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"System--2 Dry Gas+-- .  --2  Meter&-- .  -- 2 Ice-- .  -- 2 Bath-- .  --2 UvVacuumU-- .  -- 2 `Line`-- .  -- 2 nMainn-- .  --2 yValvey-- .  --2 A%VacuumAJ-- .  --2 L)GaugeLG-- .  --2 oBypasso-- .  --2 yValvey-- .  -- 2 Pump -- .  --2 KOrificeK-- .  --2  Temperature6-- .  --2 Sensors+-->%~|yvtqnligf^^--6%^^_bfjnruwxxyzz|~~-- !--%-- !--%--%----------------------------------<--=-- %#-- %####--#--##-- .  --2 Temperature-- .  --2 Sensor--$%$9%9%9';)>,@+D(G#HHHFF I J M--$%$5&6+8/<1>2A3C3E4G4H5I5I5J6K6K8M-- %  -- %|HHm----e-- .  --2 Stack-- .  -- 2 Wall -- .  --2 < Heat Traceds-- .  --2 IQuartz j-- .  --2 JProbee-- .  --2 MLinerc-- .  --2  Manometer F-- .  --2 zx S-Type Pitot z-- .  -- 2 Tube-- .  --2 w Gooseneck-- .  --2 Nozzle--- $--- %---$---%--- $--- %---$---%--- $4 ,94 --- %4 ,94 ---$KKKKK11K---%KKKKK11K-- !M --% R MMR R R-- !M6--%6R6M<M<R6R6R--% R _/m/99R--s/s3--z/z3--/3--p/p2--v/v2--}/}2--c`--fb--h#e%--k*h+--a]--b`--eb--g!e!--j'g(--`]--%                                  -- %'--X%*788:<=?@@ABBB@>=<<;;;;$;$444320/,,,/1356777$7---0$ACDFFFED B!A!AA?>=<<=>@ A A---2%ACDFFFED B!A!AA?>=<<=>@ A AA--- $SEQS--- %SEQS---$oooooKKo---%oooooKKo-- .  --2 w Temperature-- .  --2  Indicator-- !B--%SBBSS-- %CJR--%sxx--s|s--|--s--,%s|||{{zzyyxxsxryryqyqzq{q{r|s|--d}n}--dn--%xvukd-- %sxsxtuuswqyo{n~mnnoqid--- ! n} ! } ! } ! | ! | ! |---- !|---- !  !  !  !  ! z !n---.%y_z]{\|[~ZZ[\^_y_z_{a{b}d~ddcb`_--.%`_]\[[\]_```bceeedca`-Times New Roman1-- .  --62 Figure 207-1-1. 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E--%PEEPP-tM"&ğ&:t0&:t(&:f:\user\gmcalist\wp\figur1-r.wpd 6k9#  o[X` hp x (#%'0*,.8135@8:<H?AXo  _{XX@<< < !  _XhfXXXItisproposedthatAppendixMofPart51beamendedtoreadas  follows:0  1.TheauthoritycitationforPart51continuestoreadasfollows:Authority:42U.S.C.7410 (#(# 0  2.ByaddingMethod207toreadasfollows: (#(# @ METHOD207AMethodforMeasuring_Isocyanates_ԀinStationarySourceEmissions  NOTE: Thismethodisnotinclusivewithrespectto  \  specifications(e.g.,equipmentandsupplies)andsampling  @  proceduresessentialtoitsperformance.SomematerialisincorporatedbyreferencefromotherEPAmethods.Therefore,toobtainreliableresults,personsusingthismethodshouldhaveathoroughknowledgeofatleastMethod1,Method2,Method3,andMethod5foundinPart60ofthistitle.1.0  ScopeandApplication.     1.1Thismethodisapplicabletothecollectionandanalysisofisocyanatecompoundsfromtheemissionsassociatedwithmanufacturingprocesses.Thefollowingisalistofthe_isocyanates_Ԁandthemanufacturingprocessatwhichthemethodhasbeenevaluated:*01 ddd Xdd Xdd X(#(#,XX ,nXX ,XX ,XX +  323"  (3CompoundName =23,!B23 =_CAS_No. =23,!&"23 =DetectionLimits(_ng_/m3)a =23,!&""23 =Manufacturing ^# Process ND,B$  ( 23 XN2,4-TolueneDiisocyanate(_TDI_)  ' 584-84-9 'H)" '106 '"r*" 'FlexibleFoamProduction 6,H, X  X61,6-_Hexamethylene_Diisocyanate(_HDI_)  ~#0 822-06-0 '!"2" '396 ' L3" 'PaintSprayBooth 6,!"5 X  X6MethyleneDiphenylDiisocyanate(MDI)  .'~"9 101-68-8 '% ;" '112 '$<" 'PressedBoardProduction =3,% > X  0X=MethylIsocyanate(MI) 43#*X%A3 4624-83-9 =3,!2)$C"3 =228 =3,!\(#D"3 =Notusedinproduction3)'2)$F X 0  3 30  a0` (#(#Estimateddetectionlimitsarebasedonasamplevolume +'G of1m3anda10_ml_Ԁsampleextractionvolume.,'H` (#` (#  p-(I _ԇ2.0  SummaryofMethod.    2.1Gaseousand/oraerosolisocyanatesarewithdrawnfromanemissionsourceatanisokineticsamplingrateandarecollectedinamulticomponentsamplingtrain.Theprimarycomponentsofthetrainincludeaheatedprobe,threeimpingerscontainingthederivatizingreagentintoluene,anemptyimpinger,animpingercontainingcharcoalandanimpingercontainingsilicagel.  2.2Theimpingercontentsareconcentratedtodrynessundervacuum,broughttovolumewithacetonitrile(ACN)andanalyzedwithahighpressureliquidchromatograph(HPLC).3.0  Definitions.NotApplicable.   4.0  Interferences. F    4.1Thegreatestpotentialforinterferencecomesfromanimpurityinthederivatizingreagent,1-(2-pyridyl)piperazine(1,2PP).ThiscompoundmayinterferewiththeresolutionofMIfromthepeakattributedtounreacted1,2PP.  4.2Otherinterferencesthatcouldresultinpositiveornegativebiasare(1)alcoholsthatcouldcompetewiththe1,2PPforreactionwithanisocyanateand(2)othercompoundsthatmaycoelutewithoneormoreofthederivatizedisocyanates.  4.3Methodinterferencesmaybecausedbycontaminantsinsolvents,reagents,glassware,andothersampleprocessinghardware.Allthesematerialsmustberoutinelyshowntobefreefrominterferencesunderconditionsoftheanalysisbypreparingandanalyzinglaboratorymethod(orreagent)blanks.  4.3.1Glasswaremustbecleanedthoroughlybeforeusing.Theglasswareshouldbewashedwithlaboratorydetergentinhotwaterfollowedbyrinsingwithtapwateranddistilledwater.Theglasswaremaybecleanedbybakinginaglasswareovenat400$Cforatleastonehour.Aftertheglasswarehascooled, .!~" theglasswareshouldberinsedthreetimeswithmethylenechlorideandthreetimeswithacetonitrile.Volumetricglasswareshouldnotbeheatedto400$C.Instead,afterwashingand #% rinsing,volumetricglasswaremayberinsedwithACNfollowedbymethylenechlorideandallowedtodryinair.  4.3.2Theuseofhighpurityreagentsandsolventshelpstoreduceinterferenceproblemsinsampleanalysis.5.0  Safety. ($+   5.1Thetoxicityofeachreagenthasbeenpreciselydefined.Eachisocyanatecanproducedangerouslevelsofhydrogencyanide(HCN).Theexposuretothesechemicalsmustbereducedtothelowestpossiblelevelbywhatevermeansavailable.  ,8(0 Thelaboratoryisresponsibleformaintainingacurrentawareness -)1 fileofOccupationalSafetyandHealthAdministration(OSHA)regulationsregardingsafehandlingofthechemicalsspecifiedinthismethod .Areferencefileofmaterialsafetydatasheets x shouldalsobemadeavailabletoallpersonnelinvolvedinthechemicalanalysis.Additionalreferencestolaboratorysafetyareavailable.6.0  EquipmentandSupplies.     