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1、Designation:D5443?14StardTestMethodfParaffinNaphtheneAromaticHydrocarbonTypeAnalysisinPetroleumDistillatesThrough200CbyMultiDimensionalGasChromatography1ThisstardisissuedunderthefixeddesignationD5443thenumberimmediatelyf

2、ollowingthedesignationindicatestheyearofiginaladoptioninthecaseofrevisiontheyearoflastrevision.Anumberinparenthesesindicatestheyearoflastreapproval.Asuperepsilon()indicatesaneditialchangesincethelastrevisionreapproval.1.

3、Scope1.1Thistestmethodcoversthedeterminationofparaffinsnaphthenesaromaticsbycarbonnumberinlowolefinichydrocarbonstreamshavingfinalboilingpointsof200Cless.Hydrocarbonswithboilingpointsgreaterthan200Clessthan270Carerepteda

4、sasinglegroup.Olefinsifpresentarehydrogenatedtheresultantsaturatesareincludedintheparaffinnaphthenedistribution.AromaticsboilingatC9abovearereptedasasinglearomaticgroup.1.2Thistestmethodisnotintendedtodetermineindividual

5、componentsexceptfbenzenetoluenethataretheonlyC6C7aromaticsrespectivelycyclopentanethatistheonlyC5naphthene.Thelowerlimitofdetectionfasinglehydrocarboncomponentgroupis0.05%bymass.1.3Thistestmethodisapplicabletohydrocarbon

6、mixturesincludingvirgincatalyticallyconvertedthermallyconvertedalkylatedblendednaphtha.1.4ThevaluesstatedinSIunitsaretoberegardedasstard.Nootherunitsofmeasurementareincludedinthisstard.1.4.1TheabbreviationfSIunit“coulomb

7、”is“C”.1.5Thisstarddoesnotpurpttoaddressallofthesafetyconcernsifanyassociatedwithitsuse.Itistheresponsibilityoftheuserofthisstardtoestablishappropriatesafetyhealthpracticesdeterminetheapplicabilityofregulatylimitationspr

8、itouse.SpecificprecautionarystatementsaregiveninSection7Table1.2.ReferencedDocuments2.1ASTMStards:2D4057PracticefManualSamplingofPetroleumPetroleumProductsD4307PracticefPreparationofLiquidBlendsfUseasAnalyticalStardsD513

9、4TestMethodfDetailedAnalysisofPetroleumNaphthasthroughnNonanebyCapillaryGasChromatographyD6839TestMethodfHydrocarbonTypesOxygenatedCompoundsBenzeneinSparkIgnitionEngineFuelsbyGasChromatography3.SummaryofTestMethod3.1Arep

10、resentativesampleisintroducedintoagaschromatographicsystemcontainingaseriesofcolumnsswitchingvalves.Asthesamplepassesthroughapolarcolumnthepolararomaticcompoundsbinaphtheneshighboiling(200C)paraffinsnaphthenesareretained

11、.Thefractionnotretainedelutestoaplatinumcolumnthathydrogenatesolefinsifpresentinthisfractionthentoamolecularsievecolumnwhichperfmsacarbonnumberseparationbasedonmolecularstructurethatisnaphthenesparaffins.Thefractionremai

12、ningonthepolarcolumnisfurtherdividedintothreeseparatefractionsthatarethenseparatedonanonpolarcolumnbyboilingpoint.Elutingcompoundsaredetectedbyaflameionizationdetect.3.2Themassconcentrationofeachgroupisdeterminedbythemul

13、tiplicationofdetectedpeakareasbyflameionizationdetectresponsefactsnmalizationto100%.3.3Thistestmethodprovideslimitedidentificationofindividualhydrocarboncomponents.TestMethodD5134maybeusedtoobtainspeciationofanumberofind

14、ividualcompounds.FsamplescontainingolefinsTestMethodD6839providescarbonnumberdistributionsofhydrocarbontypes(PIONA).4.SignificanceUse4.1Aknowledgeofthecompositionofhydrocarbonrefinerystreamsisusefulfprocesscontrolquality

15、assurance.4.2Aromaticsingasolinearesoontobelimitedbyfederalmate.Thistestmethodcanbeusedtoprovidesuchinfmation.1ThistestmethodisunderthejurisdictionofASTMCommitteeD02onPetroleumProductsLiquidFuelsLubricantsisthedirectresp

16、onsibilityofSubcommitteeD02.04.0LonGasChromatographyMethods.CurrenteditionapprovedJune152014.PublishedSeptember2014.iginallyapprovedin1993.Lastpreviouseditionapprovedin2009asD5443–04(2009)ε1.DOI:10.1520D544314.2Freferenc

17、edASTMstardsvisittheASTMwebsitewww.astm.gcontactASTMCustomerServiceat.FAnnualBookofASTMStardsvolumeinfmationrefertothestard’sDocumentSummarypageontheASTMwebsite.ASummaryofChangessectionappearsattheendofthisstardCopyright

18、?ASTMInternational100BarrHarbDrivePOBoxC700WestConshohockenPA194282959.UnitedStates17.Materials7.1CarrierGases—Fcarriergasesitisrecommendedtoinstallcommercialactiveoxygenscrubberswaterdryerssuchasmolecularsievesaheadofth

19、einstrumenttoprotectthesystem’schromatographiccolumns.Followsupplierinstructionsintheuseofsuchgaspurifiersreplaceasnecessary.7.1.1Hydrogen99.995%bymolminimumpurity0.1L?LH2O.(Warning—Extremelyflammablegasunderhighpressure

