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    ( : D D V[V%V[- $d/RR%RQ%QR)R%R)NNN $NzN  "--{p     -  "-$  $ 4   *u)*u%u*) $>.D29D2%2D9 $LY%Y%Y%;;; $;5c;V$V%V$ $3}}}.%}+=Rh}}}"}%j/Y?MRFeHwQ`r}_o_%_ol%lljl%ljeee%e&&%&%FF%F%e4e%e4%S%S666%666&646&%&646646764%4676:7V7:7%7:7V777%777777%777v77v7%7v7777%77W77W7%7W7777%7777h777%777hh7j7h7%7h7jL\L%L\ ]E] ]%] ]E nEn n%n nEjjj%jjj j4j % j4jj4j7j4%4j7jE\E\E\,%\EmEtG|IOV]dyjqlml\lSlMhGbDZETIMOH\EVV%VVV%VlnVln%nlif Vl[Vl[ %[l\tbq3J V%%%%sls%slWPW%WP;4;%;4%%*1*%*1FMF%FMbib%bi~~%~%%%.% #%r`TNOXgz"%5Kd\BegbVC,H"% 8\yzLorNV'H Hbbb% bRRR|Ztb|s{skbbb`i`% `YPIAIPYiii`iyy% y p g `X`)g1p) yKESEKE% EKVCV:V3M+E35:.C5S>SESEKESq~y~q~% ~qibZQ~Zobgioywy~y~q~yyBByB% ByRqRiRbKZBb4i,q4<BByBIePeIe% eIvAv9v0n)e0U9NAUP^PePeIeP% xox% yqyPPP% P___XzP@8@HPPPosxsos% sof^W{NsWd^[fdxlxsxsosxY`Y% Y P I A9AIP```Y`$$$% $555{-q${ $$$% )0) t<% +P|-:DMUY^acghjnpqt:::% :KKKBw:+#+3:::% n!v!n!% !n2f2^2U*N!U^ fvv!v!n!v.%r`TNOXgz  "--    "-$     "Arial- --2 1 Dry GasS'; ZA: 2  Meter`A A'  2 Ice!:A  2 zBathMA!@ 2 8eVacuumNA:AA`  2 LineAAA  2  Main_AA 2 ValveMA;@ 2 I VacuumNA:AA` 2 GaugeZAAA@ 2  By-passM;&AA;: 2 GValveMA;A  2 PumpN@`A 2 =OrificeZ' ;A 2  TemperatureGA_AA'@!A&A 2 4 SensorsMAA;A&; 2  ThermometerGA@'`A_A!@' 2 J Check ValveTA@;; MA;A 2 e Silica GelN;A ZA 2 [ ThermometerGAA&`A`A A' 2 hm TemperatureGA_AA'@!A&A 2 SensorMAA:A' 2 iStackM!A:;  2 9WallnA 2  Glass ProbeZA:;!M&AAA 2  Manometer`@AA`A A' !2 -S-Type Pitot TubeM&H:AA N A !GAA@ 2 J GooseneckZ@A;AAA:; 2 )NozzleSA;;A $2 Glass Filter HolderZA;:!G!A&!SAAA& 2 j LinerAAA& 2 EmptyM`A ; 2  Manometer`@AA`A A' 2 #?0.1 NA!A S  2 (NaOHT@ZS 2 | ThermometerGAA'_A`A A' 92 |!Impingers with Absorbing Solution `AAAA&; T A!MA:A'AAA MAA!AA 2 1 (see below) ':AA AAAT& 2 Y AcidifiedM;A!AA 2 10% Pb AcetateAAg!MA N:A!@!A -- $ss  "-  "-ssssu|$9@U\qx 5<QXmt18MTipohSL70slWP;4wp[T?8#{ts-"Arial- --m2 DFigure XHCN-2. HCN Sampling Train, Lead Acetate/NaOH Configuration @ZAMAAAAA@@YAAAAMMAAMAZMAA   "-%-- $&d`d`&  "-  "-d,d3dHdOh`o`````````````,`3`H`O`d`k``````````` ``(`/`D`K```g`|````````````$`+`@`G`\`c`x``````````]VA:&&&&&&&&&&t&m&X&Q&<&5& &&&&&&&&&&&&x&q&\&U&@&9&$&&&&&&&&&&&&|&u&`&Y&D&=&(&!& &&&&&&&&&&&y&-(\(  "-%(\q%qq%qq%-- Courier4-g FUNC{Vsub{m(std)}~\=~Vsubmgamma~{TsubstdoverTsubm}~{Psub\bar~+~DeltaH/13.6}over{Psubstd  }~\=~Ksub1Vsubmgamma{Psub\bar~+~DeltaH/13.6}overTsubm}';'7 ORD)"   l #  _ FigureXHCN4.HydrogenCyanidebyIonChromatography(IC) iI=R"EK_TMM)s_VMM[)mMM)(MM)stdMM[))_PMM()std_100WSTMMstdSVMM s8SSAMMnPSPMMsS60S(S1SvSBMMwsdS)=;KMM4=pTMM:spVMM/:mMM:(MM:stdMM/:)dPMMi.sdVMM.s?dAMM.ndWd(d1dGdBMM.ws5d) func{STACKALIGN{I~\=&~{TsubsVsub{m(std)}~Psub{std}100}over{Tsubstd~VsubsthetaAsubnPsubs60(1Bsubws)}#\=&~Ksub4{TsubsVsub{m(std)}}over{PsubsVsubsAsubntheta(1Bsubws)}}}VMMmMM(MM stdMM)=VMM!mw*<qTMM;stdSeTMM/mqPMM;barqqqHsq/q13I q.s q6AePMM/std" = KMMA 1y VMM mM   qPMM+ ;barqq!qHq/q13qq.q6|eTMM/mk M #  _dd5 Eq.XHCN3  ; #  _ Eq.XHCN6 XXCfXX& XFXX1KXXxXX'PwTXXxV7m7(<7std7) ; #  _ Eq.XHCN8 qs w #  _ FigureXHCN4HydrogenCyanidebyIonChromatography(IC)(Continued) ,rAZ"Arial RegularGe1C<<CTABLE A($$   1  TABLE BTABLE CTable_ATABLE B'dxd _ #  _  FigureXHCN3.ExampleDataSheet  $ "  _@X@hT@RP'3 Letter Landscape3''3 Letter Landscape3'TpX!XXXp"!XpX*wq'rddd Xdd Xdd X%%w,dd ,dd ,AdK ,dd ,zdd ,dd ,dd ,dd +  %  <$ % 8.)}}  8 +!  +@%#pX!X"p霺# FIELDDATA C''2, Cp"!XpX0 Run0,# H& H&򀀀,#H&,#H& 0 Page1of򀀀 F<+pp H& H& <$ '' $ F * ..  * +!RR   + * ..  * 'RR  ' 5'(RR  $  <$5Plant '':: ' ' '':: ' 'ProbeLengthandType '':: ' ' '':: ' 'HeightofLocation(ft) ''::' ' +'::'  + F<2:: ' <$ ' <$FDate  44   44 NozzleID(In.)  44   44 DuctDimensions(In)  44   44  & <$  <$&SamplingLocation  ..   .. MeterBoxNumber  ..   .. FilterNumber  ..   ..  & <$  <$&SampleType  ((   (( MeterH@  ((   ((  AssumedMoisture(%)  ((!   (("  &" <$  <$&RunNumber  ""#   ""$ Yd  ""%   ""& O2(%)  ""'   ""(  &( <$  <$&Operator  )   * KFactor  +   , CO2(%)  -   .  &. <$  <$&AmbientTemperature($F)    /     0 ProbeHeaterSetting($F)    1     2 O2/CO2Method    3     4  &4 <$  <$&BarometricPressure(in)    5     6 HeaterBoxSetting($F)    7     8 MoistureCollected(g)    9     :  & : <$  <$&StaticPressure(inH2O)   ;    < InitialLeakcheck   =    > FinalLeakcheck   ?    @ " @ <$  "-% DiagramofDuct   @  X      `  ReadandRecordallDataEvery__________Minutes*s1'td ddd dd AdK dd zdd dd dd dd q'r%%,<< ,<< ,<< ,<< ,<< ,9<< ,<< ,<< ,<< ,<< ,<< ,<< ,<< +  +!  B 0$+#pX!X"pD#pw D'w!XpXTraverse , , C PointNumber <2#LLE" <SamplingTime(min) <2#LLH" <Clock , , I Time(24hr) <2#LLK" <GasMeterReadingVm(ft3) <2#O"JJ <VelocityHeadP LLR (inH2O) <2#S"JJ <OrificePressureDifferentialH(inH2O) <2#W"JJ <FlueGasTemperature($F) <2#LLZ"  <ProbeTemperature($F) <2#LL]" <FilterTemperature($F) <2#LL`" <DryGasMeterTemperature .$ b" .ImpingerExit($F) <2#LLe"  <PumpVacuum(in.Hg) J@)LLh"  0$ 0$J % pph % % pph % % pph % % pph % % pph % % pph % % pph % % pph % ! pph !Inlet i ($F) '00j" 'Outlet k ($F) +!00l" + % ppl % &ppl 0$  0$&  m   n   o   p   q   r   s   t   u   v   w   x  #y 0$ 0$#  z   {   |   }   ~                       # 0$ 0$#                                     # 0$ 0$#                                     # 0$ 0$#                                     # 0$ 0$#                                     # 0$ 0$#  ll   ll   ll   ll   ll   ll   ll   ll   ll   ll   ll   ll  #ll 0$ 0$#  PP   PP   PP   PP   PP   PP   PP   PP   PP   PP   PP   PP  #PP 0$ 0$#  44   44   44   44   44   44   44   44   44   44   44   44  #44 0$ 0$#                                     # 0$ 0$#                                    #pX!X'wpw DV# 0$  Comments: #X^X!XpX#,rAZ"Arial RegularTABLE ATABLE B  XHCN No.aMSDSsVollaroPHIonPacpreweighingVmprelabeledprecleanedinterferentsLimitsaLinearityreprepare intercomponent AICm2 Bwsdimensionless EAC ppbvFW ithLp MVOLMw Pbar Pstd RVOL SVOLTs Tstd VadjValiq VlcVw scm scf#wip L.M. J.W. J.L. R.G. !  _     METHODXHCNSAMPLINGANDANALYSISFORHYDROGENCYANIDE d EMISSIONSFROMSTATIONARYSOURCES   &  1.0  ScopeAndApplication.      1.1 ` ' ?MethodXHCNisapplicabletothecollectionandanalysisofhydrogencyanide   (HCN)inthegasphaseandinsuspendedwaterdroplets.TableXHCN1providestheChemicalAbstractService(CAS)number,retentiontime,anddetectionlimitforhydrogencyanide.Thismethodhasbeenevaluatedforcollectionofhydrogencyanideinthelaboratoryandisbelievedtobeapplicabletoprocesseswherehydrogencyanidemightbeemitted.Thismethodisnotinclusivewithrespecttospecifications(e.g.,equipmentandsupplies)andsamplingproceduresessentialtoitsperformance.Somematerialisincorporatedbyreferencefromothermethodsinthesamplingprocedure.Therefore,toobtainreliableresults,personsusingthismethodshouldhaveathoroughknowledgeofatleastthefollowingtestmethods:40CFRPart60AppendixA,Method1,Method2,Method3,Method4,andMethod5(Reference1).  1.2  ` Ifdesired,particulatemattermayberecoveredfromthefilterandanalyzed ( followingtheproceduresofMethod5(Reference1).  1.3 ` Whenthismethodisusedtoanalyzeunfamiliarsamplematrices,compound  identificationshouldbesupportedbyaleastoneadditionalqualitativetechnique.Anion-selectiveelectrode(ISE)maybeusedforthequalitativeconfirmationofresultsforthetargetanalytes.  1.4 ` Themethoddetectionlimit(MDL)isshownbelow,andinTableXHCN1.The h MDLforaspecificsamplemaydifferfromtheMDLlistedinTableXHCN1dependingonthenatureofinterferencesinthesamplematrix,thevolumeofsamplecollected,theamountofsampleusedintheprocedure,andtheuseofsampleconcentrationprocedures.*} 'Sddd Xdd Xdd X(#(#},dd ,dd ,dd,dd +  .;' l .CompoundName >;'-l";' >CASNo.a >;'-l";' >RetentionTime(minutes) >;'-X";' >MethodDetectionLimits(MDL)(g/m3) 3)$ D!"  ;' 3HydrogenCyanide .$("" .74908 XN("#" @6.7@X6.7 xn@("$U @6.7 @  (@12(@x12OEC("%"  (@12  (@ O*,X` XX*KhXa0  ChemicalAbstractServicesRegistryNumber#XF-XK #D#%(#(# - ,XX,X` X-  1.5 ` Samplecollectionunderthismethodmustbeperformedbytesterstrainedand $' experiencedwithisokineticsamplingtechniques.Theanalyticalproceduresinthismethodarerestrictedtouseby,orunderthesupervisionof,analystsexperiencedintheuseofchromatographyandintheinterpretationofchromatograms.Eachanalystmustdemonstratetheabilitytogenerateacceptableresultswiththismethod.  )0#,  &   2.0  SummaryofMethod.  d   2.1 ` 'dGaseousandparticulatepollutantsarewithdrawnfromanemissionsourceatan < isokineticsamplingrateandarecollectedinamulticomponentsamplingtrain.Theprimarycomponentsofthesamplingtrainincludeaheatedprobe,aheatedfilter,twoimpingerscontaining0.1Nsodiumhydroxide(NaOH),anemptyimpinger,andanimpingercontainingsilicagel.HydrogencyanidepresentinthestackgasstreamreactswiththeNaOHtoformacyanideion,whichisretainedinthealkalinesolutionuntilanalyzedbyIC.Particulatecyanidesaltsareretainedonthefilter,andarenotanalyzedduringroutineexecutionofthemethod.SamplingisconductedisokineticallybecauseofthesignificantsolubilityofHCNinwaterdropletswhichmaybepresentincombustionstacks,especiallythoseequippedwithwetscrubbersystems.Ifdesired,particulatemattermayberecoveredfromthefilterandanalyzedfollowingtheproceduresofMethod5(Reference1). &  3.0  Definitions.  P    Calibration'PԀCheckStandard 󀄀Calibrationstandardusedtoverifythecalibrationcurve ( beforeanalyzingsamples.  FieldReagentBlank 󀄀Aliquotsofeachreagentusedintheimpingertrainandeach  solutionusedtorecoverthetrainthatarecollectedinthefieldandreturnedtothelaboratoryforanalysis.  FieldSpike 󀄀Analiquotofreagentthatisspikedwithaknownamountofanalyteinthe h fieldandthatisrecoveredusingthesameproceduresasforasample.  FieldTrainBlank 󀄀Asamplingtrainthatisassembled,leakchecked,andrecoveredat D thesamplingarea,asthoughitwereanormaltrainsample,althoughnogaseoussampleiscollected.  IsokineticVariation 󀄀Measure(percentage)ofhowproportionalthesamplingvelocityis p  tothesourcegasvelocity.  