6.1SampleCollection.Thefollowingitemsarerequiredforsamplecollection:  6.1.1AschematicofthesamplingtrainusedinthismethodisshowninFigure2071.ThissamplingtrainconfigurationisadaptedfromEPAMethod5procedures,and,assuch,mostoftherequiredequipmentisidenticaltothatusedinEPAMethod5determinations.Theonlynewcomponentrequiredisacondensercoil.  6.1.2ConstructiondetailsforthebasictraincomponentsaregiveninAPTD-0581(seeMartin,1971,inSection16.0,References);commercialmodelsofthisequipmentarealsoavailable.Additionally,thefollowingsubsectionslistchangestoAPTD-0581andidentifyallowabletrainconfigurationmodifications.  6.1.3BasicoperatingandmaintenanceproceduresforthesamplingtrainaredescribedinAPTD-0576(seeRom,1972,inSection16.0,References).Ascorrectusageisimportantinobtainingvalidresults,allusersshouldrefertoAPTD-0576andadopttheoperatingandmaintenanceproceduresoutlinedthereinunlessotherwisespecified.Thesamplingtrainconsistsofthecomponentsdetailedbelow.  6.1.3.1ProbeNozzle.Glasswithsharp,tapered(30$ J angle)leadingedge.Thetapershallbeontheoutsidetopreserveaconstantinternaldiameter.Thenozzleshallbebuttonhookorelbowdesign.Arangeofnozzlesizessuitableforisokineticsamplingshouldbeavailableinincrementsof0.16cm(1/16in.),e.g.,0.32-1.27cm(1/8-1/2in.),orlargerifhighervolumesamplingtrainsareused.&  ԀEachnozzleshallbecalibratedaccordingtotheproceduresoutlinedinParagraph10.1.'#7   6.1.3.2Probeliner.Borosilicateorquartz-glasstubingwithaheatingsystemcapableofmaintainingaprobegastemperatureof12014$C(24825$F)attheexitendduring ,'|") sampling.(Thetestermayopttooperatetheequipmentatatemperaturelowerthanthatspecified.)Becausetheactualtemperatureattheoutletoftheprobeisnotusuallymonitoredduringsampling,probesconstructedaccordingtoAPTD-0581andusingthecalibrationcurvesofAPTD-0576(orcalibratedaccordingtotheprocedureoutlinedinAPTD-0576)areconsideredacceptable.Eitherborosilicateorquartzglassprobelinersmaybeusedforstacktemperaturesuptoabout480$C(900$F). -,)1 Quartzglasslinersshallbeusedfortemperaturesbetween480and900$C(900and1650$F).(Thesofteningtemperaturefor  borosilicateis820$C(1508$F),andforquartzglass1500$C \ (2732$F).)Water-coolingofthestainlesssteelsheathwillbe 2 necessaryattemperaturesapproachingandexceeding500$C. X   6.1.3.3Pitottube.TypeS,asdescribedinSection2.1ofpromulgatedEPAMethod2orotherappropriatedevices(seeVollaro,1976inSection16.0,References).Thepitottubeshallbeattachedtotheprobetoallowconstantmonitoringofthestack-gasvelocity.Theimpact(high-pressure)openingplaneofthepitottubeshallbeevenwithorabovethenozzleentryplane(seeEPAMethod2,Figure2-6b)duringsampling.TheTypeSpitottubeassemblyshallhaveaknowncoefficient,determinedasoutlinedinSection4.0ofpromulgatedEPAMethod2.  6.1.3.4DifferentialPressureGauge.InclinedmanometerorequivalentdeviceasdescribedinSection2.2ofpromulgatedEPAMethod2.Onemanometershallbeusedforvelocity-head(deltaP)readingsandtheotherfororificedifferentialpressure(deltaH)readings.  6.1.3.5ImpingerTrain.Six500mLimpingersareconnectedinserieswithleakfreegroundglassjointsfollowingimmediatelyaftertheheatedprobe.ThefirstimpingershallbeoftheGreenburgSmithdesignwiththestandardtip.TheremainingfiveimpingersshallbeofthemodifiedGreenburgSmithdesign,modifiedbyreplacingthetipwitha1.3cm(1/2in.)I.D.glasstubeextendingabout1.3cm(1/2in.)fromthebottomoftheoutercylinder.Thefirst,secondandthirdimpingersshallcontainknownquantitiesofthederivatizingreagentintoluenewiththefirstimpingercontaining300mLand200mLinthesecondandthird.Thefourthimpingerremainsempty.Thefifthimpingerisfilledwithaknownamount(2/3full)ofactivatedcharcoalandthesixthwithaknownamountofdesiccant.Awaterjacketedcondenserisplacedbetweentheoutletofthefirstimpingerandtheinlettothesecondimpingertoreducetheevaporationoftoluenefromthefirstimpinger.  6.1.3.6MeteringSystem.Thenecessarycomponentsareavacuumgauge,leak-freepump,temperaturesensorscapableofmeasuringtemperaturetowithin3$C(5.4$F),dry-gasmeter #% capableofmeasuringvolumetowithin1%,andrelatedequipment,asshowninFigure2071.Ataminimum,thepumpshouldbecapableoffourcubicfeetperminute(cfm)freeflow,andthedry-gasmetershouldhavearecordingcapacityof0-999.9cubicfeet(cuft)witharesolutionof0.005cuft.Othermeteringsystemscapableofmaintainingsamplingrateswithin10%ofisokineticityandofdeterminingsamplevolumestowithin2%maybeused.Themeteringsystemmustbeusedwithapitottubetoenablechecksofisokineticsamplingrates.SamplingtrainsusingmeteringsystemsdesignedforflowrateshigherthanthosedescribedinAPTD-0581andAPTD-0576maybeused,ifthespecificationsofthismethodaremet. -(1   6.1.3.7Barometer.Mercury,aneroid,orotherbarometercapableofmeasuringatmosphericpressuretowithin2.5mmHg(0.1in.Hg).OftenthebarometricreadingmaybeobtainedfromanearbyNationalWeatherServicestation,inwhichcasethestationvalue(whichistheabsolutebarometricpressure)isrequestedandanadjustmentforelevationdifferencesbetweentheweatherstationandsamplingpointisappliedatarateofminus2.5mmHg(0.1in.Hg)per30-m(100ft)elevationincrease(viceversaforelevationdecrease).  6.1.3.8Gasdensitydeterminationequipment.Temperaturesensorandpressuregauge(asdescribedinSections2.3and2.4ofEPAMethod2,andgasanalyzer,ifnecessary(asdescribedinEPAMethod3).Thetemperaturesensorideallyshouldbepermanentlyattachedtothepitottubeorsamplingprobeinafixedconfigurationsuchthatthetipofthesensorextendsbeyondtheleadingedgeoftheprobesheathanddoesnottouchanymetal.Alternatively,thesensormaybeattachedjustbeforeuseinthefield.Note,however,thatifthetemperaturesensorisattachedinthefield,thesensormustbeplacedinaninterference-freearrangementwithrespecttotheTypeSpitottubeopenings(seepromulgatedEPAMethod2,Figure2-7.Asasecondalternative,ifadifferenceofnomorethan1%intheaveragevelocitymeasurementistobeintroduced,thetemperaturesensorneednotbeattachedtotheprobeorpitottube.  