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XX9% pP hx(#',81X9  H7FFXXdd7  METHOD7BDETERMINATIONOFNITROGENOXIDE Z EMISSIONSFROMSTATIONARYSOURCES(ULTRAVIOLETSPECTROPHOTOMETRICMETHOD)  "   *` P pP * ` NOTE: Thismethoddoesnotincludeallofthe   specifications(e.g.,equipmentandsupplies)andprocedures  V (e.g.,samplingandanalytical)essentialtoits t  performance.Somematerialisincorporatedbyreferencefromothermethodsinthispart.Therefore,toobtainreliableresults,personsusingthismethodshouldhaveathoroughknowledgeofatleastthefollowingadditionaltestmethods:Method1,Method5,andMethod7.1.0ScopeandApplication.    ` 1.1Analytes.*q,- ddd Xdd Xdd X(#(#q, dd ,dd ,pdd +  /." . p/Analyte ..!0. .CASNo. ..!0. .Sensitivity J//9!0 p . JNitrogenoxides(NOx), @ asNO2,including: |" 0 Nitricoxide(NO)  L L 0 Nitrogendioxide(NO2) <//+ "!  L L// <1010243910102440 2//!^#// 230786ppmv1'%@$    // 1 ` 1.2Applicability.ThismethodisapplicableforthedeterminationofNOxemissionsfromnitricacidplants. $`'  ` 1.3DataQualityObjectives.Adherencetotherequirementsofthismethodwillenhancethequalityofthedataobtainedfromairpollutantsamplingmethods.  +p%/ H2.0SummaryofMethod. Z  ` 2.1Agrabsampleiscollectedinanevacuatedflaskcontainingadilutesulfuricacidhydrogenperoxideabsorbingsolution;theNOx,excludingnitrousoxide(N2O),  @ aremeasuredbyultravioletspectrophotometry.3.0Definition.[Reserved] "  4.0Interferences.[Reserved]   5.0Safety. P   ` 5.1Thismethodmayinvolvehazardousmaterials,operations,andequipment.Thistestmethodmaynotaddressallofthesafetyproblemsassociatedwithitsuse.Itistheresponsibilityoftheuserofthistestmethodtoestablishappropriatesafetyandhealthpracticesandtodeterminetheapplicabilityofregulatorylimitationspriortoperformingthistestmethod. ` 5.2Corrosivereagents.Thefollowingreagentsarehazardous.Personalprotectiveequipmentandsafeproceduresareusefulinpreventingchemicalsplashes.Ifcontactoccurs,immediatelyflushwithcopiousamountsofwateratleast15minutes.Removeclothingundershoweranddecontaminate.Treatresidualchemicalburnasthermal burn. V+$*  ` 5.2.1HydrogenPeroxide(H2O2).Irritatingtoeyes, Z  skin,nose,andlungs. ` 5.2.2SodiumHydroxide(NaOH).Causesseveredamagetoeyesandskin.Inhalationcausesirritationtonose,throat,andlungs.Reactsexothermicallywithlimitedamountsofwater. ` 5.2.3SulfuricAcid(H2SO4).Rapidlydestructiveto   bodytissue.Willcausethirddegreeburns.Eyedamagemayresultinblindness.Inhalationmaybefatalfromspasmofthelarynx,usuallywithin30minutes.Maycauselungtissuedamagewithedema.3mg/m3willcauselungdamagein  uninitiated.1mg/m3for8hourswillcauselungdamageor, l inhigherconcentrations,death.Provideventilationtolimitinhalation.Reactsviolentlywithmetalsandorganics.6.0EquipmentandSupplies.  |  ` 6.1SampleCollection.SameasMethod7,Section6.1. ` 6.2SampleRecovery.Thefollowingitemsarerequiredforsamplerecovery: ` 6.2.1WashBottle.Polyethyleneorglass. ` 6.2.2VolumetricFlasks.100ml(oneforeach sample). b+%*  ` 6.3Analysis.Thefollowingitemsarerequiredfor analysis: ` 6.3.1VolumetricPipettes.5,10,15,and20mltomakestandardsandsampledilutions. ` 6.3.2VolumetricFlasks.1000and100mlforpreparingstandardsanddilutionofsamples. ` 6.3.3Spectrophotometer.Tomeasureultravioletabsorbanceat210nm. ` 6.3.4AnalyticalBalance.Tomeasuretowithin0.1mg.7.0ReagentsandStandards.   ` NOTE: Unlessotherwiseindicated,allreagentsareto l conformtothespecificationsestablishedbytheCommitteeonAnalyticalReagentsoftheAmericanChemicalSociety,wheresuchspecificationsareavailable.Otherwise,usethebestavailablegrade. ` 7.1SampleCollection.SameasMethod7,Section7.1.Itisimportantthattheamountofhydrogenperoxideintheabsorbingsolutionnotbeincreased.Higherconcentrationsofperoxidemayinterferewithsampleanalysis. ` 7.2SampleRecovery.SameasMethod7,Section7.2. ` 7.3Analysis.SameasMethod7,Sections7.3.1,7.3.3,and7.3.4,withtheadditionofthefollowing: 6-&,  ` 7.3.1WorkingStandardKNO3Solution.Dilute10mlof Z thestandardsolutionto1000mlwithwater.Onemilliliteroftheworkingstandardisequivalentto10gNO2.   8.0SampleCollection,Preservation,Storage,andTransport.  ^    ` 8.1SampleCollection.SameasMethod7,Section8.1.    ` 8.2SampleRecovery. ` 8.2.1Lettheflasksitforaminimumof16hours,andthenshakethecontentsfor2minutes. ` 8.2.2ConnecttheflasktoamercuryfilledUtubemanometer.Openthevalvefromtheflasktothemanometer,andrecordtheflasktemperature(Tf),thebarometric T pressure,andthedifferencebetweenthemercurylevelsinthemanometer.Theabsoluteinternalpressureintheflask(Pf)isthebarometricpressurelessthemanometerreading.   ` 8.2.3Transferthecontentsoftheflasktoaleakfreewashbottle.Rinsetheflaskthreetimeswith10mlportionsofwater,andaddtothebottle.Marktheheightoftheliquidlevelsothatthecontainercanbecheckedforleakageaftertransport.Labelthecontainertoidentifyclearlyitscontents.Sealthecontainerforshipping.9.0QualityControl. V+$*   2,%+ *q01 dd dd dd pdd ,-(#(#q,xdd ,Hdd ,`dd +  /." Z 8/ Section ..!. .QualityControlMeasure ..!. .Effect F/9! 8 . F10.1 7/*N / 7Spectrophometercalibration ./!0  / .Ensureslinearityofspectrophotometerresponsetostandards J/9!    / xJ11.4 ;/*l  / ;Auditsampleanalysis 2/!N / 2Evaluatesanalyticaltechniqueandpreparationofstandards1'%0 x   / 110.0CalibrationandStandardizations.    ` SameasMethod7,Sections10.2through10.5,withtheadditionofthefollowing: ` 10.1DeterminationofSpectrophotometerStandardCurve.Add0ml,5ml,10ml,15ml,and20mloftheKNO3  workingstandardsolution(1ml=10gNO2)toaseriesof x five100mlvolumetricflasks.Toeachflask,add5mlofabsorbingsolution.Dilutetothemarkwithwater.Theresultingsolutionscontain0.0,50,100,150,and200gNO2,respectively.Measuretheabsorbancebyultraviolet % spectrophotometryat210nm,usingtheblankasazeroreference.Prepareastandardcurveplottingabsorbancevs.gNO2.  .%+  ` NOTE: Ifotherthana20mlaliquotofsampleisused & - foranalysis,thentheamountofabsorbingsolutioninthe blankandstandardsmustbeadjustedsuchthatthesame ~*$$1 amountofabsorbingsolutionisintheblankandstandardsasisinthealiquotofsampleused.  ` 10.1.1Calculatethespectrophotometercalibrationfactorasfollows:6879QA=z  0X @Xdddddddd@Ej dw/@ _ j [   (#(#                (#(#   ` where:*P ` P *  Mi0 P =MassofNO2instandardi,g.>P (#P (#   Ai0 P =AbsorbanceofNO2standardi.P (#P (#   n0 P =Totalnumberofcalibrationstandards.lP (#P (#   10.1.2Forthesetofcalibrationstandardsspecifiedhere,Equation7B1simplifiestothefollowing:' ` P '6;:<QA=z  0X @Xdddddddd@E 7fd o@*_    (#(#           (#(#   ` 10.2SpectrophotometerCalibrationQualityControl.MultiplytheabsorbancevalueobtainedforeachstandardbytheKcfactor(reciprocaloftheleastsquaresslope)to '!& determinethedistanceeachcalibrationpointliesfromthetheoreticalcalibrationline.Thedifferencebetweenthecalculatedconcentrationvaluesandtheactual 2-&, concentrations(i.e.,50,100,150,and200gNO2)should Z belessthan7percentforallstandards.11.0AnalyticalProcedures.    ` 11.1SampleLossCheck.Notetheleveloftheliquidinthecontainer,andconfirmwhetheranysamplewaslostduringshipment.Notethisontheanalyticaldatasheet.Ifanoticeableamountofleakagehasoccurred,eithervoidthesampleorusemethods,subjecttotheapprovaloftheAdministrator,tocorrectthefinalresults. ` 11.2SamplePreparation.Immediatelypriortoanalysis,transferthecontentsoftheshippingcontainertoa100mlvolumetricflask,andrinsethecontainertwicewith5mlportionsofwater.Addtherinsewatertotheflask,anddilutetomarkwithwater. ` 11.3SampleAnalysis.Mixthecontentsoftheflaskthoroughlyandpipettea20mlaliquotofsampleintoa100mlvolumetricflask.Dilutetothemarkwithwater.Usingtheblankaszeroreference,readtheabsorbanceofthesampleat210nm. ` 11.4AuditSampleAnalysis.SameasMethod7,Section11.4,exceptthatasetofauditsamplesmustbeanalyzedwitheachsetofcompliancesamplesoronceperanalysisday,oronceperweekwhenaveragingcontinuoussamples. &-&, 12.0DataAnalysisandCalculations. Z  ` SameasMethod7,Section12.0,exceptreplaceSection12.3withthefollowing: ` 12.1TotalgNO2PerSample.  L @``0m=5KcAF hhR(#Eq.7B3  j   ` where: ` 5=0 100/20,thealiquotfactor.  (# (#   ` NOTE: Ifotherthana20mlaliquotisusedfor `  analysis,thefactor5mustbereplacedbyacorrespondingfactor.13.0MethodPerformance.    ` 13.1Range.Theanalyticalrangeofthemethodasoutlinedhasbeendeterminedtobe57to1500milligramsNOx 8 (asNO2)perdrystandardcubicmeter,or30to786parts V permillionbyvolume(ppmv)NOx.  14.0PollutionPrevention.[Reserved]   15.0WasteManagement.[Reserved] "H  16.0References. f$ "  ` 1.NationalInstituteforOccupationalSafetyandHealth.RecommendationsforOccupationalExposuretoNitricAcid.In:OccupationalSafetyandHealthReporter.Washington,D.C.BureauofNationalAffairs,Inc.1976.p.149. .-&,  ` 2.Rennie,P.J.,A.M.Sumner,andF.B.Basketter.DeterminationofNitrateinRaw,Potable,andWasteWatersbyUltravioletSpectrophotometry.Analyst.104:837.   September1979.17.0Tables,Diagrams,Flowcharts,andValidationData. j  [Reserved]