20、.)7.1.2Helium99.995%bymolminimumpurity0.1LLH2O.(Warning—Compressedgasunderhighpressure.)7.2DetectGases:7.2.1Hydrogen99.99%bymolminimumpurity.(Warning—Extremelyflammablegasunderhighpressure.)7.2.2Airlessthan10L?Leachoftot

21、alhydrocarbonswater.(Warning—Compressedgasunderhighpressure.)7.3ValveActuationGas—Thistestmethodpermitstheuseofanytypeofvalveswitchingvalveactuation.Whenpneumaticvalvesareusedairofanygradethatwillresultinnowatercondensat

22、ionwillnotintroduceoilothercontaminatesintheswitchingvalvesmaybeused.Airfromapistonoperatedcompressequippedwithawateroilseparathasbeenfoundsuitable.Columnswitchingvalvesthatdonotrequireairtooperatedonothavethisairrequire

23、ment.7.4Columns—FivecolumnsasdescribedinTable2.Thesecolumnspecificationsaretobeconsideredasguidelineshavebeenfoundtobeacceptable.Othermaterialscombinationsofmaterialsmayalsoprovideacceptableperfmance.Thesuitabilityofeach

24、columnisdeterminedbytestcriteriaasdefinedinSection8.NOTE2—Itisnottheintentionofthistestmethodtoincludedetailedcolumnpreparationsteps.Columnsmaybepreparedinanywaythatfollowsacceptedsafetypracticesresultsincolumnsthatwillm

25、eettheperfmancerequirementsofSection9.7.5Valves—Thistestmethodusesvalvesfcolumnswitchingflowswitching.Anycommerciallyavailablevalvesmaybeusedthatareintendedfadaptedfuseingaschromatographythatmeetthefollowingspecification

26、s:7.5.1Thecolumnswitchingvalvesaregenerallyinstalledinthegaschromatographoven.ThesevalvesmustbecapableofcontinuousoperationattheoperatingtemperatureoftheGCoven.7.5.2Materialsusedintheconstructionofthevalvesmustbeunreacti

27、vetohydrocarbonspresentinthesampleunderanalysisconditions.StainlesssteelPFAvespelmaterialshavebeenfoundsuitable.7.5.3Valvesmustbesizedsuchthattheyofferlittlerestrictiontocarriergasflowundertheanalysisconditionsdefinedint

28、histestmethod.7.5.4Caremustbetakentopreventtheintroductionofanyfmoffeignmaterialcontaminantintothevalvethatmayadverselyaffectitsperfmance.7.6HydrocarbonTestMixture—Aquantitativesyntheticmixtureofpurehydrocarbonsanexample

29、ofwhichisidentifiedinTable1isusedtotunetheinstrumentanalysisconditionsestablishthattheinstrumentisperfmingwithinspecifications.IndividualhydrocarboncomponentsinadditiontothoselistedinTable1maybeusedtoaidintheanalysis.The

30、concentrationlevelofeachcomponentinthehydrocarbontestmixtureisnotcriticalaslongastheconcentrationisaccuratelyknown.Percentagerangesfrom1.0%to6.0%bymasshavebeenfoundsuitable.Impuritiesintheindividualcomponentsmayhaveanadv

31、erseeffectonthequantitativeaspectoftheanalysis.Ifanimpurityisofthesamecarbonnumberbasicmolecularstructureasthemaincomponentitselfitwillbecrectlygroupedquantitatedwithinthegroup.Asanexampleisobutylcyclopentaneisopropylcyc

32、lohexanewillbothbedeterminedasC9naphthenes.Eachoftheindividualhydrocarboncomponentsusedfthistestmixturemusthaveaminimumpuritylevelof99%bymol.RefertoPracticeD4307finstructionsonthepreparationofliquidblendsfuseasanalytical

33、stards.7.7GasFlowsPressures:7.7.1CarrierGases:7.7.1.1Theheliumcarriergasthroughtheinjectionptpolarcolumnplatinumcolumnmolecularsievecolumnisflowcontrolled.Flowratesof16mLminto23mLminhavebeenfoundsuitable.Aheliumsupplypre

34、ssureof620kPa(90psi)hasbeenfoundsuitabletomeettheheliumflowrequirement.Theheliumcarriergasflowwillbereferredtoasthe“A”flowwithinthistestmethod.7.7.1.2Theheliumcarriergasusedasthemakeupgaswhenthepolarcolumnisinstopflowiss

35、ettothesameflowrateastheheliumcarriergasthroughtheinjectionpt.7.7.1.3ThehydrogencarriergasflowthroughtheTenaxcolumnnonpolarcolumnisflowcontrolled.FlowratesofTABLE2TypicalColumnSpecificationsSpecificationColumnTypePolarNo

36、nPolarTenax3MolsievePlatinumColumnlengthm340.16to0.181.80.002to0.06Columninsidediametermm2.0to2.11.8to2.02.51.6to2.01.6LiquidphaseOV275AOV101A.........Percentliquidphase304–5.........SupptmaterialChromasbBChromasbB......

37、...PAWWAW.........Packingmaterial......Tenax3Molecularsieve13XCD...Meshsize60808010080100......AOV101OV275areregisteredtrademarksofOhioValleySpecialtyChemicalCo.115IndustryRd.MariettaOH45750.BChromasbisaregisteredtradema

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