6.1.3.9Calibration/Field-PreparationRecord.Apermanentboundlaboratorynotebook,inwhichduplicatecopiesofdatamaybemadeastheyarebeingrecorded,isrequiredfordocumentingandrecordingcalibrationsandpreparationprocedures(i.e.,silicageltareweights,qualityassurance/qualitycontrolcheckresults,dry-gasmeter,andthermocouplecalibrations,etc.).Theduplicatecopiesshouldbedetachableandshouldbestoredseparatelyinthetestprogramarchives.  6.2SampleRecovery.Thefollowingitemsarerequiredforsamplerecovery:  6.2.1ProbeLiner.Probeandnozzlebrushes;TeflonbristlebrusheswithstainlesssteelwireorTeflonhandlesarerequired.Theprobebrushshallhaveextensionsconstructedofstainlesssteel,Teflon,orinertmaterialatleastaslongastheprobe.Thebrushesshallbeproperlysizedandshapedtobrushouttheprobelinerandtheprobenozzle.  6.2.2WashBottles.Three.Teflonorglasswashbottlesarerecommended;polyethylenewashbottlesshouldnotbeusedbecauseorganiccontaminantsmaybeextractedbyexposuretoorganicsolventsusedforsamplerecovery.  6.2.3GlassSampleStorageContainers.Chemicallyresistant,borosilicateamberglassbottles,500-mLor1,000-mL.Bottlesshouldbetintedtopreventtheactionoflightonthesample.Screw-caplinersshallbeeitherTeflonorconstructedtobeleak-freeandresistanttochemicalattackbyorganicrecoverysolvents.Narrow-mouthglassbottleshavebeenfoundto -(1 leaklessfrequently.  6.2.4GraduatedCylinderand/orBalances.Tomeasureimpingercontentstothenearest1mlor1g.Graduatedcylindersshallhavesubdivisionsnot>2mL.Laboratorybalancescapableofweighingto0.5gorbetterarerequired.  6.2.5PlasticStorageContainers.Screw-cappolypropyleneorpolyethylenecontainerstostoresilicagelandcharcoal.  6.2.6FunnelandRubberPoliceman.Toaidintransferofsilicagelorcharcoaltocontainer(notnecessaryifsilicagelisweighedinfield).  6.2.7Funnels.Glass,toaidinsamplerecovery.  6.3CrushedIce.Quantitiesrangingfrom10-50lbmaybenecessaryduringasamplingrun,dependingonambientairtemperature.  6.4StopcockGrease.Theuseofsiliconegreaseisnotpermitted.Siliconegreaseusageisnotnecessaryifscrew-onconnectorsandTeflonsleevesorground-glassjointsareused.  6.5SampleAnalysis.Thefollowingitemsarerequiredforsampleanalysis  6.5.1RotaryEvaporator.BuchiiModelEL-130orequivalent.  6.5.21000mlroundbottomflaskforusewitharotaryevaporator.  6.5.3SeparatoryFunnel.500mlorlarger,withTeflonStopcock.  6.5.4GlassFunnel.Shortstemmedorequivalent.  6.5.5Vials.15mlcapacitywithTeflonlinedcaps.  6.5.6ClassAVolumetricFlasks.10mlforbringingsamplestovolumeafterconcentration.  6.5.7FilterPaper.ScientificProductsGrade370Qualitativeorequivalent.  6.5.8BuchnerFunnel.Porcelainwith100mmIDorequivalent.  6.5.9ErlenmeyerFlask.500mlwithsidearmandvacuumsource.  6.5.10HPLCwithatleastabinarypumpingsystemcapableofaprogrammedgradient.  6.5.11Column.AlltechAltimaC18,250mmx4.6mmID,5mparticlesize(orequivalent).  6.5.12GuardColumn.AlltechHypersilODSC18,10mmx4.6mmID,5mparticlesize(orequivalent).  6.5.13UVdetectorat254nm.  6.5.14Datasystemformeasuringpeakareasandretentiontimes.7.0  ReagentsandStandards. T*%-   7.1SampleCollectionReagents.  7.1.1Charcoal.Activated,616mesh.Usedtoabsorbtoluenevaporsandpreventthemfromenteringthemetering -)1 device.Useoncewitheachtrainanddiscard.  7.1.2SilicaGel.Indicatingtype,6-16mesh.Ifpreviouslyused,dryat175$C(350$F)for2hoursbeforeusing. \ Newsilicagelmaybeusedasreceived.Alternatively,othertypesofdesiccants(equivalentorbetter)maybeused,subjecttotheapprovaloftheAdministrator.  7.1.3ImpingerSolution.Theimpingersolutionispreparedinthelaboratorybymixingaknownamountof1(2pyridyl)piperazine(purity99.5+%)intoluene(HPLCgradeorequivalent).Theactualconcentrationof1,2PPshouldbeapproximatelyfourtimestheamountneededtoensurethatthecapacityofthederivatizingsolutionisnotexceeded.Thisamountshallbecalculatedfromthestoichiometricrelationshipbetween1,2PPandtheisocyanateofinterestandpreliminaryinformationabouttheconcentrationoftheisocyanateinthestackemissions.Aconcentrationof130g/mlof1,2PPintoluenecanbeusedasareferencepoint.Thissolutionshouldbepreparedinthelaboratory,storedinarefrigeratedareaawayfromlight,andusedwithintendaysofpreparation.  7.2SampleRecoveryReagents.  7.2.1Toluene.Distilled-in-glassgradeisrequiredforsamplerecoveryandcleanup(see NOTE to7.2.2below). >   7.2.2Acetonitrile.Distilled-in-glassgradeisrequiredforsamplerecoveryandcleanup.  NOTE: Organicsolventsfrommetalcontainersmayhavea  highresidueblankandshouldnotbeused.Sometimessupplierstransfersolventsfrommetaltoglassbottles;thusblanksshallberunbeforefielduseandonlysolventswithalowblankvalue(<0.001%)shallbeused.  7.3Reagentgradechemicalsshouldbeusedinalltests.AllreagentsshallconformtothespecificationsoftheCommitteeonAnalyticalReagentsoftheAmericanChemicalSociety,wheresuchspecificationsareavailable.  7.3.1Toluene,C6H5CH3.HPLCGradeorequivalent. "^#   7.3.2Acetonitrile,CH3CN(ACN).HPLCGradeorequivalent. "4$   7.3.3MethyleneChloride,CH2CL2.HPLCGradeor # % equivalent.  7.3.4Hexane,C6H14.PesticideGradeorequivalent. f% '   7.3.5Water,H2O.HPLCGradeorequivalent. <&!(   7.3.6AmmoniumAcetate,CH3CO2NH4. 'b")   7.3.7AceticAcid(glacial),CH3CO2H. '8#*   7.3.81(2Pyridyl)piperazine,(1,2pp).Aldrich,99.5+%orequivalent.  7.3.9AbsorptionSolution.Prepareasolutionof1-(2-pyridyl)piperazineintolueneataconcentrationof40mg/300ml.Thissolutionisusedformethodblanksandmethodspikes.  7.3.10AmmoniumAcetateBufferSolution(AAB).Preparea -)1 solutionofammoniumacetateinwaterataconcentrationof0.1Mbytransferring7.705gofammoniumacetatetoa1000mlvolumetricflaskanddilutingtovolumewithHPLCGradewater.AdjustpHto6.2withglacialaceticacid.8.0  SampleCollection,Preservation,StorageandTransport. .   8.1Becauseofthecomplexityofthismethod,fieldpersonnelshouldbetrainedinandexperiencedwiththetestproceduresinordertoobtainreliableresults.  8.2PreliminaryFieldDeterminations.  