astm d7504-18 氣相色譜法和有效碳數(shù)測定單環(huán)芳烴中微量雜質(zhì)的標(biāo)準(zhǔn)試驗(yàn)方法

1、Designation:D7504?18StardTestMethodfTraceImpuritiesinMonocyclicAromaticHydrocarbonsbyGasChromatographyEffectiveCarbonNumber1ThisstardisissuedunderthefixeddesignationD7504thenumberimmediatelyfollowingthedesignationindicat

2、estheyearofiginaladoptioninthecaseofrevisiontheyearoflastrevision.Anumberinparenthesesindicatestheyearoflastreapproval.Asuperepsilon()indicatesaneditialchangesincethelastrevisionreapproval.1.Scope1.1Thistestmethodcoverst

3、hedeterminationoftotalnonaromatichydrocarbonsmonocyclicaromatichydrocarbonsinbenzenetolueneethylbenzenepxyleneoxylenestyrenemixedxylenesbygaschromatography.Thepurityofbenzenetolueneethylbenzenepxyleneoxylenestyrenemixedx

4、ylenesisalsocalculated.SimilartestmethodsusingtheinternalstardcalibrationtechniquetheexternalstardcalibrationtechniqueareTestMethodsD2360D3797D4492D5060D5135D5917D6563respectively.1.2Thelimitofdetection(LOD)is0.0002wt%li

5、mitofquantitation(LOQ)is0.0006wt%fimpuritiesintoluenemixedxylenespxyleneoxyleneethylbenzenebenzenestyrene.1.3Indeterminingtheconfmanceofthetestresultsusingthismethodtoapplicablespecificationsresultsshallberoundedoffinacc

6、dancewiththeroundingoffmethodofPracticeE29.1.4ThevaluesstatedinSIunitsaretoberegardedasstard.Nootherunitsofmeasurementareincludedinthisstard.1.5Thisstarddoesnotpurpttoaddressallofthesafetyconcernsifanyassociatedwithitsus

7、e.Itistheresponsibilityoftheuserofthisstardtoestablishappropriatesafetyhealthenvironmentalpracticesdeterminetheapplicabilityofregulatylimitationspritouse.1.6Thisinternationalstardwasdevelopedinaccdancewithinternationally

8、recognizedprinciplesonstardizationestablishedintheDecisiononPrinciplesftheDevelopmentofInternationalStardsGuidesRecommendationsissuedbytheWldTradeganizationTechnicalBarrierstoTrade(TBT)Committee.2.ReferencedDocuments2.1A

9、STMStards:2D841SpecificationfNitrationGradeTolueneD1555MTestMethodfCalculationofVolumeWeightofIndustrialAromaticHydrocarbonsCyclohexane[Metric]D2360TestMethodfTraceImpuritiesinMonocyclicAromaticHydrocarbonsbyGasChromatog

10、raphy(Withdrawn2016)3D3437PracticefSamplingHlingLiquidCyclicProductsD3797TestMethodfAnalysisofoXylenebyGasChromatography(Withdrawn2014)3D4492TestMethodfAnalysisofBenzenebyGasChromatography(Withdrawn2018)3D4790Terminology

11、ofAromaticHydrocarbonsRelatedChemicalsD5060TestMethodfDeterminingImpuritiesinHighPurityEthylbenzenebyGasChromatographyD5135TestMethodfAnalysisofStyrenebyCapillaryGasChromatographyD5136SpecificationfHighPuritypXyleneD5211

12、SpecificationfXylenesfpXyleneFeedstockD5917TestMethodfTraceImpuritiesinMonocyclicAromaticHydrocarbonsbyGasChromatographyExternalCalibrationD6229TestMethodfTraceBenzeneinHydrocarbonSolventsbyCapillaryGasChromatographyD656

13、3TestMethodfBenzeneTolueneXylene(BTX)ConcentratesAnalysisbyGasChromatography(Withdrawn2018)3D6809GuidefQualityControlQualityAssuranceProceduresfAromaticHydrocarbonsRelatedMaterialsE29PracticefUsingSignificantDigitsinTest

14、DatatoDetermineConfmancewithSpecifications1ThistestmethodisunderthejurisdictionofASTMCommitteeD16onAromaticIndustrialSpecialtyRelatedChemicalsisthedirectresponsibilityofSubcommitteeD16.01onBenzeneTolueneXylenesCyclohexan

15、eTheirDerivatives.CurrenteditionapprovedFeb.12018.PublishedMarch2018.iginallyapprovedin2009.Lastpreviouseditionapprovedin2017asD7504–17a.DOI:10.1520D750418.2FreferencedASTMstardsvisittheASTMwebsitewww.astm.gcontactASTMCu

16、stomerServiceat.FAnnualBookofASTMStardsvolumeinfmationrefertothestard’sDocumentSummarypageontheASTMwebsite.3Thelastapprovedversionofthishisticalstardisreferencedonwww.astm.g.ASummaryofChangessectionappearsattheendofthiss

17、tardCopyright?ASTMInternational100BarrHarbDrivePOBoxC700WestConshohockenPA194282959.UnitedStatesThisinternationalstardwasdevelopedinaccdancewithinternationallyrecognizedprinciplesonstardizationestablishedintheDecisiononP

18、rinciplesftheDevelopmentofInternationalStardsGuidesRecommendationsissuedbytheWldTradeganizationTechnicalBarrierstoTrade(TBT)Committee.18.2CarrierGasMakeupGasDetectGases99.999%Pure.Oxygenincarriergaslessthan1ppmlessthan0.