LaboratoryMethodBlank 󀄀Blankreagentthatisprocessedthroughthesample L  preparationprocedureswiththesamplesandthatisusedtoevaluatewhetherornotanycontaminationhasoccurredinthelaboratory.  MatrixSpike 󀄀Analiquotofsamplethatisspikedwithaknownamountofanalyteinthe # laboratoryandthencarriedthroughthesamplepreparationprocedureswiththesamples.  ReplicateSample 󀄀Asecondaliquotofsamplethatisprocessedthroughthesample $! preparationprocedureswiththefieldsamples. &  4.0  Interferences.  'T!$   4.1 ` ''Highconcentrationsofacidicgases,includingcarbondioxide,maylowerthepH ),#& ofthesodiumhydroxideimpingersolution.AsthepHoftheimpingersolutiondecreases,theabilityoftheimpingertoretainhydrogencyanidealsodecreases.Theperformanceofthemethod l+%( dependsonmaintainingahighpH(12)intheimpingers.Asaresult,thepHinbothimpingers d mustberoutinelymonitoredthroughoutthedurationofsampling.ThepHintheimpingermaybemonitoredbyaddingapHindicatortotheimpingersolution,byinsertingapHsensorintotheimpinger,orbyroutinelystoppingtherunandmanuallycheckingthepHwithpHpaper.ThepHintheimpingershouldbemonitoredat15minuteintervalsandtheresultsnotedonthesamplingdatasheet.Whensamplingsourcesthatareknownorsuspectedtobehighlyacidic,modifythesamplingprocedureusingoneormoreofthefollowingprecautions:useahigherconcentration(upto1N)ofsodiumhydroxidesolutionintheimpingers,addadditionalimpingerstothetrain,addadditionalimpingersolutiontoeachimpinger,oraddaleadacetateimpingeratthefrontofthetraintoabsorbsomeoftheacidity.AlthoughtheleadacetatesolutionisusedprimarilytoremovesulfideinterferencesasdiscussedinSection4.2,theimpingerwithleadacetatewillalsoreducetheamountofacidgasesreachingthesodiumhydroxideimpingersbycollectingcondensedmoistureandbyscrubbingsomeoftheacidoutofthesampledgas.Priorknowledgeofthequalitativecompositionofthegasstreamwillaidinminimizingthistypeofinterference.Thereagentmustbestoredinanuncontaminatedenvironmentbothbeforeandaftersamplingtominimizeblankproblems.  4.2 ` Sulfideinterfereswiththedeterminationofhydrogencyanideintwoways.First,  concentrationsofsulfidegreaterthan50ppminsolution(25mgofH2Spercubicmeterofairfor  an849Lsample)interferewiththeanalysisofcyanidebecausesulfideelutesbeforecyanide.Thus,thelargesulfidepeakwillcoverupasmallcyanidepeak.Second,cyanideisdegradedovertimeinthepresenceofsulfideatanyconcentration.Thus,whensamplingsourcesknowntocontainsulfide,animpingercontainingleadacetateshouldbeaddedtothetraintoprecipitatesulfideasleadsulfidebeforeitreachesthesodiumhydroxidesolution.Althoughverylittlecyanideisexpectedtocollectintheleadacetateimpinger,itshouldberecoveredasaseparatesampleandanalyzedforcyanideion.  4.3 ` Oxidizingagentsmaydecomposemostofthecyanides.Oxidizingagentsmaybe ` removedduringsamplerecoverybyaddingascorbicacid.However,theaffectofascorbicacidontheICanalysishasnotbeendetermined.Thus,beforeremovingoxidizingagentsusingascorbicacidthetestermustdemonstratethattheascorbicacidwillnotinterferewiththeanalysis.Toremoveoxidizingagents,testadropofthesamplewithpotassiumiodidestarchtestpaper.Abluecolorindicatesthepresenceofoxidizingagents.Toremovetheoxidizingagents,addascorbicacid,afewcrystalsatatime,untiladropofsampleproducesnocoloronthepotassiumiodidestarchindicatorpaper.Thenaddanadditional0.6gofascorbicacidforeachliterofsamplevolume(Reference2).  4.4 ` Methodinterferencesmaybecausedbycontaminantsinsolvents,reagents,oron &L # thesurfacesofglasswareandothersampleprocessinghardware.Thesemethodinterferencesleadtodiscreteartifactsand/orelevatedbaselinesinthechromatograms.Allreagents,glassware,andassociatedlaboratoryhardwaremustberoutinelydemonstratedtobefreefrominterferencesbyanalyzinglaboratoryreagentblanks.  4.4.1 ` Glasswaremustbescrupulouslycleaned.Cleanallglasswareassoonaspossible P+$( afterusebyrinsingwiththelastsolventused.Followthisrinsebywashingtheglasswarewith @,%) hotwateranddetergent,andrinsingwithtapwateranddeionizedwater.Draintheglasswareandthenrinseitusingreagentgradeacetone.Storetheglasswareinacleanenvironmenttopreventanyaccumulationofdustorothercontaminants.  4.4.2 ` Usehighpurityreagentsandsolventstominimizeinterferenceproblems.Purify (  solventsbydistillationinanallglasssystemifrequired.ffff  4.5 ` Matrixinterferencesmaybecausedbycontaminantsthatareabsorbedfromthe   sample.Theextentofmatrixinterferencesmayvaryconsiderablyfromsourcetosource,dependinguponthenatureanddiversityoftheemissionmatrixbeingsampled.Ifinterferencesoccurinsubsequentsamples,somecleanupofthesolutionmaybenecessary.  4.6 ` Theextentofinterferencesthatmaybeencounteredusingionchromatographic T  techniqueshasnotbeenfullyassessed.AlthoughtheICconditionsdescribedallowforaresolutionofthehydrogencyanidefromsulfide,othermatrixcomponentsmayinterfere.SincetheICprovidesgoodseparationcapabilityandtheelectrolyticdetectionsystemcanbemadeselectiveforcyanideion,thetwoworkingtogethershouldofferverygoodresolution.Incasesofextremeinterference,adifferentanalyticalfinishcanbesubstituted.  4.7 ` Anygaseousmaterialwhichcanpassthroughthefilterandformcyanideionin D  thecollectionmediumwillcauseapositivebiasinthismethod.Fortunately,onlycyanogenisknowntodoso.Furtherinvestigationoftheexistenceofothercompoundswiththeabilitytointerfereinthismannerwouldbeworthwhile.    ffd- &  5.0  Safety.  B ff  5.1 ` 'B2Thetoxicityorcarcinogenicityofeachreagentusedinthismethodhasnotbeen r preciselydefined.However,eachchemicalcompoundshouldbetreatedasapotentialhealthhazard.Fromthisviewpoint,exposuretothesechemicalsmustbereducedtothelowestpossiblelevelbywhatevermeansareavailable.Fieldsamplecollectionandrecoveryshouldbeconductedusingapprovedpersonalsafetyapparatusaswellasanexhausthoodforcollectionofhazardousfumes.ThelaboratoryisresponsibleformaintainingacurrentawarenessfileofOccupationalSafety&HealthAdministration(OSHA)regulationsregardingthesafehandlingofthechemicalsspecifiedinthismethod.Areferencefileofmaterialsafetydatasheets(MSDSs)shouldalsobemadeavailabletoallpersonnelinvolvedinthechemicalanalysis.Additionalreferencestolaboratorysafetyareavailable.ff)3ff  5.2 ` Hydrogencyanidesmellslikealmonds.Itisflammableintherangeof5.640%in %  air.Itisextremelytoxicwheninhaled. &  6.0  EquipmentAndSupplies.  'v!#   6.1  ` Thefollowingitemsarerequiredforsamplecollection. ''7Aschematicdiagramof )N#% thesamplingtrainusedinthismethodisshowninFigureXHCN1.ThissamplingtrainconfigurationisadaptedfromtheEPAMethod5procedures.Themajorityoftherequired +*%' equipmentisidenticaltothatusedintheEPAMethod5train,withtheonlychangebeingtheuseofcausticsolutionintheimpingers. Whensamplingsourcescontainingsulfides,usethe P samplingtrainshowninFigureXHCN2toeliminateanysulfideinterferencewiththeanalysisandwiththestabilityofcyanideinsolution.ThistrainusesaninitialimpingercontainingleadacetatetoprecipitatesulfideasleadsulfideandpreventanysulfidefrombeingcollectedwiththecyanideintheNaOHsolution.XuXXX%  ConstructiondetailsforthebasictraincomponentsaregiveninAPTD-0581(Reference   3).Commercialmodelsofthisequipmentarealsoavailable.ThefollowingsubsectionslistchangestoAPTD-0581andidentifyallowabletrainconfigurationmodifications. Basic  h operatingandmaintenanceproceduresforthesamplingtrainaredescribedinAPTD-0576(Reference4).Correctusageisimportantinobtainingvalidresults.AllusersofthismethodologyshouldthereforerefertoAPTD-0576andadopttheoperatingandmaintenanceproceduresoutlinedthereinunlessotherwisespecified.Thesamplingtrainconsistsofthecomponentsdetailedbelow.-,XXhX,XX-#X%XXXu;#XuXXX%  6.1.1  ` ProbeNozzle.Quartzorborosilicateglasswithsharp,leadingedge,tapered30$ l  angle.Thetapershallbeontheoutsidetopreserveaconstantinternaldiameter.Thenozzleshallbebuttonhookorelbowdesign.Arangeofnozzlesizessuitableforisokineticsamplingshouldbeavailableinincrementsof0.16cm(1/16in.),e.g.,0.32-1.27cm(1/8-1/2in.),orlargerifhighervolumesamplingtrainsareused.&  ԀEachnozzleshallbecalibratedaccordingtotheproceduresoutlinedinSection110.1.',@  6.1.2  ` Probeliner.Borosilicateorquartz-glasstubingwithaheatingsystemcapableof   maintainingaprobegastemperatureof12014$C(24825$F)attheexitendduring  sampling.Becausetheactualtemperatureattheoutletoftheprobeisnotusuallymonitoredduringsampling,probesconstructedaccordingtoAPTD-0581andutilizingthecalibrationcurvesofAPTD-0576(orcalibratedaccordingtotheprocedureoutlinedinAPTD-0576)areconsideredacceptable.Eitherborosilicateorquartzglassprobelinersmaybeusedforstacktemperaturesuptoabout480$C(900$F).Quartzglasslinersshallbeusedfortemperatures H between480and900$C(900and1650$F).Thesofteningtemperatureforborosilicateis820 8 $C(1508$F),andforquartzglass1500$C(2732$F).Water-coolingofthestainlesssteel  ( sheathwillbenecessaryattemperaturesapproachingandexceeding500$C. |! #X%XXXu>#   6.1.3  ` HeatedFilter.Aglassorquartzfilter,similartothatusedwithMethod5,isused l" tocollectparticulatematerialforsubsequentextractionandanalysis.ThefilterissupportedbyaTeflonfiltersupportwhichishousedinanall-glassfilterholder.Thefilterismaintainedat12014$C(24825$F)duringsampling. 4%! XuXXX%  6.1.4  ` Pitottube.TypeS,asdescribedinSection2.1ofpromulgatedMethod2(Section  &" 6.1ofReformattedDraftMethod2),orotherappropriatedevices(seeVollaro,1976inSection17.0,Reference5).ThePitottubeshallbeattachedtotheprobetoallowconstantmonitoringofthestackgasvelocity.Theimpact(high-pressure)openingplaneofthePitottubeshallbeevenwithorabovethenozzleentryplane(seeMethod2,Figure62b)duringsampling.TheTypeSPitottubeassemblyshallhaveaknowncoefficient,determinedasoutlinedinSection4.0ofpromulgatedEPAMethod2(Section10.0ofReformattedDraftMethod2).#X%XXXuSG#XuXXX% +\%(   6.1.5  ` DifferentialPressureGauge.Twoinclinedmanometersorequivalentdeviceas d describedinSection2.2ofpromulgatedMethod2(Section10.0ofReformattedDraftMethod2).Onemanometershallbeusedforvelocity-headreadings(P)andtheotherfororifice D differentialpressure(H)readings. 