8.2.1SelectthesamplingsiteandtheminimumnumberofsamplingpointsaccordingtoEPAMethod1orasspecifiedbytheAdministrator.Determinethestackpressure,temperature,andrangeofvelocityheadsusingEPAMethod2.Itisrecommendedthataleak-checkofthepitotlines(seepromulgatedEPAMethod2,Section3.1)beperformed.DeterminethestackgasmoisturecontentusingEPAApproximationMethod4oritsalternativestoestablishestimatesofisokineticsampling-ratesettings.Determinethestack-gasdrymolecularweight,asdescribedinpromulgatedEPAMethod2,Section3.6.IfintegratedEPAMethod3samplingisusedformolecularweightdetermination,theintegratedbagsampleshallbetakensimultaneouslywith,andforthesametotallengthoftimeas,thesamplerun.  8.2.2Selectanozzlesizebasedontherangeofvelocityheadssothatchangingthenozzlesizeinordertomaintainisokineticsamplingratesisnotnecessary.Duringtherun,donotchangethenozzle.Ensurethattheproperdifferentialpressuregaugeischosenfortherangeofvelocityheadsencountered(seeSection2.2ofpromulgatedEPAMethod2).  8.2.3Selectasuitableprobelinerandprobelengthsothatalltraversepointscanbesampled.Forlargestacks,toreducethelengthoftheprobe,considersamplingfromoppositesidesofthestack.  8.2.4Atypicalsamplevolumetobecollectedis1dscm(35.31dscf).Thesamplevolumecanbeadjustedasrequiredbyanalyticaldetectionlimitconstraintsand/orestimatedstackconcentrations.Amaximumlimitshouldbedeterminedtoavoidexceedingthecapacityofthereagent.  8.2.5Determinethetotallengthofsamplingtimeneededtoobtaintheidentifiedminimumvolumebycomparingtheanticipatedaveragesamplingratewiththevolumerequirement.AllocatethesametimetoalltraversepointsdefinedbyEPAMethod1.Toavoidtimekeepingerrors,thelengthoftimesampledateachtraversepointshouldbeanintegeroranintegerplusone-halfmin.  8.2.6Insomecircumstances(e.g.,batchcycles)samplingforshortertimesatthetraversepointsmaybenecessaryandtoobtainsmallergas-samplevolumes.Inthesecases,theAdministrator'sapprovalmustfirstbeobtained. -(1   8.3PreparationofSamplingTrain.  8.3.1Duringpreparationandassemblyofthesamplingtrain,keepallopeningswherecontaminationcanoccurcoveredwithTeflonfilmoraluminumfoiluntiljustbeforeassemblyoruntilsamplingisabouttobegin.  8.3.2Place300mloftheimpingerabsorbingsolutioninthefirstimpingerand200mleachinthesecondandthirdimpingers.Thefourthimpingershallremainempty.Thefifthandsixthimpingersshallhave400gofpreweighedcharcoaland200300gofsilicagel,respectively.  8.3.3Whenglassprobelinersareused,installtheselectednozzleusingaViton-AO-ringwhenstacktemperaturesare<260$C(500$F)andawovenglass-fibergasketwhen   temperaturesarehigher.SeeAPTD-0576(Rom,1972)fordetails.OtherconnectingsystemsusingTeflonferrulesmaybeused.Marktheprobewithheat-resistanttapeorbyanothermethodtodenotetheproperdistanceintothestackorductforeachsamplingpoint.  8.3.4SetupthetrainasshowninFigure2071.Duringassembly,donotuseanysiliconegreaseonground-glassjoints.Connectalltemperaturesensorstoanappropriatepotentiometer/displayunit.Checkalltemperaturesensorsatambienttemperature.  8.3.5Placecrushedicearoundtheimpingers.  8.3.6Turnonthecondensercoilcoolantrecirculatingpumpandbeginmonitoringthegasentrytemperature.Ensurepropergasentrytemperaturebeforeproceedingandagainbeforeanysamplingisinitiated.Itisimportantthatthegasentrytemperaturenotexceed50$C(122$F),thusreducingthelossof h toluenefromthefirstimpinger.  8.3.7Turnonandsettheprobeheatingsystemsatthedesiredoperatingtemperatures.Allowtimeforthetemperaturetostabilize.  8.4Leak-CheckProcedures.  8.4.1Pre-testleak-check.  8.4.1.1Becausetheadditionalconnectioninthetrain(overtheEPAMethod5Train)increasesthepossibilityofleakage,apre-testleak-checkisrequired.  8.4.1.2Afterthesamplingtrainhasbeenassembled,turnonandsettheprobeheatingsystemsatthedesiredoperatingtemperatures.Allowtimeforthetemperaturestostabilize.IfaVitonAO-ringorotherleak-freeconnectionisusedinassemblingtheprobenozzletotheprobeliner,leak-checkthetrainatthesamplingsitebypluggingthenozzleandpullinga381-mmHg(15-in.Hg)vacuum.Leakageratesgreaterthan4%oftheaveragesamplingrateor>0.00057m3/min(0.020cfm), N*%- whicheverisless,areunacceptable.  NOTE: Alowervacuummaybeused,ifitisnotexceeded , (0 duringthetest. -)1 Ї  8.4.1.3Thefollowingleak-checkinstructionsforthesamplingtraindescribedinAPTD-0576andAPTD-0581maybehelpful.Startthepumpwiththefine-adjustvalvefullyopenandthecoarse-adjustvalvecompletelyclosed.Partiallyopenthecoarse-adjustvalveandslowlyclosethefine-adjustvalveuntilthedesiredvacuumisreached.Donotreversedirectionofthe . fine-adjustvalve;thiswillcauseimpingercontentstobackupinthetrain.Ifthedesiredvacuumisexceeded,eitherleak-checkatthishighervacuumorendtheleak-check,asshownbelow,andstartover.  8.4.1.4Whentheleak-checkiscompleted,firstslowlyremovetheplugfromtheinlettotheprobe.Whenthevacuumdropsto127mm(5in.)Hgorless,immediatelyclosethecoarse-adjustvalve.Switchoffthepumpingsystemandreopenthefine-adjustvalve.Donotreopenthefine-adjustvalveuntilthecoarse-adjustvalvehasbeenclosed.Thispreventsthereagentintheimpingersfrombeingforcedbackwardintotheprobeandsilicagelfrombeingentrainedbackwardintothefifthimpinger.  8.4.2Leak-ChecksDuringSamplingRun.  8.4.2.1If,duringthesamplingrun,acomponentchangebecomesnecessary,aleak-checkshallbeconductedimmediatelyaftertheinterruptionofsamplingandbeforethechangeismade.Theleak-checkshallbedoneaccordingtotheprocedureoutlinedinParagraph8.4.1,exceptthatitshallbedoneatavacuumgreaterthanorequaltothemaximumvaluerecordeduptothatpointinthetest.Iftheleakagerateisnogreaterthan0.00057m3/min(0.020cfm)or4%oftheaveragesamplingrate B (whicheverisless),theresultsareacceptable,andnocorrectionwillneedtobeappliedtothetotalvolumeofdrygasmetered.Ifahigherleakagerateisobtained,thetestershallvoidthesamplingrun.  NOTE: Any"correction"ofthesamplevolumebycalculation F ! reducestheintegrityofthepollutantconcentrationdatageneratedandmustbeavoided.  8.4.2.2Immediatelyafteracomponentchange,andbeforesamplingisrestarted,aleak-checksimilartoapre-testleak-checkmustalsobeconducted.  8.4.3Post-TestLeak-Check.  