAirandWaterPollution.6:7581.1963. p   2.Conner,WilliamD.andJ.S.Nader.AirSamplingwithPlasticBags.JournaloftheAmericanIndustrialHygieneAssociation.25:291297.1964. P   3.BurrellManualforGasAnalysts,Seventhedition.BurrellCorporation,2223FifthAvenue,Pittsburgh,PA.15219.1951. 4.Mitchell,W.J.andM.R.Midgett.FieldReliabilityoftheOrsatAnalyzer.JournalofAirPollutionControlAssociation.26:491495.May1976. T  5.Shigehara,R.T.,R.M.Neulicht,andW.S.Smith.ValidatingOrsatAnalysisDatafromFossilFuelFiredUnits.StackSamplingNews.4(2):2126.August1976. "4  17.0Tables,Diagrams,Flowcharts,andValidationData.  d$" ?ABL<8x , `n3'3333@@ElH - l    (#(#                                          (#(#   P    (#(#                                                                  (#(#   ?DE1111K;7x ( `n3'LL @E l  Al  $ *qFG dddd @ dd @ dd 23(#(#q,fdd",td",6td",td"+  /1" N /Time 011!j1 0TraversePoint 011!L11 0Q(liter/min) 011!L11 0%Deviationa F19!j  11 PF 011!" 1 0 011!"  11 0 011!"  11 0 F19!"   P 11 PF 011!  1 0 011!  11 0 011! 11 0 F19!  P 11 PF 011! 1 0 011! 11 0 011! 11 0 F19!  P 11 PF 011!`1 0 011!`11 0 011!`11 0 N11=!` P 11 `NAverage 5111$^ 11 5 2111!^ 111 21'%^   `  111 1 a%Dev.=[(QQavg)/Qavg]x100(Mustbe<+10%) 2   Figure33.SamplingRateData.