4  #X%XXXuCJ#   6.1.6 ` TemperatureSensor.Atemperaturesensorcapableofmeasuringtemperatureto $  within3$C(5.4$F)shallbeinstalledsothatthetemperatureattheimpingeroutletcanbe   regulatedandmonitoredduringsampling.  6.1.7 ` ImpingerTrain.Thesamplingtrainrequiresaminimumoffour500-mL   impingers,connectedinseriesimmediatelyfollowingtheheatedfilter(asshowninFiguresXHCN1andXHCN2),withgroundglass(orequivalent)vacuum-tightfittings.9,XXX,XXhX9   6.1.7.1 ` NaOHTrainConfiguration.Thefirstandsecondimpingersshallbeofthe P  GreenburgSmithdesignwiththestandardtip.TheremainingtwoimpingersshallbeofthemodifiedGreenburgSmithdesign,modifiedbyreplacingthetipwitha1.3cm(in.)insidediameterglasstubeextendingto1.3cm(in.)fromthebottomoftheoutercylinder.Fillthefirstandsecondimpingerswith100mLof0.1NNaOHperimpinger.Leavethethirdimpingeremptyandfillthefourthimpingerwithaknownmass(2/3full)ofdesiccant.   6.1.7.2 ` LeadAcetate/NaOHTrainConfiguration.Thefirst,third,andfourthimpingers @ shallbeoftheGreenburgSmithdesignwiththestandardtip.TheremainingtwoimpingersshallbeofthemodifiedGreenburgSmithdesign,modifiedbyreplacingthetipwitha1.3cm(in.)insidediameterglasstubeextendingto1.3cm(in.)fromthebottomoftheoutercylinder.Fillthefirstimpingerwith10%byweightacidifiedleadacetatesolution.LeavethesecondimpingeremptytopreventcarryoveroftheleadacetatesolutionintotheNaOHsolution.Fillthethirdandfourthimpingerswith100mLof0.1NNaOHperimpinger.Fillthefifthimpinger(2/3full)withaknownmassofdesiccant.?X XXX%Ԁ#X%X X?XS#AlthoughthePbacetate/NaOHsamplingtrainperformedwellinthe T laboratory,withnosignofexcessivepressuredropacrossthesystem,experiencedsamplershaveexpressedconcernthatthepresenceofthreeGSimpingerswithtipsmightleadtoproblemsinfieldsituations.Ifparticulatecollectiononthefilterbecomesheavy,thecombinedpressuredropacrossthetrainmightbecomeunacceptable.Ifthatsituationoccurs,atubewithamoreopentipshouldbesubstitutedforthestandardGStubeinthesecondNaOHimpinger(the4thimpingeroverall).Sinceitisdesirabletokeepthebubblesizeassmallaspossibleinordertomaximizegasliquidcontact,atubewithataperedtip(maybe"opening)wouldbepreferabletotheusual"modifiedGStip.  6.1.8 ` MeteringSystem.Thenecessarycomponentsofthemeteringsystemarea $  vacuumgauge,leakfreepump,temperaturesensorscapableofmeasuringtemperaturewithin3 $! $C(5.4$F),drygasmetercapableofmeasuringvolumetowithin1%,andrelatedequipmentas %~" showninFigureXHCN1.Ataminimum,thepumpshouldbecapableof4cubicfeetperminute(cfm)freeflow,andthedrygasmetershouldhaveavolumemeasuringcapacityof0999.9cubicfeetwitharesolutionof0.005cubicfeet.Othermeteringsystemscapableofmaintainingsamplerateswithin10%ofisokineticvariationandofdeterminingsamplevolumestowithin2%oftheactualvaluemaybeused.Themeteringsystemmustbeusedinconjunctionwithapitottubetoenablechecksofisokineticsamplingrates.Samplingtrainsusingmetering j+%( systemsdesignedforflowrateshigherthanthosedescribedinAPTD-0581andAPTD-0576maybeused,providedthatthespecificationsofthismethodaremet.  6.1.9 ` Barometer.Mercury,aneroid,orotherbarometercapableofmeasuring < atmosphericpressuretowithin2.5mmHg(0.1in.Hg).ThebarometricpressurereadingmaybeobtainedfromanearbyNationalWeatherServiceStation.Inthiscase,requestthestationvalue(whichistheabsolutebarometricpressure)andadjustthevalueforelevationdifferencesbetweentheweatherstationandsamplingpointatarateofminus2.5mm(0.1in.)Hgper30meters(100ft.)elevationincreaseorplus2.5mm(0.1in.)Hgper30meters(100ft.)elevationdecrease.  6.1.10 ` GasDensityDeterminationEquipment.Temperaturesensorandpressuregauge  d (asdescribedinSections2.3and2.4ofPromulgatedMethod2aswellasSections6.3and6.4ofReformattedMethod2),andgasanalyzer,ifnecessary,asdescribedinMethod3.Thetemperaturesensorshall,preferably,bepermanentlyattachedtothepitottubeorsamplingprobeinafixedconfigurationsothatthetipofthesensorextendsin.beyondtheleadingedgeoftheprobesheathanddoesnottouchanymetal.Alternatively,thesensormaybeattachedjustpriortouseinthefield.Note,however,thatifthetemperaturesensorisattachedinthefield,thesensormustbeplacedinaninterferencefreearrangementwithrespecttotheTypeSpitottubeopenings(seePromulgatedMethod2,Figure27,aswellasReformattedMethod2,Figure24).Asasecondalternative,ifadifferenceofnomorethan1%intheaveragevelocitymeasurementsistobeintroduced,thetemperaturesensorneednotbeattachedtotheprobeorpitottube(subjecttotheapprovaloftheAdministrator).  6.1.11  ` Calibration/FieldPreparationRecord.Apermanentlyboundlaboratorynotebook, x inwhichduplicatecopiesofdatamaybemadeastheyarebeingrecorded,isrequiredfordocumentingandrecordingcalibrationsandpreparationprocedures(i.e.,silicageltareweights,qualityassurance/qualitycontrolcheckresults,drygasmeterreadings,andthermocouplecalibrations,etc.).Theduplicatecopiesshouldbedetachableandshouldbestoredseparatelyinthetestprogramarchives.  6.1.12 ` VitonAOring. h    6.1.13 ` HeatResistantTape. X    6.1.14 ` TeflonTape. H      6.2 ` SampleRecovery.Thefollowingitemsarerequiredforsamplerecovery. 8!   6.2.1 ` ProbeLinerandProbeNozzleBrushes.Teflonbristlebrusheswithstainlesssteel (" wireorTeflonhandlesarerequired.Theprobebrushshallhaveextensionsconstructedofstainlesssteel,Teflon,orinertmaterialatleastaslongastheprobe.Thebrushesmustbeproperlysizedandshapedtobrushouttheprobelinerandtheprobenozzle.  6.2.2 ` WashBottles.Teflonorglasswashbottlesarerecommended;polyethylenewash %x" bottlesshouldnotbeusedforacetonebecauseorganiccontaminantsmaybeextractedbyexposuretoacetone.  6.2.3  ` SampleStorageContainers.Alkaliresistantpolyethylene(notforacetone) (@"% bottles,500mLor1000mL.ScrewcaplinersshallbeeitherTeflonorconstructedtobeleak-freeandresistanttochemicalattackbycausticsolution.Narrow-mouthbottleshavebeenfoundtoexhibitlesstendencytowardleakage.Foldthefilterintoquartersbeforetransferringit l+%( tothebottle.  6.2.4 ` GraduatedCylinderand/orBalance.Tomeasureimpingercontentstothenearest P 1mLor1g,graduatedcylindersshallhavesubdivisionsnot>2mL.Laboratorybalancescapableofweighingto0.5gorbetterarerequired.XuXXX%  6.2.5  ` PlasticStorageContainers.Screw-cappolypropyleneorpolyethylenecontainers   tostoresilicagel.#X%XXXuJk#   6.2.6  ` GlassFunnelandRubberPoliceman.Toaidinthetransferofmaterialintoand   outofcontainersinthefield.  6.2.7 ` Coolers.Tostoreandshipsamplecontainers.  p    6.3 ` ReagentPreparationApparatus. `    6.3.1 ` Bottles/Caps.Highdensitypolyethylene1or4LbottleswithTeflonlinedcaps P  arerequiredforstoring0.1NNaOHsolutionandleadacetatesolution.  6.3.2 ` LargeGlassContainer.Atleastonelargeglasscontainer(8to16L)isrequired ,  forpreparingtheaqueous0.1NNaOHsolutionandtheleadacetatesolution.  6.3.3 ` StirPlate/LargeStirBars/StirBarRetriever.Amagneticstirplateandlargestir l  bararerequiredtomixtheaqueous0.1NNaOHsolutionandtheleadacetatesolution.AstirbarretrieverisneededforremovingthestirbarfromtheNaOHsolutioncontainer.  6.3.4 ` Beakers.Beakers(150mL,250mL,and400mL)areusefulfor 4 holding/measuringliquidswhenpreparingtheaqueous0.1NNaOHandtheleadacetatesolutionsandforweighingNaOHpelletsandleadacetate.  6.3.5 ` Funnels.Atleastonelargefunnelisneededforpouringtheaqueous0.1NNaOH  andtheleadacetatesolutionsintobottles.  6.3.6 ` GraduatedCylinders.Atleastonelargegraduatedcylinder(1to2L)isrequired t formeasuringwaterwhenpreparingtheNaOHandleadacetatesolutions.  6.3.7 ` TopLoadingBalance.Atoploadingbalancereadabletothenearest0.1gis P neededforweighingtheNaOHpelletsusedtopreparetheaqueous0.1NNaOHsolutionandtheleadacetateusedtopreparethe10%leadacetatesolution.  6.3.8 ` Spatulas.SpatulasareneededforhandlingNaOHpelletswhenpreparingthe | aqueousNaOHsolutionandtheleadacetatewhenpreparingthe10%leadacetatesolution.   6.4 ` Analysis X!   6.4.1 ` Vials.10and25mL,glasswithTeflon-linedscrewcapsorcrimptops. H"   6.4.2 ` AnalyticalBalance.Capableofaccuratelyweighingtothenearest0.1mg. 8#   6.4.3 ` VolumetricFlasks. ($    6.4.4 ` IonChromatograph(Modular). %!   6.4.4.1 ` Pumpingsystem.Isocraticwithconstantflowcontrolcapableof1.0mL/min. &"   6.4.4.2 ` HighPressureInjectionValvewith50Lloop. & #   6.4.4.3 ` Column.250_mm_Ԁx4_mm_ԀID,IonPacAS7A(orequivalent)withanAG7A(or '!$ equivalent)guardcolumn.  6.4.4.4 ` ElectrochemicalDetectorwithSilverWorkingElectrodeandSilver/Silver )`#& ChlorideReferenceElectrode. +<%(   6.4.4.5 ` StripChartRecorderCompatibleWithDetector.Useofadataacquisitionsystem d formeasuringpeakareasandretentiontimesisrecommended.%  &  7.0  ReagentsAndStandards.  ,    7.1 ` ', )zReagentgradechemicalsshallbeusedinalltests.Unlessotherwiseindicated,all   reagentsshallconformtothespecificationsoftheCommitteeonAnalyticalReagentsoftheAmericanChemicalSociety,wheresuchspecificationsareavailable.Othergradesmaybeused,providedthatthereagentisofsufficientlyhighpuritytousewithoutjeopardizingaccuracy.  7.2 ` Water.Allreferencestowaterinthismethodrefertodeionized,distilledwater T  thatconformstoAmericanSocietyofTestingandMaterials(ASTM)SpecificationD119391,Type3(Reference6).Ifhighconcentrationsoforganicmatterarenotexpectedtobepresent,theanalystmayomitthepotassiumpermanganatetestforoxidizableorganicmatter.  7.2.1  ` Alllaboratoryglasswaremustbewashedwithlaboratorydetergentandrinsed l  withwaterandacetonebeforeuse.  7.2.2  ` PreparationofAqueous0.1NNaOHReagent:EachbatchofNaOHreagent H  shouldbepreparedaccordingtotheproceduredescribedbelow.?,XX h*X,XXX?  NOTE: NaOHpelletsorsolutionshouldbehandledwithplasticglovesatalltimeswith $ promptandextensiveuseofrunningwaterincaseofskinexposure.?,XXX,XX h*X?  7.2.2.1  ` Placean8L(orotherappropriatelysized)containerunderafumehoodona  magneticstirrer.Addalargestirbarandfillthecontainerhalffullwithwater.Startthestirringbarandadjustittostirasfastaspossible.WeightheNaOHpelletsonaoneplacebalance(32g/8L)andaddtothestirringwater.Fumesmaybegeneratedandthewatermaybecomewarm.Fillthe8Lcontainertothe8Lmarkwithwaterandstiruntildissolved.  