8.4.3.1Aleak-checkofthesamplingtrainismandatoryattheconclusionofeachsamplingrun.Theleak-checkshallbeperformedwiththesameproceduresasthosewiththepre-testleak-check,exceptthatitshallbeconductedatavacuumgreaterthanorequaltothemaximumvaluereachedduringthesamplingrun.Iftheleakagerateisnogreaterthan0.00057m3/min 2+&. (0.020cfm)or4%oftheaveragesamplingrate(whicheverisless),theresultsareacceptable,andnocorrectionneedbeappliedtothetotalvolumeofdrygasmetered.If,however,a -)1 higherleakagerateisobtained,thetestershalleitherrecordtheleakagerate,correctthesamplevolume(asshowninSection6.3ofMethod5),andconsiderthedataobtainedofquestionablereliability,orvoidthesamplingrun.&    8.5Sampling-TrainOperation.  8.5.1During'tthesamplingrun,maintainanisokineticsamplingratetowithin10%oftrueisokinetic,unlessotherwisespecifiedbytheAdministrator.  8.5.2Foreachrun,recordthedatarequiredonadatasheetsuchastheoneshowninFigure2072.Besuretorecordtheinitialdry-gasmeterreading.Recordthedry-gasmeterreadingsatthebeginningandendofeachsamplingtimeincrement,whenchangesinflowratesaremadebeforeandaftereachleak-check,andwhensamplingishalted.TakeotherreadingsshownbyFigure2072atleastonceateachsamplepointduringeachtimeincrementandadditionalreadingswhensignificantchanges(20%variationinvelocity-headreadings)requireadditionaladjustmentsinflowrate.Levelandzerothemanometer.Becausethemanometerlevelandzeromaydriftduetovibrationsandtemperaturechanges,makeperiodicchecksduringthetraverse.  8.5.3Cleanthestackaccessportsbeforethetestruntoeliminatethechanceofcollectingdepositedmaterial.Tobeginsampling,verifythattheprobeheatingsystemisatthespecifiedtemperature,removethenozzlecap,andverifythatthepitottubeandprobeareproperlypositioned.Positionthenozzleatthefirsttraversepoint,withthetippointingdirectlyintothegasstream.Immediatelystartthepumpandadjusttheflowtoisokineticconditions.Nomographs,whichaidintherapidadjustmentoftheisokineticsamplingratewithoutexcessivecomputations,areavailable.ThesenomographsaredesignedforusewhentheTypeSpitot-tubecoefficientis0.840.02andthestack-gasequivalentdensity(drymolecularweight)isequalto294.APTD-0576detailstheprocedureforusingthenomographs.Ifthestack-gasmolecularweightandthepitot-tubecoefficientareoutsidetheaboveranges,donotusethenomographsunlessappropriatesteps(Shigehara,1974,inSection16.0,References)aretakentocompensateforthedeviations.  8.5.4Whenthestackisundersignificantnegativepressure(equivalenttotheheightoftheimpingerstem),takecaretoclosethecoarse-adjustvalvebeforeinsertingtheprobeintothestack,topreventtheimpingersolutionsfrombackingintotheprobe.Ifnecessary,thepumpmaybeturnedonwiththecoarse-adjustvalveclosed.  8.5.5Whentheprobeisinposition,blockofftheopeningsaroundtheprobeandstackaccessporttopreventunrepresentativedilutionofthegasstream.  8.5.6Traversethestackcrosssection,asrequiredbyEPAMethod1orasspecifiedbytheAdministrator,beingcarefulnottobumptheprobenozzleintothestackwallswhensamplingnear -(1 thewallsorwhenremovingorinsertingtheprobethroughtheaccessport,inordertoreducethechanceofextractingdepositedmaterial.  8.5.7Duringthetestrun,makeperiodicadjustmentstokeepthetemperatureofthecondenserattheproperlevels;addmoreiceand,ifnecessary,salttomaintainthetemperature.Also,periodicallycheckthelevelandzeroofthemanometer.  8.5.8Asingletrainshallbeusedfortheentiresamplerun,exceptincaseswheresimultaneoussamplingisrequiredintwoormoreseparateductsorattwoormoredifferentlocationswithinthesameduct,orincaseswhereequipmentfailurerequiresachangeoftrains.Inallothersituations,theuseoftwoormoretrainswillbesubjecttotheapprovaloftheAdministrator.  8.5.9Attheendofthesamplerun,closethecoarse-adjustvalve,removetheprobeandnozzlefromthestack,turnoffthepump,recordthefinaldry-gasmeterreading,andconductapost-testleak-check.Also,leak-checkthepitotlinesasdescribedinEPAMethod2.Thelinesmustpassthisleak-checkinordertovalidatethevelocity-headdata.  8.5.10Calculatepercentisokineticity(seeSection6.11ofMethod5)todeterminewhethertherunwasvalidoranothertestrunshouldbeperformed.  8.6SampleRecovery.  8.6.1Preparation.  8.6.1.1Propercleanupprocedurebeginsassoonastheprobeisremovedfromthestackattheendofthesamplingperiod.Allowtheprobetocool.Whentheprobecanbehandledsafely,wipeoffallexternalparticulatematternearthetipoftheprobenozzleandplaceacapoverthetiptopreventlosingorgainingparticulatematter.Donotcaptheprobetiptightlywhilethesamplingtrainiscoolingdownbecausethiswillcreateavacuuminthetrain.  8.6.1.2Beforemovingthesampletraintothecleanupsite,removetheprobefromthesampletrainandcaptheopenoutlet,beingcarefulnottoloseanycondensatethatmightbepresent.Captheimpingerinlet.Removetheumbilicalcordfromthelastimpingerandcaptheimpinger.  8.6.1.3Transfertheprobeandtheimpinger/condenserassemblytothecleanuparea.Thisareashouldbecleanandprotectedfromtheweathertoreducesamplecontaminationorloss.  8.6.1.4Saveaportionofallwashingsolutions(toluene/acetonitrile)usedforthecleanupasablank.Transfer200mlofeachsolutiondirectlyfromthewashbottlebeingusedandplaceeachinaseparate,prelabeledglasssamplecontainer.  8.6.1.5Inspectthetrainpriortoandduringdisassemblyandnoteanyabnormalconditions.  8.6.2SampleContainers.  8.6.2.1ContainerNo.1.Withtheaidofanassistant, -(1 rinsetheprobe/nozzlefirstwithtolueneandthenwithacetonitrilebytiltingandrotatingtheprobewhilesquirtingthesolventintotheupperendoftheprobesothatallofthesurfacesarewettedwithsolvent. Whenusingthesesolvents 2 insurethatproperventilationisavailable .Letthesolvent f drainintothecontainer.Ifparticulateisvisible,useaTeflonbrushtoloosen/removetheparticulateandfollowwithasecondrinseofeachsolvent.Afterweighingthecontentsofthefirstimpinger,addittocontainerNo.1alongwiththetolueneandacetonitrilerinsesoftheimpinger.(Acetonitrilewillalwaysbethefinalrinse.)Iftwoliquidlayersarepresentaddbothtothecontainer.Afterallcomponentshavebeencollectedinthecontainer,sealthecontainer,marktheliquidlevelonthebottleandaddtheproperlabel.  