19、5ppmispreferred.Purifycarriermakeupdetectgasestoremoveoxygenwaterhydrocarbons.8.3AirftheFIDshouldcontainlessthan0.1ppmtotalhydrocarbon.8.4EquipmentSetupCheckSample8.4.1HighPuritypxylene(99.99wt.%greaterpurity)—Mostpxylen

20、eisavailablecommerciallyatapuritylessthan99.9wt.%butcanbepurifiedbyrecrystallization.Toprepare2Lofhighpuritypxylenebeginwithapproximately4Lofreagentgradepxylenecoolinanexplosionprooffreezeratbetween–10Cto10Cuntilapproxim

21、ately1?2to3?4ofthepxylenehasfrozen.Removethesampledecanttheliquidption.Allowthepxylenetothawrepeatthecrystallizationstepontheremainingsampleuntilthepxyleneisfreeofcontamination(nopeaksdetectedotherthanpxylene)asindicated

22、bygaschromatography.8.4.2Filla100mLvolumetricflaskapproximately3?4fullofthehighpuritypxylene.8.4.3Add0.1mLmxylene.8.4.4Add0.01mLoftolueneethylbenzenecumeneoxylenestyrenealphamethylstyrenephenylacetylene.8.4.5Add0.001mLbe

23、nzene14dioxane.8.4.6Dilutetovolumewithhighpuritypxylene.8.4.7Impuritiesthatarenotpresentinthesamplesbeinganalyzedmaybeomittedfromthechecksample.8.4.8Thepurposeofthesetupchecksampleistohelpdeterminetheretentiontimeoftheva

24、riouscomponentsthatthepxylenemxyleneareadequatelyseparated.Thissampleshouldnotbeusedfcalibration.9.Hazards9.1ConsultcurrentOSHAregulationssupplier’sSafetyDataSheetslocalregulationsfallmaterialsusedinthistestmethod.10.Sam

25、pling10.1SamplethematerialinaccdancewithPracticeD3437.11.PreparationofApparatus11.1Followmanufacturer’sinstructionsfmountingconditioningthecolumnintothechromatographadjustingtheinstrumenttotheconditionsdescribedinTable1a

26、llowingsufficienttimeftheequipmenttoreachequilibrium.SeePracticesE260E355E1510fadditionalinfmationongaschromatographypracticesterminology.12.Calibration12.1PritoimplementationoftheECNmethodalabatyshoulddemonstratethatthe

27、equipmentissetupproperlyusinganequipmentsetupchecksample.Thissampleshouldbeusedto:determineretentiontimesofeachcomponentthattheseparationofmxylenefrompxyleneissatisfacty.See6.1fthedefinitionofanadequateseparation.13.Proc

28、edure13.1Bringthesampletoroomtemperature.13.2Checkthechromatographyperfmancetomakesurethatthecolumnisproperlyresolvingpeaks.13.3Injectanappropriateamountofsampleintotheinstrument.13.4Reviewthechromatographicdatasystemres

29、ult.Measuretheareaofallpeaks.Thenonaromaticsfractionincludesallpeaksuptoethylbenzeneexceptfthepeaksassignedtobenzenetoluene.Sumtogetherallthenonaromaticpeaksasatotalarea.Wheneitherbenzenetolueneisanalyzed14dioxaneisrequi

30、redtobereptedthenonaromaticfractiondoesnotincludethepeakassignedto14dioxane.NOTE1—Apolyresolvedpeaksuchaspxylenefromhighpurityethylbenzenemxylenefromhighpuritypxylenewilloftenrequireatangentskimfromtheneighbingpeak.13.5S

31、eeFigs.18frepresentativechromatograms.14.CalculationInterpretationofResults14.1UsingtheECNweightcrectionfactslistedinTable2calculatetheconcentrationofeachcomponentasfollows:Ci51003~Ai3Ri!(i51n~Ai3Ri!(1)where:Ci=concentra

32、tionfcomponentiweight%Ai=peakareaofcomponentiRi=ECNcrectionfactfcomponenti.14.2CalculatethevolumepercentconcentrationofeachcomponentusingthedensityinTable2asfollows:TABLE2EffectiveCarbonNumberCrectionFactsDensityComponen

33、tECNCrectionFactADensityat20CNonAromatics1.00000.7255(average)BBenzene0.90950.8780CToluene0.91950.8658CEthylbenzene0.92710.8658Cpxylene0.92710.8597Cmxylene0.92710.8630Coxylene0.92710.8786CCumene0.93290.8605C14Dioxane3.07

34、741.0329DC9Aromatics0.93290.8715EaverageStyrene0.92100.9048CC10Aromatics0.93760.8694Eaveragepdiethylbenzene(PDEB)0.93760.8620EPhenylacetylene0.82960.9300FAlphamethylstyreneAMS0.92760.9077FACrectionfactsarerelativetonhept

35、ane.BDS#4APhysicalConstantsofHydrocarbonsC1throughC10ASTM1971.Averageofhexanemethylcyclopentanemethylcyclohexaneheptaneethylcyclopentane.CTestMethodD1555M.DKeithL.H.WaltersDB.CompendiumofSafetyDataSheetsfResearchIndustri