7.2.2.2  ` Transferthe0.1NNaOHreagentsolutionintoahighdensitypolyethylenebottle. < Labelthebottlewiththereagentidentificationandconcentration,thedateprepared,andwhopreparedit.  7.2.3  ` Preparationof10%LeadAcetateSolution:Eachbatchofleadacetatereagent h shouldbepreparedaccordingtotheproceduredescribedbelow.  7.2.3.1 ` Placean8L(orotherappropriatelysized)containerunderafumehoodona D! magneticstirrer.Addalargestirbarandfillthecontainerhalffullwithwater.Startthestirringbarandadjustittostirasfastaspossible.Weighthelead(II)acetatetrihydrateonaoneplacebalance(933g/8L)andaddtothestirringwater.AdjustthepHtolessthan4.5byaddingglacialaceticacid.Fillthe8Lcontainertothe8Lmarkwithdeionized,distilledwaterandstiruntilwellmixed.CheckthepH.Ifgreaterthan4.5,addadditionalglacialaceticacidtoadjustthepHbelow4.5.  7.2.3.2  ` Transfertheleadacetatesolutionintoahighdensitypolyethylenebottle. 'X!$   7.2.4  ` ShipmenttotheField:Tightlycapthebottlescontaining0.1NNaOHreagentand (H"% leadacetatereagentusingTeflonlinedcaps.SealthebottleswithTeflontape.Ifnumerousbottlesareshipped,cushionthebottlestoensurethatbreakagedoesnotoccur. IftheNaOH *$$' reagentandtheleadacetatereagenthavepassedtheQualityControlcriteriainSection9.2.5,the t+%( reagentsmaybepackagedtomeetnecessaryshippingrequirementsandsenttothesamplingarea.IftheQualityControlcriteriaarenotmet,thereagentsolutionsmustbereprepared.  7.3 ` FieldSpikeStandardPreparation.Toprepareacyanidefieldspikingstandardat < 4.0mg/mL,weigh500mgofpotassiumcyanideina50mLvolumetricflask.Filltheflaskhalffullwith0.1NNaOHandshakevigorously.Afterallofthepotassiumcyanidedissolves,diluteto50mLwith0.1NNaOH.  7.4 ` AscorbicAcid.AscorbicAcidmayberequiredtoremoveoxidizingagentsduring   samplerecovery.  7.5 ` SodiumHydroxide. NaOHpelletsarerequiredforpreparationoftheimpinger  h reagentsolution,themobilephasebuffer,andthe10NNaOHusedtoadjustthepHofrecoveredsamples.  7.6 ` AlizarinYellowRIndicatorSolution.Dissolve0.10gofAlizarinYellowRin 0  100mLofdeionized,distilledwater.Agitateonastirplatefor30minutestocompletelydissolvetheAlizarinYellowR.  7.7 ` Acetone.HPLCgradeorequivalentisrequiredforrinsingglassware. \    7.8 ` SodiumAcetateandEthyleneDiamine.RerequiredfortheMobilePhaseBuffer. L    7.9 ` PotassiumCyanide.Requiredforpreparationofanalyticalstandards. <   7.10 ` SodiumAcetateBufferSolution.Neededformobilephase.Preparethesodium , acetatebuffersolutioneachdaybydissolving4gofNaOHand41gofsodiumacetateinwater.Add5mLofethylenediamineanddiluteto1Lwithwater.  7.11 ` PreparationofStandardsforChromatographicAnalyses.    7.11.1 ` StockStandards.Preparepotassiumcyanidestockstandardsatconcentrationsof  100ng/%Lbyweighing25mg(0.01mg)ofpotassiumcyanideinto100-mLvolumetricflasks, p dissolvingthecrystalsin0.1NNaOH,anddilutingtothelinewith0.1NNaOH.Transferthestocksolutionstobottleswithapolyfluoroethylenelinedscrewcapsandstoreat4$C(39$F). H   7.11.2 ` CalibrationStandards.Preparecalibrationstandardsbydiluting100,500,1,000, 4 1,500,and2,000%Lofoneofthepotassiumcyanidestocksolutionsto100mLwith0.1NNaOH $ toprovideastandardcurvewithCNcalibrationpointsat0.1,0.5,1.0,1.5,and2.0ng/%Lof t 0.1NNaOH.  7.11.3 ` CheckStandard.Prepareacheckstandard,usingpotassiumcyanidefroma L! secondvendor,ataconcentrationof1.0ng/%LofCNbytaking1000%Lofa100ng/%L <" potassiumcyanidestockstandardanddilutingto100mLwith0.1NNaOH.Usethecheckstandardtochecktheinstrumentresponseandthecalibrationaccuracy. Replacestandard $  solutionsaftersixmonths,orsooner,ifcomparisonwithcheckstandardsindicatesaproblem. XuXXX%  7.12  ` CrushedIce.Quantitiesrangingfrom10-50poundsmaybenecessaryduringa %" samplingrun,dependinguponthetemperatureofambientairandthemoisturecontentofthegasstream.Althoughnormalambienttemperatureswillnotharmthesamples,theymayneedtobepackedinicetoavoidexcessiveheatduringshippinginhotweather;sufficienticeforthispurposemustbeallowed.  7.13  ` StopcockGrease.Theuseofsiliconegreaseisnotpermitted.Siliconegrease *8$' usageisnotnecessaryifscrew-onconnectors,Teflonsleevesorground-glassjointsareused. +(%(   7.14  ` SilicaGel.Indicatingtype,616mesh.Ifpreviouslyused,dryat180$C d (350$F)for2hoursbeforeusing.Newsilicagelmaybeusedasreceived.Alternatively,other T typesofdesiccants(equivalenttosilicagelorbetter)maybeused,subjecttotheapprovaloftheAdministrator.  7.15  ` _Impinger_ԀSolutions.Theimpingersolutionscanbepreparedinthelaboratoryor $  inthefield.Placelabelsonthecontainersspecifyingthereagentidentificationandconcentration,thedateprepared,andwhopreparedit.  7.15#X%XXXuG#XuXXX%.1 ` The0.1NNaOH#X%XXXu#XuXXX%Ԁsolution#X%XXXuQ#XuXXX%isprepared(Section87.2.2)bydissolving4gramsof   sodiumhydroxideindeionized,distilledwateranddilutingto1literwithwater.Thissolutionshouldbestoredinhighdensitypolyethylenecontainersandusedwithintendaysofpreparation.Alternatively,commercially-preparedNaOHsolutionmaybeused.#X%XXXu#XuXXX%  7.1{5{#X%XXXuC#XuXXX%.2 ` The10%byweightacidifiedleadacetatesolution#X%XXXu#XuXXX%isprepared(Section7.2.3)by P  dissolving117gramsoflead(II)acetatetrihydrateinwater,dilutingto1literwithwater(10%leadacetate),andacidifyingthesolutiontoapHof4.5orbelowwithglacialaceticacid.Thissolutionshouldbestoredinhighdensitypolyethylenecontainersandusedwithintendaysofpreparation.#X%XXXu'#   &  8.0  SampleCollection,Preservation,StorageAndTransport.  P   8.1 ` 'PݠBecauseofthecomplexityofthismethod,fieldpersonnelshouldbetrainedinand ( experiencedwiththetestproceduresinordertoobtainreliableresults.&    8.2 ` LaboratoryPreparation.    8.2.1 ` '3Allthecomponentsmustbemaintainedandcalibratedaccordingtotheprocedure  describedinAPTD0576(Reference4),unlessotherwisespecified.  8.2.2 ` Weighseveral200to300gportionsofsilicageltothenearest0.5gandplacethe l silicagelinairtightcontainers.Recordoneachcontainerthetotalweightofthesilicagelpluscontainers.Asanalternativetopreweighingthesilicagel,thesilicagelmaybeweigheddirectlyintheimpingerorsamplingholderjustpriortoassemblyofthesamplingtrain.&    8.3 ` PreliminaryFieldDeterminations.     8.3.1 ` ' Selectthesamplingsiteandtheminimumnumberofsamplingpointsaccordingto t! Method1orotherrelevantcriteria.Determinethestackpressure,temperature,andrangeofvelocityheadsusingMethod2(Reference1).CheckthePitotlinesforleaksaccordingtoPromulgatedMethod2,Section3.1(ReformattedMethod2,Section8.1).DeterminethestackgasmoisturecontentusingApproximationMethod4oritsalternativestoestablishestimatesofisokineticsamplingratesettings.Determinethestackgasdrymolecularweight,asdescribedinPromulgatedMethod2,Section3.6(ReformattedMethod2,Section8.6).IfintegratedMethod3samplingisusedformolecularweightdetermination,theintegratedbagsampleshallbetakensimultaneouslywith,andforthesametotallengthoftimeas,thesamplerun.  8.3.2 ` Selectanozzlesizebasedontherangeofvelocityheadssothatitisnotnecessary )`#& tochangethenozzlesizeinordertomaintainisokineticsamplingrates.Duringthesamplingrun,donotchangethenozzle.Ensurethattheproperdifferentialpressuregaugeischosenfor +<%( therangeofvelocityheadsencountered(seeSection2.2ofPromulgatedMethod2,aswellasSection8.2ofReformattedMethod2).  8.3.3 ` Selectasuitableprobelinerandprobelengthsothatalltraversepointscanbe < sampled.Forlargestacks,toreducethelengthoftheprobe,considersamplingfromoppositesidesofthestack.  8.3.4 ` Atypicalsamplevolumetobecollectedis1drystandardcubicmeter(dscm)   (35.31drystandardcubicfeet[dscf]).Thesamplevolumecanbeadjustedasnecessitatedbyanalyticaldetectionlimitconstraintsand/orestimatedstackconcentrations.Amaximumlimitshouldbedeterminedtoavoidexceedingthecapacityofthereagent.Aminimumsamplevolumeshouldalsobedeterminedthatwillprovidesufficientcollectionoftheanalytesothattheinstackdetectionlimitisconsistentwiththedataqualityobjectivefortheproject.  8.3.5 ` Determinethetotallengthofsamplingtimeneededtoobtaintheidentified ,  minimumvolumebycomparingtheanticipatedaveragesamplingratewiththevolumerequirement.AllocatethesametimetoalltraversepointsdefinedbyMethod1(Reference1).Toavoidtimekeepingerrors,thelengthoftimesampledateachtraversepointshouldbeanintegerplusonehalfminute.  8.3.6 ` Insomecircumstances(e.g.,batchcycles)itmaybenecessarytosamplefor 0 shortertimesatthetraversepointsandtoobtainsmallergasvolumesamples.Inthesecases,carefuldocumentationmustbemaintainedinordertoallowaccurateconcentrationcalculation.&    8.4 ` PreparationofCollectionTrain.    8.4.1 ` 'Duringpreparationandassemblyofthesamplingtrain,keepallopeningswhere  contaminationcanoccurcoveredwithTeflonfilmoraluminumfoiluntiljustpriortoassemblyoruntilsamplingisabouttobegin.  8.4.2 ` ThissectiondescribesthebasicNaOHtrainconfigurationwhichmaybemodified L asoutlinedtoreducepotentialinterferences.  8.4.2.1 ` ForthebasicNaOHtrainconfiguration,place100mLof0.1NNaOHabsorbing ( solutionineachofthefirsttwoimpingers.Add10dropsofAlizarinYellowindicatorsolutiontoeachimpinger(ifnotusingapHprobeorpHpapertomonitorimpingerpH).Thethirdimpingershallremainempty.Thefourthimpingershallhave200to300gofpreweighedsilicagel.Becarefultoensurethatthesilicagelisnotentrainedandcarriedoutfromtheimpingerduringsampling.Placethesilicagelcontainerinacleanplaceforlateruseinthesamplerecovery.Alternatively,theweightofthesilicagelplusimpingermaybedeterminedtothenearest0.5gandrecorded.Formoisturedetermination,weighalloftheimpingersafterfillingthemwithreagent.  