8.6.2.2ContainerNo.2.Afterweighingthecontentsofthesecond,thirdandfourthimpingers,addthemtocontainerNo.2alongwiththetolueneandacetonitrilerinsesoftheimpingers,thecondenserandallconnectingglassware.Afterallcomponentshavebeencollectedinthecontainer,sealthecontainer,marktheliquidlevelonthebottleandaddtheproperlabel.  8.6.3Thecontentsofthefifthandsixthimpingers(charcoalandsilicagel)canbediscardedaftertheyhavebeenweighed.  8.6.4SamplePreparationforShipment.Priortoshipment,recheckallsamplecontainerstoensurethatthecapsarewellsecured.SealthelidswithTeflontape.Shipallsamplesupright,packedinice,usingthepropershippingmaterialsasprescribedforhazardousmaterials.Thesamplesmustbestoredat4$Cbetweenthetimeofsamplingandconcentration.Each  Z sampleshouldbeextractedandconcentratedwithin30daysaftercollectionandanalyzedwithin30daysafterextraction.Theextractedsamplemustbestoredat4$C.   9.0  QualityControl. 8!"   9.1Sampling.SeeEPAManual600/477027bforMethod5qualitycontrol.  9.1.1FieldBlanks.Fieldblanksmustbesubmittedwiththesamplescollectedateachsamplingsite.Thefieldblanksincludethesamplebottlescontainingaliquotsofsamplerecoverysolvents,andimpingersolutions.Ataminimum,onecompletesamplingtrainwillbeassembledinthefieldstagingarea,takentothesamplingarea,andleak-checkedatthebeginningandendofthetesting(orforthesametotalnumberoftimesastheactualtesttrain).Theprobeoftheblanktrainshallbeheatedduringthesampletest.Thetrainwillberecoveredasifitwereanactualtestsample.Nogaseoussamplewillbepassedthroughthesamplingtrain.  9.1.2ReagentBlanks.Analiquotoftoluene,acetonitrile -)1 andtheimpingersolutionwillbecollectedinthefieldasseparatesamplesandreturnedtothelaboratoryforanalysistoevaluateartifactsthatmaybeobservedintheactualsamples.  9.2Analysis  9.2.1Thecorrelationcoefficientforthecalibrationcurvemustbe0.995orgreater.Ifthecorrelationcoefficientislessthan0.995,theHPLCsystemshouldbeexaminedforproblems,andanewcalibrationcurveshouldbepreparedandanalyzed.  9.2.2Asolventblankshouldbeanalyzeddailytoverifythatthesystemisnotcontaminated.  9.2.3Acalibrationstandardshouldbeanalyzedpriortoanysamplesbeinganalyzed,afterevery10injectionsandattheendofthesampleset.Samplesmustbebracketedbycalibrationstandardsthathavearesponsethatdoesnotvarybymorethan10%ofthetargetvalue.Ifthecalibrationstandardsareoutsidethelimit,thesamplesmustbereanalyzedafteritisverifiedthattheanalyticalsystemisincontrol.  9.2.4Amethodblankshouldbepreparedandanalyzedforevery10samplesconcentrated(Section11.4).  9.2.5Amethodspikeshouldbepreparedandanalyzedforevery20samples.Theresponseforeachanalyteshouldbewithin20%oftheexpectedtheoreticalvalueofthemethodspike(Section11.3).&  10.0  CalibrationandStandardization.    NOTE: Maintainalaboratorylogofallcalibrations. r   10.1ProbeNozzle.Probenozzlesshallbecalibratedbeforetheirinitialuseinthefield.Usingamicrometer,'͛measuretheinsidediameterofthenozzletothenearest0.025mm(0.001in.).Makemeasurementsatthreeseparateplacesacrossthediameterandobtaintheaverageofthemeasurements.Thedifferencebetweenthehighandlownumbersshallnotexceed0.1mm(0.004in.).Whennozzlesbecomenicked,dented,orcorroded,theyshallbereshaped,sharpened,andrecalibratedbeforeuse.Eachnozzleshallbepermanentlyanduniquelyidentified.  10.2PitotTubeAssembly.TheTypeSpitottubeassemblyshallbecalibratedaccordingtotheprocedureoutlinedinSection4ofpromulgatedEPAMethod2,orassignedanominalcoefficientof0.84ifitisnotvisiblynicked,dented,orcorrodedandifitmeetsdesignandintercomponentspacingspecifications.  10.3MeteringSystem.  10.3.1Beforeitsinitialuseinthefield,themeteringsystemshallbecalibratedaccordingtotheprocedureoutlinedinAPTD-0576.Insteadofphysicallyadjustingthedry-gasmeterdialreadingstocorrespondtothewet-testmeterreadings,calibrationfactorsmaybeusedtocorrectthegasmeterdialreadingsmathematicallytothepropervalues.Beforecalibrating - )1 themeteringsystem,itissuggestedthataleak-checkbeconducted.Formeteringsystemshavingdiaphragmpumps,thenormalleak-checkprocedurewillnotdetectleakageswithinthepump.Forthesecasesthefollowingleak-checkprocedureissuggested:Makea10-mincalibrationrunat0.00057m3/min(0.020 X cfm);attheendoftherun,takethedifferenceofthemeasuredwet-testanddry-gasmetervolumesanddividethedifferenceby10togettheleakrate.Theleakrateshouldnotexceed0.00057m3/min(0.020cfm). `    10.3.2Aftereachfielduse,thecalibrationofthemeteringsystemshallbecheckedbyperformingthreecalibrationrunsatasingleintermediateorificesetting(basedonthepreviousfieldtest).Thevacuumshallbesetatthemaximumvaluereachedduringthetestseries.Toadjustthevacuum,insertavalvebetweenthewet-testmeterandtheinletofthemeteringsystem.Calculatetheaveragevalueofthecalibrationfactor.Ifthecalibrationhaschangedbymorethan5%,recalibratethemeteroverthefullrangeoforificesettings,asoutlinedinAPTD-0576.  10.3.3Leak-checkofmeteringsystem.Thatportionofthesamplingtrainfromthepumptotheorificemeter(seeFigure2071)shouldbeleak-checkedpriortoinitialuseandaftereachshipment.Leakageafterthepumpwillresultinlessvolumebeingrecordedthanisactuallysampled.Closethemainvalveonthemeterbox.Insertaone-holerubberstopperwithrubbertubingattachedintotheorificeexhaustpipe.Disconnectandventthelowsideoftheorificemanometer.Closeoffthelowsideorificetap.Pressurizethesystemto13-18cm(5-7in.)watercolumnbyblowingintotherubbertubing.Pinchoffthetubingandobservethemanometerfor1min.Alossofpressureonthemanometerindicatesaleakinthemeterbox.Leaks,ifpresent,mustbecorrected.  NOTE: Ifthedry-gas-metercoefficientvaluesobtained F ! beforeandafteratestseriesdifferby>5%,eitherthetestseriesshallbevoidedorcalculationsfortestseriesshallbeperformedusingwhichevermetercoefficientvalue(i.e.,beforeorafter)givesthelowervalueoftotalsamplevolume.  10.4ProbeHeater.Theprobe-heatingsystemshallbecalibratedbeforeitsinitialuseinthefieldaccordingtotheprocedureoutlinedinAPTD-0576.ProbesconstructedaccordingtoAPTD-0581neednotbecalibratedifthecalibrationcurvesinAPTD-0576areused.  10.5TemperatureSensors.Eachthermocouplemustbepermanentlyanduniquelymarkedonthecasing;allmercury-in-glassreferencethermometersmustconformtoASTME-163specifications.Thermocouplesshouldbecalibratedinthelaboratorywithandwithouttheuseofextensionleads.Ifextensionleadsareusedinthefield,thethermocouplereadings -)1 atambientairtemperatures,withandwithouttheextensionlead,mustbenotedandrecorded.Correctionisnecessaryiftheuseofanextensionleadproducesachange>1.5%.  10.5.1Dry-gasmeterthermocouples.Forthethermocouplesusedtomeasurethetemperatureofthegasleavingtheimpingertrainthree-pointcalibrationatice-water,room-air,andboiling-watertemperaturesisnecessary.Acceptthethermocouplesonlyifthereadingsatallthreetemperaturesagreeto2$C(3.6$F)withthoseoftheabsolutevalueofthe `  referencethermometer.  10.5.2Probeandstackthermocouples.Forthethermocouplesusedtoindicatetheprobeandstacktemperatures,athree-pointcalibrationatice-water,boiling-water,andhot-oil-bathtemperaturesmustbeperformed;itisrecommendedthatroom-airtemperaturebeadded,andthatthethermometerandthethermocoupleagreetowithin1.5%ateachofthecalibrationpoints.Acalibrationcurve(equation)maybeconstructed(calculated)andthedataextrapolatedtocovertheentiretemperaturerangesuggestedbythemanufacturer.  10.6Barometer.Adjustthebarometerinitiallyandpriortoeachtestseriestoagreetowithin2.5mmHg(0.1in.Hg)ofthemercurybarometerorthecorrectedbarometricpressurevaluereportedbyanearbyNationalWeatherServiceStation(samealtitudeabovesealevel).  10.7Balance.Calibratethebalancebeforeeachtestseries,usingClass-Sstandardweights;theweightsmustbewithin0.5%ofthestandards,orthebalancemustbeadjustedtomeettheselimits.  10.8HighPerformanceLiquidChromatograph.EstablishtheretentiontimesforeachoftheisocyanatesofinterestusingthechromatographicconditionsprovidedinSection11.5.1.TheretentiontimesprovidedinTable11.5.11areprovidedasaguidetorelativeretentiontimes.Preparederivatizedcalibrationstandards(concentrationsexpressedintermsofthefreeisocyanate,Section12.4)accordingtotheprocedureinSection10.8.1.Calibratethechromatographicsystemusingtheexternalstandardtechnique(Section10.8.2)  10.8.1Preparationofcalibrationstandards.Preparea100g/mlstocksolutionoftheisocyanatesofinterestfromtheindividualisocyanateureaderivativeaspreparedinSections11.1.1and11.1.2.Thisisaccomplishedbydissolving1mgofeachisocyanateureaderivativein10mlofACN.CalibrationstandardsarepreparedfromthisstocksolutionbymakingappropriatedilutionsofaliquotsofthestockintoACN.Calibratetheinstrumentfrom1to20g/mlforHDI,TDIandMDI,andfrom1to80g/mlforMIusingatleastsixcalibrationpoints.  10.8.2Externalstandardcalibrationprocedure.AnalyzeeachderivatizedcalibrationstandardusingthechromatographicconditionslistedinSection11.5.1andtabulatepeakarea -(1 againstconcentrationinjected.Theworkingcalibrationcurvemustbeverifiedoneachworkingdaybythemeasurementofoneormorecalibrationstandards.Iftheresponseforanyanalytevariesfromthetargetresponsebymorethan10%,thetestmustberepeatedusingafreshcalibrationstandard(s)afteritisverifiedthattheanalyticalsystemisundercontrol.Alternatively,anewcalibrationcurvemaybepreparedforthatcompound.11.0  AnalyticalProcedure. 6   Ѐ11.1Preparationofisocyanatederivatives.  11.1.1HDI,TDI,MDI.  11.1.1.1Dissolve500mgofeachisocyanateinindividual100mlaliquotsofMeCl2,exceptMDIwhichrequires250mlof j  MeCl2.Transfera5mlaliquotof1,2pp(seeSection7.3.8)to @  eachsolution,stirandallowtostandovernightatroomtemperature.Transfer150mlaliquotsofhexanetoeachsolutiontoprecipitatetheisocyanateureaderivative.UsingaBuchnerfunnel,vacuumfilterthesolidisocyanateureaderivativeandwashwith50mlofhexane.DissolvetheprecipitateinaminimumaliquotofMeCl2.Repeatthehexaneprecipitationandfiltration D twice.Afterthethirdfiltration,drythecrystalsat50$Cand j transfertobottlesforstorage.Thecrystalsarestableforatleast21monthswhenstoredatroomtemperatureinaclosedcontainer.  11.1.2MI.  11.1.2.1 Topreparea200g/mlstocksolutionofmethyl H isocyanateurea,transfer60mgof1,2pptoa100mlvolumetricflaskcontaining50mlofMeCl2.Carefullytransfer20mgof D methylisocyanatetothevolumetricflaskandshakefor2minutes.DilutethesolutiontovolumewithMeCl2andtransfer  toabottleforstorage.Methylisocyanatedoesnotproduceasolidderivativeandstandardsmustbepreparedfromthisstocksolution.  11.2ConcentrationofSamples.  11.2.1Transfereachsampletoa1000mlroundbottomflask.Attachtheflasktoarotaryevaporatorandgentlyevaporatetodrynessundervacuumina65$Cwaterbath.Rinse z$& theroundbottomflaskthreetimeseachwithtwomlofACNandtransfertherinsetoa10mlvolumetricflask.DilutethesampletovolumewithACNandtransfertoa15mlvialandsealwithaTeflonlinedlid.Storethevialat4$Cuntilanalysis. '"#*   11.3PreparationofMethodSpikes.  11.3.1Prepareamethodspikeforeverytwentysamples.Transfer300mloftheabsorptionsolutiontoa1000mlroundbottomflask.Transfer1mlofa100g/mlstandardcontainingtheisocyanateureaderivativesofinterest.FollowtheprocedureoutlinedinSection11.2.1forsampleconcentration.Thiswillresultinamethodspikewithatheoretical -(1 concentrationof10g/ml.  11.4PreparationofMethodBlanks.  11.4.1Prepareamethodblankforeverytensamplesbytransferring300mloftheabsorptionsolutiontoa1000mlroundbottomflaskandconcentrateasoutlinedinSection11.2.1.  11.5ChromatographicAnalysis.0  11.5.1ChromatographicConditions. (#(#   Column:   0 h C18,250mmx4.6mmID,5mparticle `  size. h(#h(#   MobilePhase:  0 h Acetonitrile/AmmoniumAcetateBuffer. \ h(#h(#   Gradient:   0 h 10:90(v/v)ACN:AABto60:40(v/v)  2  ACN:AABover30minutes. h(#h(#   FlowRate:   h 2ml/min.     UVDetector:   h 254nm. d    InjectionVolume:0 h 50l.: h(#h(#   11.5.2Analysis.  