8.4.2.2 ` Whenhighconcentrationsofacidicgasesareexpectedtobepresentinthesource, %x" modifythebasicNaOHtrainconfigurationbyoneormoreofthefollowingprocedures:1)increasethevolumeof0.1NNaOHabsorbingsolutionineachofthefirsttwoimpingersto200mL;2)addoneormoreadditionalimpingerscontainingNaOHsolutiontothetrain;3)increasetheconcentrationoftheNaOHsolutionintheimpingersto0.2N,0.5N,1Nor2N;or4)usetheleadacetate/NaOHtrainconfiguration. h+%(   8.4.2.3 ` Fortheleadacetate/NaOHtrainconfiguration,place100mLof10%acidified d leadacetatesolutioninthefirstimpinger.Leavethesecondimpingerempty.Fillthethirdandfourthimpingerswith100mLof0.1NNaOHabsorbingsolution.Add10dropsofAlizarinYellowindicatorsolutiontoeachimpinger(ifnotusingapHprobeorpHpapertomonitorimpingerpH).Place200to300gofpreweighedsilicagelinthefifthimpinger.  8.4.3 ` Whenglassprobelinersareused,installtheselectednozzleusingaViton-AO   ringwhenstacktemperaturesare<260$C(500$F)andawovenglass-fibergasketwhen   temperaturesarehigher.SeeAPTD0576(Reference4)fordetails.Otherconnectingsystemsusingeither316stainlesssteelorTeflonferrulesmaybeused.Marktheprobewithheatresistanttapeorbysomeothermethodtodenotetheproperdistanceintothestackorductforeachtraversesamplingpoint.  8.4.4 ` AssemblethetrainasshowninFigureXHCN1.Duringassembly,donotuseany ,  siliconegreaseontheground-glassjointsoftheimpingers.UseTeflontapeorTeflon Orings,ifrequired.Checkalltemperaturesensorsatambienttemperatures.  8.4.5 ` Placecrushedicearoundtheimpingers. X    8.4.6 ` Switchonandsettheprobeandfilterheatingsystemsatthedesiredtemperature. H  Allowtimeforthetemperaturetostabilizefor30min.&    8.5 0 ` Leak-CheckProcedures.$` (#` (#   8.5.1 ` '$4PretestLeakcheck.    8.5.1.1  ` Apretestleakcheckofthesamplingsystemisnotrequiredbutishighly  recommended.Apretestleakcheckofthepitotlinesisalsonotrequiredbutishighlyrecommended(seeMethod2).  8.5.1.2 ` Afterthesamplingtrainhasbeenassembled,switchonandsettheprobeheating h systemtothedesiredoperatingtemperature.Allowtimeforthetemperaturetostabilize.IfaViton-AO-ringorotherleak-freeconnectionisusedinassemblingtheprobenozzletotheprobeliner,leak-checkthetrainatthesamplingsitebypluggingthenozzleandpullinga381-mmHg(15-in.Hg)vacuum.Leakageratesinexcessof4%oftheaveragesamplingrateor>0.00057m3/min(0.020cfm),whicheverisless,areunacceptable. l   NOTE: Alowervacuummaybeused,providedthatitisnotexceededduringthetest. X    8.5.1.3 ` Thefollowingleakcheckinstructionsforthesamplingtraindescribedin H! APTD-0581andAPTD-0576(References3and4)maybehelpful.Startthepumpwiththefine-adjustvalvefullyopenandcoarse-adjustvalvecompletelyclosed.Partiallyopenthecoarse-adjustvalveandslowlyclosethefine-adjustvalveuntilthedesiredvacuumisreached.Donotreversedirectionofthefineadjustvalve,asliquidwillbackupintothetrain.Ifthe $! desiredvacuumisexceeded,eitherperformtheleakcheckatthishighervacuumorendtheleakcheck,asshownbelow,andstartover.  8.5.1.4 ` Whentheleakcheckiscompleted,firstslowlyremovetheplugfromtheinletto '\!$ theprobe.Whenthevacuumdropsto127mm(5in.Hg)orless,immediatelyclosethecoarse-adjustvalve.Switchoffthepumpingsystemandreopenthefine-adjustvalve.Donotreopenthefine-adjustvalveuntilthecoarse-adjustvalvehasbeenclosedtopreventtheliquidintheimpingersfrombeingforcedbackwardinthesamplinglineandsilicagelfrombeing t+%( entrainedbackwardintothethirdimpinger.&  0  8.5.2 ` LeakChecksDuringtheSamplingRun.P(#(#   8.5.2.1 ` 'PIf,duringthesamplingrun,acomponentchangebecomesnecessary,aleak-check @ shallbeconductedimmediatelyaftertheinterruptionofsamplingandbeforethechangeismade.TheleakcheckshallbeperformedaccordingtotheproceduredescribedinSection98.5.1,exceptthatitshallbeperformedatavacuumgreaterthanorequaltothemaximumvaluerecordeduptothatpointinthetest.Iftheleakagerateisfoundtobenogreaterthan0.00057m3/min   (0.020cfm)or4%oftheaveragesamplingrate(whicheverisless),theresultsareacceptableandnocorrectionwillneedtobeappliedtothetotalvolumeofdrygasmetered.Ifahigherleakagerateisobtained,thetestermustvoidthesamplingrun.   NOTE: Anycorrectionofthesamplevolumebycalculationreducestheintegrityofthe @  pollutantconcentrationdatageneratedandmustbeavoided.  8.5.2.2 ` Immediatelyafteracomponentchangeandbeforesamplingisreinitiated,aleak   checksimilartoapretestleakcheckshouldalsobeconducted.&    8.5.3 ` PostTestLeakCheck. \    8.5.3.1 ` '\Aleakcheckofthesamplingtrainismandatoryattheconclusionofeach L  samplingrun.Theleakcheckshallbeperformedinaccordancewiththesameproceduresasthepretestleakcheck,exceptthattheposttestleakcheckshallbeconductedatavacuumgreaterthanorequaltothemaximumvaluereachedduringthesamplingrun.Iftheleakagerateisfoundtobenogreaterthan0.00057m3/min(0.020cfm)or4%oftheaveragesamplingrate(whichever  isless),theresultsareacceptable.If,however,ahigherleakagerateisobtained,thetestershallrecordtheleakagerate,correctthesamplevolume(asshowninSection_12.__3.0_Ԁofthismethod)andclearlymarkthedataobtainedofquestionablereliability,orvoidthesamplingrun. &    8.6 ` SamplingTrainOperation. L   8.6.1 ` ' Duringthesamplingrun,maintainanisokineticsamplingratetowithin10%of < trueisokinetic,below28L/min(1.0cfm).Maintainaprobetemperatureof120$C14$C , (248$F25$F). |    8.6.2  ` Foreachrun,recordthedataonadatasheetsuchastheoneshowninFigure h XHCN3.Besuretorecordtheinitialdrygasmeterreading.Recordthedry-gasmeterreadingsatthebeginningandendofeachsamplingtimeincrement,whenchangesinflowratesaremade,beforeandaftereachleakcheck,andwhensamplingishalted.TakeotherreadingsindicatedbyFigureXHCN3atleastonceateachsamplingpointduringeachtimeincrementandadditionalreadingswhensignificantadjustments(20%variationinvelocityheadreadings)necessitateadditionaladjustmentsinflowrate.Levelandzerothemanometer.Becausethemanometerlevelandzeromaydriftduetovibrationsandtemperaturechanges,makeperiodicchecksduringthetraverse.Also,recordtheresultsofanypHchecksthatweremadeandthetimethattheyweremade.  8.6.3 ` Cleanthestackaccessportspriortothetestruntoeliminatethechanceof (@"% collectingdepositedmaterial.Tobeginsampling,verifythattheprobeheatingsystemsareatthespecifiedtemperature,removethenozzlecap,andverifythatthePitottubeandprobeareproperlypositioned.Positionthenozzleatthefirsttraversepointwiththetippointingdirectly l+%( intothegasstream.Immediatelystartthepumpandadjusttheflowtoisokineticconditions.Nomographs,whichaidintherapidadjustmentoftheisokineticsamplingratewithoutexcessivecomputations,areavailable.ThesenomographsaredesignedforusewiththeTypeSPitottubewithacoefficientof0.840.02andthestackgasequivalentdensity(drymolecularweight)isequalto294.APTD0576(Reference4)detailstheprocedureforusingthenomographs.IfthestackgasmolecularweightandthePitottubecoefficientareoutsidetheaboveranges,donotusethenomographsunlessappropriatesteps(Reference7)aretakentocompensateforthedeviations.  8.6.4  ` Whenthestackisundersignificantnegativepressure,takecaretoclosethe  ` coarseadjustvalvebeforeinsertingtheprobeintothestackinordertopreventtheimpingersolutionsfrombackingupintotheprobe.Ifnecessary,thepumpmaybeswitchedonwiththecoarse-adjustvalveclosed.  8.6.5  ` Whentheprobeisinposition,blockofftheopeningsaroundtheprobeandstack x  accessporttopreventunrepresentativedilutionofthegasstream.  8.6.6  ` Traversethestackcrosssection,asrequiredbyMethod1(Reference1).To T  minimizethechanceofextractingdepositedmaterial,becarefulnottobumptheprobenozzleintothestackwallswhensamplingnearthewallsorwhenremovingorinsertingtheprobethroughtheaccessport.  8.6.7  ` Duringthetestrun,makeperiodicadjustmentstokeepthetemperatureofthe  probeandtheheatedfilterattheproperlevels.Addmoreiceand,ifnecessary,salt,tomaintainatemperatureof<20$C(68$F)atthesilicageloutlet.Also,periodicallychecktheleveland  zeroofthemanometerandthepHoftheimpingerscontaining0.1NNaOHsolution.IfthepHoftheNaOHsolutionis<12,replacethatimpingerwithanotherimpingercontainingfreshNaOHsolution.Documentthechangeonthedatasheet.  8.6.8  ` Asingletrainshallbeusedfortheentiresamplingrun,exceptincaseswhere 0 simultaneoussamplingisrequiredintwoormoreseparateducts;attwoormoredifferentlocationswithinthesameduct;or,incaseswhereequipmentfailurenecessitatesachangeoftrains.Additionaltrain(s)mayalsobeusedforsamplingwhenthecapacityofasingletrainisexceeded(e.g.,whenthepHdropsbelow12).Documentonthedatasheetthetimeswhenchangesintrainsoccur,especiallyifmeterboxesarechanged.  8.6.9  ` Whentwoormoretrainsareused,componentsfromeachtrainshallbeanalyzed  " separately.Ifmultipletrainshavebeenusedbecausethecapacityofasingletrainwouldbeexceeded,firstimpingersfromeachtrainmaybecombinedandsecondimpingersfromeachtrainmaybecombined.   8.6.10  ` Attheendofthesamplingrun,turnoffthecoarseadjustvalve,removetheprobe %p" andnozzlefromthestack,switchoffthepump,recordthefinaldrygasmeterreading,andconductaposttestleakcheckasoutlinedinSection8.5.3.Also,leakcheckthePitotlinesasdescribedinMethod2(Section8.1ofReformattedMethod2).Thelinesmustpassthisleakcheckinordertovalidatethevelocityheaddata.  8.6.11  ` Calculatepercentisokineticvariation(asdescribedinSection6.11ofMethod5, t*$' aswellasinSection12.11ofReformattedMethod5)todeterminewhethertherunwasvalidor d+%( anothertestshouldbeperformed. & h   8.7  ` SampleRecovery. Thesamplingtrainisrecoveredinthreefractions(four,ifthe P Pbacetateimpingerisneeded):thefronthalfrinseofthenozzle,probe,andconnectingglasswareaheadofthefilterconstitutethefirstfraction;thefiltermakesupthesecondsubsample;thethreeimpingersolutionsandrinsesfromimpingersandconnectingbackhalfglasswarecomprisethethirdportion.AfourthfractionisnecessaryifthePbAcetate/NaOHtrainconfigurationisemployed.  8.7.1  ` Preparation.  x   8.7.1.1  ` 'hPPropercleanupprocedurebeginsassoonastheprobeisremovedfromthestackat  h theendofthesamplingperiod.Allowtheprobetocool.Whentheprobecanbehandledsafely,wipeoffallexternalparticulatematternearthetipoftheprobenozzleandplaceacapoverthetiptopreventlosingorgainingparticulatematter.Donotcaptheprobetiptightlywhilethesamplingtrainiscoolingbecauseavacuumwillbecreateddrawingliquidformtheimpingersbackthroughthesamplingtrain.  8.7.1.2  ` Beforemovingthesamplingtraintothecleanupsite,removetheprobefromthe X  samplingtrainandcaptheopenoutlet,beingcarefulnottoloseanycondensateorparticulatethatmightbepresent.Removetheumbilicalcordfromthelastimpingerandcaptheimpinger.Ifaflexiblelineisused,letanycondensedwaterorliquiddrainintotheimpingers.Capoffanyopenimpingerinletsandoutlets.Groundglassstoppers,Tefloncaps,orcapsortapeofotherinertmaterialsmaybeusedtosealallopenings.  8.7.1.3  ` Transfertheprobeandimpingerassemblytoanareathatiscleanandprotected  fromwindsothatthechancesofcontaminatingorlosingthesampleareminimized.  8.7.1.4  ` Inspectthetrainbeforeandduringdisassembly,anddocumentonthedatasheet \ anyabnormalconditions.Ifindicatorwasaddedtotheimpingers,documentonthedatasheetthecoloroftheindicator;otherwise,measurethepHofeachofthe0.1NNaOHimpingersolutionswithpHpaperorapHmeterandrecordtheseparatepHmeasurementsonthedatasheet.  8.7.1.5  ` Saveaportionofallwashingsolutions(0.1NNaOHandacetone)usedfor ` cleanupasablank.Transfer100mLofeachsolutiondirectlyfromthewashbottleandplaceeachinaseparateprelabeledsamplereagent blankcontainer(seeSection9.2.2).&    8.7.2  ` SampleContainers. ("   8.7.2.1 ` '("ContainerNo.1(fronthalfrinseforparticulatedetermination).Usingtwo # people,rinsetheprobe/nozzlewithacetonebytiltingandrotatingtheprobewhilesquirtingsolventintotheupperendsothatallofthesurfacesarewettedwiththerinsesolution.Letthesolventdrainintothesamplecontainer.Ifparticulateisvisible,useaTeflonbrushtoloosen/removetheparticulatematerialandfollowwithasecondrinseandbrushing,whichisfollowedbyafinalrinse.Addtherinseofthefronthalfofthefilterhousing(see8.7.2.2)tothiscontainer.Addtheproperlabeldescribingthefacilitytested,testlocation,runnumber,date,time,contents,samplevolumeorweight,andanyapplicablenotes.Ifadeterminationofparticulatematterisnotneeded,thefiltercatchandfronthalfrinsesmaybediscardedfollowingproceduresforproperdisposalofpotentiallyhazardousmaterials. h+%( Ї  8.7.2.2  ` ContainerNo.2(filtercatchforparticulatedetermination).Disassemblethefilter d holderandcarefullyremovethefilterwithTeflontweezers,foldintoquartersandplaceinaprecleanedglassbottle.Capthebottle,addtheproperlabel,andsealwithTeflontape.Rinsethefronthalfofthefilterholder,thefiltersupport,andanyotherfronthalfconnectingglasspieceswithacetoneandaddtherinsestoContainerNo.1.MarktheliquidlevelinContainerNo.1andsealforshipment.Ifadeterminationofparticulatematterisnotneeded,thefiltercatchandfronthalfrinsesmaybediscardedfollowingproceduresforproperdisposalofpotentiallyhazardousmaterials.  8.7.2.3  ` ContainerNo.3.AfterrecordingthepHandweighing,pourthecontentsof  d ImpingersNo.1,2and3intoContainerNo.3alongwiththe0.1NNaOHrinsesoftheimpingersandconnectingglassware.Rinsetheimpingersaminimumofthreetimes.Donotrinsetheback @  halfofthefilterholder.Rinsingthebackofthefilterholdermay,undercertaincircumstances, ,  increasetransferofwatersolublecyanidesaltsfromthefronthalfandtherebycauseapositivebiasintheHCNresults.Marktheliquidlevel,sealthecontainer,andaddthepropersamplelabelwithappropriatedescriptiveinformation.IfthePbAcetate/NaOHtrainconfigurationisemployed,afourthcontainerisnecessary.ThecontentsofthePbAcetateimpinger,thefollowingemptyimpinger,andrinsesofthetwo(PbAcetaterelatedimpingers)andconnectingglasswarebetweenthetwoarerecovered,shipped,andanalyzedseparatelyfromtheNaOHsolution.  8.7.2.4  ` MoistureDetermination.Ifamoisturedeterminationistobemade,measurethe  volume(orweight)gainofeachimpingeraswellastheimpingercontainingthesilicagelbeforetransferringthecontentstothesamplecontainers.  8.7.2.5  ` SamplePreparationforShipment.Priortoshipment,recheckallsample T containerstoensurethatthecapsarewellsecured.SealthelidswithTeflontape.Shipallsamplesupright,packedinice(ifnecessarytoavoidexcessiveheatingduringshippinginhotweather),usingthepropershippingmaterialsasprescribedforhazardousmaterials.  8.7.2.6  ` Samplesarestableinbasicsolutionforapproximatelyfourmonthswhenno l interferents,suchassulfide,arepresentinthesolution.Whensulfideispresentinsolution,thecyanideisstableforlessthanonemonth.Allsamplesshouldbeanalyzedwithin30daysofacquisition,sincethepresenceofimpuritiesfromtheemissionmatrixisalwaysinquestion. &  9.0  QualityControl.   #   9.1  ` ' #-Sampling.SamplingqualitycontrolproceduresarelistedinTableXHCN2.See $! References8and9foradditionalMethod5qualitycontrol.  9.2  ` Analysis.Thequalityassuranceprogramrequiredforthismethodincludesthe &\ # analysisofthefield,reagentandmethodblanks,procedurevalidations,andanalysisoffieldspikes.Theassessmentofcombustiondataandpositiveidentificationandquantitationofhydrogencyanideisdependentontheintegrityofthesamplesreceivedandtheprecisionandaccuracyoftheanalyticalmethodology.Qualityassuranceproceduresforthismethodaredesignedtomonitortheperformanceoftheanalyticalmethodologyandtoprovidethe `+$( informationnecessaryforundertakingcorrectiveactionifproblemsareobservedinlaboratoryoperationsorinfieldsamplingactivities.TableXHCN3listslaboratoryqualitycontrolprocedures.  <   9.2.1 ` FieldTrainBlanks.Submitfieldblankswiththesamplescollectedateach (  samplingsite.ThefieldblanksincludethesamplebottlescontainingaliquotsofunusedNaOHreagent(andleadacetatereagent,ifused).Ataminimum,assembleonecompletesamplingtraininthefieldstagingarea,transportthetraintothesamplingarea,andleakcheckthetrainatthebeginningandendofthetesting(orforthesametotalnumberoftimesastheactualsamplingtrain).Heattheprobeoftheblanktrainduringthesampletest.Recoverthetrainasifitwereanactualtestsample.Donotpassanystackgasthroughtheblanksamplingtrain.  9.2.2  ` ReagentBlanks.Collecta100mLaliquotof0.1NNaOHinthefieldasa <  separatesampleandreturntothelaboratoryforanalysistoevaluateartifactsthatmaybeobservedintheactualsamples.Whentheleadacetate/NaOHtrainconfigurationisused,collecta100mLaliquotof10%leadacetatesolution.Whenparticulatematterisbeingmeasured,itisalsonecessarytocollecta100mLaliquotoftheacetone.  9.2.3 ` LaboratoryMethodBlanks.Prepareamethodblankforeachsetofanalytical @  operations,toevaluatecontaminationandartifactsthatcanbederivedfromglassware,reagents,andsamplehandlinginthelaboratory.  9.2.4 ` FieldSpike.Performafieldspikebyintroducing2mLoftheFieldSpike  Standardintoasingleimpinger(takentothefieldexpresslyforthispurpose,andnotpartoftheactualstacksample)containing100mLofNaOHsolution.Followstandardimpingerrecoveryproceduresandusethespikeasacheckonfieldhandlingandrecoveryprocedures.RetainanaliquotoftheFieldSpikeStandardinthelaboratoryforcomparativeanalysis.   9.2.5 ` PreparationofReagent.TaketwoaliquotsoftheNaOHreagentandtwoaliquots D oftheleadacetatereagent.Thesizeofthealiquotsdependsontheexactsamplingprocedureused,but100mLisreasonablyrepresentative.Toensurethatthebackgroundinthereagentisacceptableforfielduse,analyzeonealiquotofeachreagentaccordingtotheprocedureinSection11.Savetheremainingportionofeachreagentforuseasalaboratorymethodblankwhentheanalysisisperformed.   &  10.0  CalibrationandStandardization.   "    NOTE: Maintainalaboratorylogofallcalibrations. #    10.1  ` ' "QProbeNozzle.Probenozzlesshallbecalibratedbeforetheirinitialuseinthe $! field.Usingamicrometer,measuretheinsidediameterofthenozzletothenearest0.025mm(0.001in.).Makemeasurementsatthreeseparateplacesacrossthediameterandobtaintheaverageofthemeasurements.Thedifferencebetweenthehighandlownumbersshallnotexceed0.1mm(0.004in.).Whentheglassnozzlesbecomecracked,chipped,orbrokentheymustbereplaced.Eachnozzlemustbepermanentlyanduniquelyidentified.  10.2  ` PitotTubeAssembly.TheTypeSPitottubeassemblymustbecalibrated t*$' accordingtotheprocedureoutlinedinSection4ofPromulgatedMethod2(Section10.1of d+%( ReformattedDraftMethod2),orassignedanominalcoefficientof0.84ifitisnotvisiblynickedorcorroded,and,ifitmeetsdesignandintercomponentspacingspecifications.&    10.3  ` MeteringSystem. <   10.3.1  ` '<CalibrationPriortoUse.Beforeitsinitialuseinthefield,themeteringsystem ,  shallbecalibratedaccordingtotheprocedureoutlinedinAPTD0576(Reference4).Insteadofphysicallyadjustingthedrygasmeterdialreadingstocorrespondtothewettestmeterreadings,calibrationfactorsmaybeusedtocorrectthegasmeterdialreadingsmathematicallytothepropervalues.Beforecalibratingthemeteringsystem,itissuggestedthataleak-checkbeconducted.Formeteringsystemshavingdiaphragmpumps,aleakcheckproceduremaynotdetectleakageswithinthepump.Forthesecases,thefollowingleakcheckprocedurewillapply.Makeatenminutecalibrationrunat0.00057m3/min(0.020cfm).Attheendoftherun,record @  thedifferenceofthemeasuredwettestanddrygasmetervolumesanddividethedifferenceby10togettheleakrate.Theleakrateshouldnotexceed0.00057m3/min(0.020cfm). |    10.3.2  ` CalibrationAfterUse.Aftereachfielduse,checkthecalibrationofthemetering h  systembyperformingthreecalibrationrunsatasingleintermediateorificesetting(basedonthepreviousfieldtest).Setthevacuumatthemaximumvaluereachedduringthetestseries.Toadjustthevacuum,insertavalvebetweenthewet-testmeterandtheinletofthemeteringsystem.Calculatetheaveragevalueofthecalibrationfactor.Ifthevaluehaschangedbymorethe5%,recalibratethemeteroverthefullrangeoforificesettings,asoutlinedinAPTD0576(Reference4).  10.3.3  ` LeakCheckofMeteringSystem.Theportionofthesamplingtrainfromthe | pumptotheorificemeter(seeFigureXHCN1)shouldbeleakcheckedpriortoinitialuseandaftereachshipment.Leakageafterthepumpwillresultinlessvolumebeingrecordedthanisactuallysampled.Usethefollowingprocedure.Closethemainvalveonthemeterbox.Insertaoneholerubberstopperwithrubbertubingattachedintotheorificeexhaustpipe.Disconnectandventthelowsideoftheorificemanometer.Closeoffthelowsideorificetap.Pressurizethesystemto1318cm(57in.)watercolumnbyblowingintotherubbertubing.Pinchoffthetubingandobservethemanometerfor1minute.Alossofpressureonthemanometerindicatesaleakinthemeterbox.Leaks,ifpresent,mustbecorrected.   