11.5.2.1AnalyzesamplesbyHPLC,usingconditionsestablishedinSection11.5.1.  11.5.2.2Thewidthoftheretentiontimewindowusedtomakeidentificationsshouldbebaseduponmeasurementsofactualretentiontimevariationsofstandardsoverthecourseofaday.  Threetimesthestandarddeviationofaretentiontimeforacompoundcanbeusedtocalculateasuggestedwindowsize;however,theexperienceoftheanalystshouldweighheavilyintheinterpretationofthechromatograms.  11.5.2.3Ifthepeakareaexceedsthelinearrangeofthecalibrationcurve,thesampleshouldbedilutedwithACNandreanalyzed.12.0  DataAnalysisandCalculations.  ̀SameasinMethod5,Section6,withthefollowingadditions.  12.1PerformCalculations.Roundofffiguresafterthefinalcalculationtothecorrectnumberofsignificantfigures.  12.2Nomenclature.=.ԀSameasMethod5,Section6.1withthefollowingadditions:-,XX` XX-  ((` AS=0 Responseofthesample,areacounts.P% ' (# (#   ((` b=0 Yinterceptofthelinearregressionline,area &&v!( counts.  (# (#   ((` CI=0 Concentrationofaspecificisocyanatecompoundin '"#* thesample,g/ml.  (# (#   pp` M=0 Slopeofthelinearregressionline, ~)$, areacounts-ml/g.  (# (#   ((` mI=0 Massofisocyanateinthetotalsample.*+z&. (# (#   ((` VF=0 Finalvolumeofconcentratedsample,typically ,P'/ 10ml.  (# (#   ` ` `  Vm(std)=0 Volumeofgassamplemeasuredbythedry-gas -(1 meter,correctedtostandardconditions,dscm(dscf).  (# (# 12.3Conversionfromisocyanatetotheisocyanateureaderivative.Theequationforconvertingtheamountoffreeisocyanatetothecorrespondingamountofisocyanate-ureaderivativeisasfollows:?WXYWGCz (x p @Xdddd@E xgd x (#(#    (#(#Theequationforconvertingtheamountofisocyanateureaderivativetothecorrespondingamountoffreeisocyanateisasfollows:?stG\LHzx  ! p @Xdddd@Exgrdx (#(#    (#(#12.4Calculatethecorrelationcoefficient,slope,andinterceptsforthecalibrationdatausingtheleastsquaresmethodforlinearregression.Concentrationsareexpressedasthexvariableandresponseisexpressedasthey-variable.12.5Calculatetheconcentrationofisocyanateinthesample:?PSHRB>zx p @Xdddd@EBxdR9' Bx  (#(#    (#(#12.6Calculatethetotalamountcollectedinthesamplebymultiplyingtheconcentration(g/ml)timesthefinalvolumeofACN(10ml).?TUJRB>zx p @Xdddd@E!xnd]9m' !x+ (#(#   (#(#12.7Calculatetheconcentrationofisocyanate(g/dscm)inthestackgas.?CgNRB>zx p @Xdddd@E &x8dp9&'  &x (#(#     (#(#where:?DE\LHzx 0x p @Xdddd@E+xEd.}7+x  (#(#    -)1 13.0MethodPerformance.  13.1MethodPerformanceEvaluation.Evaluationofanalyticalproceduresforaselectedseriesofcompoundsmustincludethesample-preparationproceduresandeachassociatedanalyticaldetermination.Theanalyticalproceduresshouldbechallengedbythetestcompoundsspikedatappropriatelevelsandcarriedthroughtheprocedures.13.2MethodDetectionLimit.Theoverallmethoddetectionlimits(lowerandupper)mustbedeterminedonacompound-by-compoundbasisbecausedifferentcompoundsmayexhibitdifferentcollection,retention,andextractionefficienciesaswellastheinstrumentalminimumdetectionlimit(MDL).Themethoddetectionlimitmustbequotedrelativetoagivensamplevolume.Theupperlimitsforthemethodmustbedeterminedrelativetocompoundretentionvolumes(breakthrough).MethodDetectionLimitsmayvaryduetomatrixeffectsandinstrumentconditions.13.3MethodPrecisionandBias.Theoverallmethodprecisionandbiasmustbedeterminedonacompound-by-compoundbasisatagivenconcentrationlevel.Themethodprecisionvaluewouldincludeacombinedvariabilityduetosampling,samplepreparation,andinstrumentalanalysis.Themethodbiaswouldbedependentuponthecollection,retention,andextractionefficiencyofthetraincomponents.Fromevaluationstudiestodateusingadynamicspikingsystem,acceptablemethodbiases(perEPAMethod301)havebeendeterminedforallfourisocyanates.Aprecisionoflessthan10%relativestandarddeviation(RSD)hasbeencalculatedfromfieldtestdatasetswhichresultedfromaseriesofpaired,unspikedandspikedtrains.14.0PollutionPrevention.NotApplicable. R ! 15.0WasteManagement.NotApplicable. "T# 16.0References. #% 1.Martin,R.M.,ConstructionDetailsofIsokineticSource-SamplingEquipment,ResearchTrianglePark,NC,U.S.EnvironmentalProtectionAgency,April1971,PB-203060/BE,APTD-0581,35pp.2.Rom,J.J.,Maintenance,Calibration,andOperationofIsokineticSourceSamplingEquipment,ResearchTrianglePark,NC,U.S.EnvironmentalProtectionAgency,March1972,PB-209022/BE,APTD-0576,39pp.3.Schlickenrieder,L.M.,Adams,J.W.,andThrun,K.E.,ModifiedMethod5TrainandSourceAssessmentSamplingSystem:Operator'sManual,U.S.EnvironmentalProtectionAgency,EPA/600/8-85/003 -)1 (1985).4.Shigehara,R.T.,AdjustmentsintheEPANomographforDifferentPitotTubeCoefficientsandDryMolecularWeights,StackSamplingNews,2:4-11(October1974).5.U.S.EnvironmentalProtectionAgency,40CFRPart60,AppendixA,Methods1-5.6.Vollaro,R.F.,ASurveyofCommerciallyAvailableInstrumentationfortheMeasurementofLow-RangeGasVelocities,ResearchTrianglePark,NC,U.S.EnvironmentalProtectionAgency,EmissionsMeasurementBranch,November1976(unpublishedpaper).   2  17.0Tables,Diagrams,Flowcharts,and% ; ԀValidationData.  *mu ddXX nXX nXX XX 01(#(#,LL ,LL,LLe+  72& b L@7Table1  MolecularWeightoftheFreeIsocyanatesandtheIsocyanateUreaDerivative X3G/Z " L@  2 4L XAnalyte =3,! 3 =MW(FreeIsocyanate) =3,!  "3 =MW(Derivative) ND,  " L 4 3 $LN1,6HDI   N  168   N  494.44 6, N L $ $L62,4TDI  0  174.16  0  500.56 =3,0  L $ 4L =MDI   43#b 3 4250.25 43#b 3 4576.653)'b  L 4  3 3*Re ddLL LLLLemu(#(#,LL ,LL,LLe+  0& * |L0Table2 &v MolecularWeightofFreeMethylIsocyanateandMethylIsocyanateureaDerivative I238 "" L |  d| IAnalyte =23,!B23 =MW(FreeIsocyanate) =23,!&v"23 =MW(Derivative) U3D,&v " | d 23 4L UMI  43#v!3 457.1 43#v"3 4220.323)'v# L 4  3 3*yz ddLL LLLLeRe(#(#,LL ,LL+  32" >& L3Table3 :' RetentionTimesoftheFourIsocyanates X3G/6*" L0  2 $LXCompound =3,!F!+3 =RetentionTime(minutes) ND,*"z-" L $ 3 LNMI   j#. 10.0 6,j#/ L  L61,6HDI  $0 19.9 6,$1 L  L62,4TDI  % 2 27.1 92(% 3 L  DL9MDI 42#& "42 427.33)'& "5 L0 D  2 3  _  )$7 8-|}M=9z|  x * p @@@Ex0*x/*j)x +   #XeXXXhf0#