NOTE: Ifthedrygasmetercoefficientvaluesobtainedbeforeandafteratestseries 0! differby>5%,eitherthetestseriesmustbevoidedorcalculationsforthetestseriesshallbeperformedusingwhichevermetercoefficientvalue(i.e.,beforeorafter)givesthelowervalueoftotalsamplevolume.  10.4  ` ProbeHeater.Theprobeheatingsystemmustbecalibratedbeforeitsinitialusein $! thefieldaccordingtotheprocedureoutlinedinAPTD0576(Reference4).ProbesconstructedaccordingtoAPTD0581(Reference3)neednotbecalibratedifthecalibrationcurvesinAPTD0576(Reference4)areused.  10.5  ` TemperatureSensors.Eachtemperaturesensormustbepermanentlyand (4"% uniquelymarkedonthecasing.AllmercuryinglassreferencethermometersmustconformtoASTME163Cor63Fspecifications.Temperaturesensorsshouldbecalibratedinthelaboratorywithandwithouttheuseofextensionleads.Ifextensionleadsareusedinthefield, `+$( thetemperaturesensorreadingsattheambientairtemperatures,withandwithouttheextensionlead,mustbenotedandrecorded.Theinitialtemperatureacquiredfromthesensormustbecorrectedtoobtainthefinaltemperatureifusinganextensionleadproducesachange>1.5%.  10.5.1  ` ImpingerandDryGasMeterTemperatureSensors.Forthetemperaturesensors (  usedtomeasurethetemperatureofthegasleavingtheimpingertrain,athree-pointcalibrationaticewater,roomair,andboilingwatertemperaturesisnecessary.Acceptthetemperaturesensorsonlyifthereadingsatallthreetemperaturesagreeto2$C(3.6$F)withthoseoftheabsolute   valueofthereferencethermometer.  10.5.2  ` ProbeandStackTemperatureSensor.Forthetemperaturesensorsusedto  d indicatetheprobeandstacktemperatures,athreepointcalibrationaticewater,boilingwater,androomairtemperaturesmustbeperformed.Thereferencethermometerandthermocouplemustagreetowithin1.5%ateachofthecalibrationpoints.Acalibrationcurvemaybeconstructedandthedataextrapolatedtocovertheentiretemperaturerangesuggestedbythemanufacturer.$Xv XXX% h  #X%X X$Xv(#   10.6  ` Barometer.Adjustthebarometerinitiallyandbeforeeachtestseriestoagreeto T  within2.5mmHg(0.1in.Hg)ofthemercurybarometerorthecorrectbarometricpressurevaluereportedbyanearbyNationalWeatherServiceStation(samealtitudeabovesealevel).  10.7  ` TopLoadingElectronicBalance.Calibratethebalancebeforeeachtestseries,  usingClassSstandardweights.Theweightsmustbewithin0.5%ofthestandards,orthebalancemustbeadjustedtomeettheselimits.&    10.8  ` AnalyticalCalibration.    10.8.1  ` ']+Establishionchromatographicoperatingparameterstoproducearetentiontime p equivalenttothatindicatedinTableXHCN1.SuggestedchromatographicconditionsareprovidedinSection11.2.PreparecalibrationstandardsaccordingtotheprocedureinSection_7.11.12._ԀCalibratethechromatographicsystemusingtheexternalstandardtechnique(Section10.8.2).&  0  10.8.2  ` ExternalStandardCalibrationProcedure.t(#(#   10.8.2.1 't-Analyzeeachcalibrationstandardusingthechromatographicconditionslistedin d Section11.2,andtabulatepeakareaagainsttheconcentrationinjected.Usetheresultstoprepareacalibrationcurveforhydrogencyanide.  10.8.2.2 Theworkingcalibrationcurvemustbeverifiedoneachworkingdaybythe ," measurementofoneormorecalibrationstandards.Iftheresponseforhydrogencyanidevariesfromthepreviouslyestablishedresponsebymorethan10%(seeTableXHCN3),thetestmustberepeatedusingafreshcalibrationstandard,butonlyafterithasbeenverifiedthattheanalyticalsystemisincontrol.Alternatively,anewcalibrationcurvemaybepreparedforhydrogencyanide.Ifanautosamplerisavailable,itisconvenienttoprepareacalibrationcurvedailybyanalyzingstandardsalongwithtestsamples.  10.8.2.3 PeriodicallyusethecheckstandardpreparedinSection7.11.1.3tocheckthe (@"% instrumentresponseandcalibrationcurve.  *$'     & x 11.0  AnalyticalProcedures.  d 0  11.1  ` AnalysisofStackGasSamples:ImpingerContents(ContainerNo.3,Section < 8.7.2.3).IfthePbAcetate/NaOHtrainconfigurationisemployed,thecontentsofthePbAcetateimpingerisanalyzedseparatelyfromtheNaOHsolution,butthesameanalysisprocedureisfollowed. (#(#   11.1.1  ` 'xd2Measurethesamplevolume.Decidewhetherthesamplesneedtobediluted.   Performanalysis.Ifanalytessaturate,dilutethesolution.  11.1.2  ` Storethesamplesat42$C(394$F).Thesamplesshouldbeanalyzedwithin30  h daysofcollection.  &  11.2  ` ChromatographicConditions. D    '5 ` Column:0  0h(#(#IonPacAS7Analytical,4x250mmwithAG7AGuard 4  column h(#h(#    ` MobilePhase:0  0h(#(#0.1NNaOHand0.5Msodiumacetatein0.5%ethylene p  diamine h(#h(#    ` FlowRate:  0 h 1.0mL/min.H h(#h(#    ` Detector:0  0h(#(#Electrochemicaldetectorwithsilverworkingelectrodeand 4 silver/silverchloridereferenceelectrode h(#h(#    ` InjectorVolume: h 50%L   $Xv XXX%  &    #X%X X$Xv9#11.3  ` ICAnalysis.    11.3.1 'F9AnalyzesamplesbyIC,usingconditionsestablishedinSection11.2.Table t XHCN1liststheretentiontimeandMDLthatwereobtainedundertheseconditions.OtherICcolumns,chromatographicconditions,ordetectorsmaybeusediftherequirementsforSection9.2.aremetorifthedataarewithinthelimitsdescribedinTableXHCN1.  11.3.2  ` Thewidthoftheretentiontimewindowusedtomakeidentificationsshouldbe ( baseduponmeasurementsofactualretentiontimevariationsofstandardsoverthecourseofaday.Threetimesthestandarddeviationofaretentiontimeforacompoundcanbeusedtocalculateasuggestedwindowsize;however,theexperienceoftheanalystshouldweighheavilyintheinterpretationofthechromatograms.  11.3.3  ` Ifthepeakareaexceedsthelinearrangeofthecalibrationcurve,asmallersample ," volumeshouldbeused.Alternatively,thefinalsolutionmaybedilutedwithmobilephaseandreanalyzed.  11.3.4  ` Ifthepeakareameasurementispreventedbythepresenceofobserved $! interferences,differentchromatographicproceduresorsamplecleanupmayberequired.However,nomethodhasbeenevaluatedforthisprocedure.Ifabsolutelynecessarytoavoidspecificinterferences,alternatemethodsforanalysisofcyanideioncanbesubstituted. 'X!$ 0  11.4  ` AnalysisofFilterCatchandFrontHalfRinses(Containers1and2,Sections (D"% 98.7.2.1and_98.7.2.2)._ (#(#    11.4.1  ` Thefiltercatchandfronthalfrinsesmaybeanalyzedforparticulatematter * $' followingtheproceduresofMethod5(Reference1).Ifadeterminationofparticulatematteris t+%( notneeded,thefiltercatchandfronthalfrinsesmaybediscardedfollowingproperproceduresfordisposalofpotentiallyhazardousmaterials.Thefilterandfronthalfrinsesarenotanalyzedforcyanideion,sincetheywillcontainonlyparticulatecyanidematerialandshouldnotbeaddedtotheHCNresults. &  12.0  CalculationsandDataAnalysis.      ' BCarryoutcalculations,retainingatleastoneextradecimalfigurebeyondthatoftheacquireddata.Roundofffigurestothecorrectnumberofsignificantfiguresafterfinalcalculations.    12.1  ` Nomenclature: 8  9,XX X,XXX9XuXXX%   ` AIC =  AcceptableImpurityConcentration(%g/mL) x     ` An =0  Cross-sectionalareaofnozzle,m2(ft2).h (#(#    ` Bws =0  Watervaporinthegasstream,proportionbyvolume.X (#(#    ` Cd0 =0 (# (#TypeSPitottubecoefficient(nominally0.840.02), H  dimensionless. (#(#    ` Cf =  Concentrationofhydrogencyanideinstackgas(%g/dscm) (    ` EAC =  ExpectedAnalyteConcentration(ppbv)     ` FW =  Formulaweightofanalyte(g/mole)     ` I0 =0 (# (#Percentofisokineticsampling.(#(# #X%XXXuiD#   ` K =  35.31ft3/m3ifVm(std)isexpressedinEnglishunits     ` K =  1.00m3/m3ifVm(std)isexpressedinmetricunitsXuXXX% p    ` K1 =  0.3853K/_mm_ԀHgformetricunits,or \    ` K1 =  17.64$R/in.HgforEnglishunits. L #X%XXXuI#XuXXX%   ` K2 =  0.001333m3/mLformetricunits,or <    ` K2 =  0.04707ft3/mLforEnglishunits.#X%XXXu)K#XuXXX% ,    ` K3 =  0.003454_mm_ԀHgm3/mLKformetricunits,or     ` K3 =  0.002669in.Hgft3/mL$RforEnglishunits.#X%XXXuBL#XuXXX% p     ` K4 =  4.320formetricunits,or `!    ` K4 =  0.09450forEnglishunits. P" #X%XXXuM#XuXXX%   ` L10 =0 (# (#Individualleakagerateobservedduringtheleak-checkconducted @# priortothefirstcomponentchangem3/min(cfm).0$ (#(#    ` La0 =0 (# (#Maximumacceptableleakagerateforaleak-check,eitherpretest  %! orfollowingacomponentchange;equalto0.00057m3/min &" (0.020cfm)or4%oftheaveragesamplingrate,whicheverisless. (#(#    ` Li0 =0 (# (#Individualleakagerateobservedduringtheleak-checkconducted '!$ priortothe"ith"componentchange(i=1,2,3...n)m3/min(cfm).(|"%(#(#    ` Lp0 =0 (# (#Leakagerateobservedduringthepost-testleak-check,m3/min )l#& (cfm). (#(#    ` Md0 =0 (# (#Stackgasdrymolecularweight,g/g-mole(lb/lb-mole).+L%((#(#    ` _Mvol_ =  Totalvolumeofrecoveredsample(mL) d    ` Mw0 =0 (# (#Molecularweightofwater,18.0g/g-mole(18.0lb/lb-mole).T(#(#    ` Pbar0 =0 (# (#Barometricpressureatthesamplingsite,mmHg(in.Hg).D(#(#    ` PC =  Concentrationofhydrogencyanideinsample(%g/mL) 4     ` Ps0 =0 (# (#Absolutestackgaspressure,mmHg(in.Hg).$ (#(#    ` Pstd0 =0 (# (#Standardabsolutepressure,760mmHg(29.92in.Hg). (#(#    ` PT =  Totalhydrogencyanideinsample(%g).      ` R0 =0 (# (#Idealgasconstant,0.06236_mm_ԀHg-m3/K-g-mole(21.85in.   Hg-ft3/$R-lb-mole). (#(#    ` _Rvol_ =0  VolumeofNaOHreagentusedintheimpingers(mL).p (#(#    ` _Svol_ =0  Volumeofairsampledatstandardconditions(L).` (#(#    ` Tm0 =0 (# (#Absoluteaveragedrygasmetertemperature,K($R).P (#(#    ` Ts0 =0 (# (#Absoluteaveragestackgastemperature,K($R).@ (#(#    ` Tstd0 =0 (# (#Standardabsolutetemperature,293K(528$R).0 (#(#    ` Vadj =  Volumeofsamplealiquotafterdilution.      ` Valiq =  Volumeofaliquotused. t    ` Vlc0 =0 (# (#Totalvolumeofliquidcollectedintheimpingersandsilicagel, d mL. (#(#    ` Vm0 =0 (# (#Volumeofgassampleasmeasuredbydrygasmeter,dscm(dscf).D(#(#    ` Vm(std) =0  Volumeofgassamplemeasuredbythedrygasmeter,correctedto 4 standardconditions,dscm(dscf). (#(#    ` Vw(std) =0  Volumeofwatervaporinthegassample,correctedtostandard  conditions,scm(scf). (#(#    ` Vs0 =0 (# (#Stackgasvelocity,calculatedbyMethod2,Equation2-9,using  dataobtainedfromMethod5,m/sec(ft/sec). (#(#    ` 0 =0 (# (#Drygasmetercalibrationfactor,dimensionless.p(#(#    ` H0 =0 (# (#Averagepressuredifferentialacrosstheorificemeter,mmH2O(in. ` H2O).P(#(#    ` #w0 =0 (# (#Densityofwater,0.9982g/mL(0.002201lb/mL). @(#(#    ` 0 =0 (# (#Totalsamplingtime,min.!0(#(#    ` 10 =0 (# (#Samplingtimeintervalfromthebeginningofarununtilthefirst "  componentchange,min. (#(#    ` i0 =0 (# (#Samplingtimeintervalbetweentwosuccessivecomponent d$  changes,beginningwiththeintervalbetweenthefirstandsecondchanges,min. (#(#    ` p0 =0 (# (#Samplingtimeintervalfromthefinal(nth)componentchangeuntil 4' # theendofthesamplingrun,min. (#(#    ` 13.60 =0 (# (#Specificgravityofmercury.)"%(#(#    ` 600 =0 (# (#sec/min.*#&(#(#    ` 1000 =0 (# (#Conversiontopercent.*$'(#(#  +%( - ,XX,XX X-#X%XXXuO#  12.2  ` AverageDryGasMeterTemperatureandAverageOrificePressureDrop.See d fielddatasheet.XuXXX%  12.3  ` DryGasVolume.Correctthesamplemeasuredbythedrygasmetertostandard @ conditions(20$C,760mmHg[68$F,29.92in.Hg])byusingEquationXHCN1: 0  DRX%H84zx `v p @E x  L x  (#(#   (#(#  ItshouldbenotedthatEquationXHCN1canbeusedaswritten,unlesstheleakagerateobservedduringanyofthemandatoryleak-checks(i.e.,thepost-testleak-checkorleak-checksconductedpriortocomponentchanges)exceedsLa.IfLporLiexceedsLa,EquationXHCN1 l  mustbemodifiedasfollows:  a.0 ` CaseI(nocomponentchangesmadeduringsamplingrun):ReplaceVmin <  EquationXHCN1withtheexpression: ` (#` (# @aa"Vm-(Lp-La)       b.0 ` CaseII(oneormorecomponentchangesmadeduringthesamplingrun):Replace ` VminEquationXHCN1bytheexpression:P` (#` (# D-.QA=zx 0 @Xdddddddd@E@x!<dYL@@ (#(#    (#(#  0 ` 0 ` (#` (#andsubstituteonlyforthoseleakagerates(LiorLp)thatexceedLa. (# (#   &  12.4  ` VolumeofWaterVaporCondensed.  'Bo  12.5  ` MoistureContent. | D/LZRB>zx p @Xdddddddd@Ex d LL@7 (#(#    (#(#0   ` NOTE: Insaturatedorwaterdroplet-ladengasstreams,twocalculationsofthe p#  moisturecontentofthestackgasshallbemade,onefromtheimpingeranalysis(EquationXHCN3)andasecondfromtheassumptionofsaturatedconditions.ThelowerofthetwovaluesofBwsshallbeconsideredcorrect.Theprocedurefordetermining @&" themoisturecontentbaseduponassumptionofsaturatedconditionsisgiveninthe NOTE toSection1.2ofPromulgatedMethod4(Section4.0ofReformattedDraft  (!$ Method4).Forthepurposesofthismethod,theaveragestackgastemperaturemaybeusedtomakethisdetermination,providedthattheaccuracyofthein-stacktemperaturesensoris1$C(2$F).*$'(#(#  +|%(   &   12.6  ` ConversionFactors. d *23` dddd dd dddd '(#(#,LL ,LL ,LL +  ," D L@,From ',@ @'To ',@ @'Multiplyby ?5,@ L  L?scf   h m3 C9  h wJ?0.02832wJ?C0.02832 [Q9 h wJ?0.02832 L  wJ? L[g/ft3     gr/ft3 A7    \(.@15.43\(.@A15.43 YO7   \(.@15.43 L  \(.@ LYg/ft3  D   lb/ft3  D   2.205x103 6,D  L  L6g/ft3    g/m3 A7   HzA@35.31HzA@A35.31' dntG=;  HzA@35.31 L   HzA@ G  12.6.1  ` Nomenclature. `    ` scf standardcubicfeet P     ` g/ft3 gramspercubicfoot @     ` gr/ft3 grainspercubicfoot 0    12.7  ` IsokineticVariation.      ` 12.7.1  CalculationFromRawData.  D67HRB>zx p @Xdddddddd@Ex4d LL@7 (#(#    (#(#   ` 12.7.2  CalculationForIntermediateValues. , DWVIQA=zx 0 @Xdddddddd@Ex[ dLL@% (#(#      (#(##X%XXXu7h#  12.8  ` ConcentrationofHydrogenCyanideinSample.Aleastsquareslinearregression  "& analysisofthecalibrationstandardsshallbeusedtocalculateacorrelationcoefficient,slope,andintercept.ConcentrationsaretheXvariable,andresponseistheY-variable.  12.9  ` CalculationofTotalWeightofHydrogenCyanideintheSample.Todetermine $) thetotalhydrogencyanideusethefollowingequation:kD ![3#p 0  `E&x8 dp&L& k (#(#     (#(#  NOTE: Addthe%gofHCNfoundinthePbAcetateimpinger(wheneveritisutilized)to `+$0 thetotalbeforecalculatingtheconcentrationinthestackgas.  12.10  ` HydrogenCyanideConcentrationinStackGas.Determinethehydrogencyanide P concentrationinthestackgasusingthefollowingequation:kDK\>3#p 0  `E- x8 d3p&L,  k (#(#     (#(#  12.11  ` CalculatetheAcceptableConcentrationsofImpuritiesinNaOHReagentas  d follows:kD]3#p 0  `Exd NL k (#(#& L ԰      (#(#   ` where:   `  'L0.1istheacceptablecontaminantconcentration,   `  22.4isafactorrelatingppbvtog/L,   `  1,000isaunitconversionfactor.   &  13.0  MethodPerformance.  P   13.1  ` 'MethodPerformanceEvaluation.Theexpectedmethodperformanceparameters ( forprecisionandaccuracyareprovidedinTableXHCN4.ThisinformationwasdeterminedaspartofthemethoddevelopmentandevaluationprojectreportedinReferences10and11.@X%XXX%Afield h testprogramwasconductedinordertoevaluatethemethodaccordingtoMethod301.Thedraft T samplingmethodexhibitedoutstandingperformanceinthelaboratorycollectionefficiencytrials,butperformedpoorlyduringtheMethod301(Reference12)fieldtestatahazardouswasteincinerator.Subsequentlaboratoryexperimentssupportedthehypothesisthatthefieldfailurewasduetoexcessivelevelsofacidityintheincineratoremissions.Thisreviseddraftmethod,whichisdesignedtobetoleranttohigheracidlevelsispresentedinthisdocumentandisrecommendedforuseonhazardouswasteincinerators,coalfiredpowerplants,andsimilarcombustionsources. Inspiteofthefailedfieldtest,thisisthebestdocumentedandverified %d" methodavailableforsamplingHCNfromstationarysources(References10and11).  &P #  #X%XX@X%|#  13.2  ` TheMDLconcentrationslistedinTableXHCN1wereobtainedusinginstrument ',%) p  y&8TC 3/p> ;  `T #Erx&x%%%.e'P' y (#(#                                          >,%) y&*`C 3/p> H  `a #Erx&x% %8e'P' y (#(#                                          >,%) q  qTABLEXHCN1.LISTOF_ANALYTES_,_CAS_ԀNUMBERS,RETENTIONTIMES,AND@"DETECTIONLIMITS*}B'CSd` dLL LL LL 23(#(#},dd ,dd ,dd,dd +  .;' 6  .CompoundName @;'/! (";' @_CAS_ԀNo.a @;'/! (";' @RetentionTime(minutes)b @;'/! ";' @MethodDetectionLimits(_MDL_)(_g_/_m3_)c 5+&r  "  ;' 5HydrogenCyanide 0&   074908 ZP!  " @6.7@Z6.7 zpB  U @6.7 @  (@12(@z12QGE "  (@12  (@ Q-,X` X,XX-r ra0  ʗXX%ChemicalAbstractServicesRegistryNumber(#(# b0  Analyticalconditions(ionchromatography,IC):AS7Acolumn,4x250mm,withAG7Aguardcolumn;   _isocratic_Ԁelutionusing0.5%ethylenediamine,0.5Msodiumacetate,and0.1Nsodiumhydroxide;flowrate1.0_mL_/min.;electrochemicaldetectorwithsilverworkingelectrodeandsilver/silverchloridereferenceelectrode;injectionvolume50_L_. (#(# c0  Foran849Liter(30cubicfoot)sample,basedonaninstrumentdetectionlimitof24.54_ppb_Ԁasdetermined d  usingAppendixBPart136DefinitionandProcedurefortheDeterminationoftheMethodDetectionLimitRevision1.11,FederalRegister,Vol.49,No.209,Friday,October26,1984. (#(# #X%Xʗ#r r   TABLEXHCN2.SAMPLINGQUALITYCONTROLPROCEDURES  r *'fSdddd dd dddd B'C(#(#,( dd ,( dd ,( dd +   J  Criteria -#!<" ;' - ControlLimits a 0&!<" ;' 0 CorrectiveAction 2(&<"   ;' 2FinalLeakRateDryGasMeterCalibrationIndividualCorrectionFactor f  () R  AverageCorrectionFactorIntermediateDryGasMeterAnalyticalBalance(toploader)Barometer -#!v -0.00057_m3_/minor4%of .  samplingrate,whicheverisless.Posttestaveragedrygasmetercalibrationfactoragrees5%ofpretestdrygasmetercalibrationfactor.Agreewith2%ofaveragefactor.1.001%.CalibratedeverysixmonthsagainstEPAstandard.0.1gofNBSClassSWeights.Within2.55mmHgofmercuryinglassbarometer. 0&!b4 0  None:Resultsarequestionableandshouldbecomparedwithothertrainresults.Adjustsamplevolumesusingthefactorthatgivesthesmallestvolume.Redocorrectionfactor.Adjustthedrygasmeterand_recalibrate_.̄Repairbalanceand_recalibrate_._Recalibrate_. -#!vK - -#! pL - 0&! pM 01'% pN"   1aControllimitsareestablishedbasedonprevioustestprogramsconductedbytheEPA. "xO   '!T @&&TABLEXHCN3.LABORATORYQUALITYCONTROLPROCEDURES@#FORICANALYSIS  ^ *}g'hSdd( dd ( dd ( dd 'f(#(#},dd ,xdd ,dd ,dd ,` dd +  2;% 6  <2ʗXX%Parameter <;/!r ";' <QualityControlCheck <;/!8 ";' <Frequency <;/!r ";' <AcceptanceCriteria <;/!8  ";' <CorrectiveAction C9,r   <  ;' <CLinearityCheck 'R   'Run5pointcurve. '   'Atsetuporwhencheckstandardisoutofrange ' 2 'Correlationcoefficient   0.995 0& l 0Checkintegration,reintegrate.Ifnecessary_recalibrate_. >4'  <  <>RetentionTime 'L 'Analyzecheckstandard '  '1/10samples 'L 'Withinthreestandarddeviationsofaveragecalibrationrelativeretentiontime 0&( " 0Checkinstrumentfunctionforplug,etc.Heatcolumn. >4' $ <  <>CalibrationCheck '& 'Analyzecheckstandard '( '1/10injections,minimum2/set '* '10%ofcalibrationcurve 0&". 0Checkintegration,remakestandard.Or_recalibrate_. >4'0 <  <>MethodBlank '<1 'Analyze0.1N_NaOH_ 't3 '1/day '<4 '<5%levelofexpected_analyte_ 0&8 0Locatesourceofcontamination;_reanalyze_ >4't: <  <>MatrixSpike/MatrixSpikeDuplicate '4= 'Analyzespikedsample 'n? '1/setor1/10samples 'nA '15%ofspikedamount 0&nC 0Checkintegration,checkinstrumentfunction,_reanalyze_Ԁ,reprepareifpossible >4'lG <  <>ReplicateSamples 'L I 'Analyzeduplicatesamplealiquot '!L '1/setor1/10samples 'L N '25%offirstaliquot 0&L P 0Checkintegration,checkinstrumentfunction,_reanalyze_,reprepareifpossible#X%Xʗ#7-+!S <   7  "jT TABLEXHCN4.EXPECTEDMETHODPERFORMANCEFORHYDROGENCYANIDEBASEDONLABORATORYEVALUATION  ^ ʗXX%*ij dddd xdd dd dd ` dd g'h(#(#,dd ,ddb,dd",dd",dd"+  /;"   c<$/Train 9;,!L "; 9Precision L  (%_RSD_)a 9;,! "; 9Accuracy(%Recovery)b 9;,! "; 9Matrix 9;,!L  "; 9ConcentrationLevel(_ppmv_) K'>, f " <$ c ; q<$K_NaOH_ U'H  ' RQ@4.08RQ@U4.08 'sC " RQ@4.08 RQ@' @X@97.0@X@97.0 ^'QC " @X@97.0 @X@' ^Dryair ]'P! "' 333333?1.2333333?]1.2 dZM " 333333?1.2 <$ q 333333?' <$ d_PbAc_/_NaOH_ RH$   zG?1.18zG? R1.18 }sC$ " zG?1.18 zG?  `W@93.5`W@ }93.5 [QC$ " `W@93.5 `W@   [25%moisture ZP!$ "  333333?1.2333333? Z1.2 _UH$ " 333333?1.2 <$ 333333?  <$ __PbAc_/_NaOH_ SIJ  = ףp]D@40.73= ףp]D@ S40.73 ~tDJ" = ףp]D@40.73 = ףp]D@  fffff&L@56.3fffff&L@ ~56.3 [QCJ" fffff&L@56.3 fffff&L@   [Dryair/10_ppmv_H2S ZP!"  ?0.5? Z0.5 f;UHJ" ?0.5 <$ ?  <$f_NaOH_ Z;I6 ; Q+:@26.17Q+:@Z26.17 ;tD6 " Q+:@26.17 Q+:@; 33333SQ@69.333333SQ@69.3 b;QC6 " 33333SQ@69.3 33333SQ@; b27%moisture/10_ppmv_ԀH2S a;P! !"; ?0.5?a0.5XNL6 "" ?0.5 <$  ?; XaRelativeStandardDeviation(%)forthreespikedtrains. : # bAveragepercentofspikedHCNrecoveredforthreespikedtrains r $ #X%Xʗ_#