ASTM D5008-22 氣相色譜法測(cè)定2-乙基己醇的乙基甲基戊醇含量和純度值的標(biāo)準(zhǔn)試驗(yàn)方法

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ThisinternationalstandardwasdevelopedinaccordancewithinternationallyrecognizedprinciplesonstandardizationestablishedintheDecisiononPrinciplesforthe

DevelopmentofInternationalStandards,GuidesandRecommendationsissuedbytheWorldTradeOrganizationTechnicalBarrierstoTrade(TBT)Committee.

Designation:D5008-22

StandardTestMethodfor

EthylMethylPentanolContentandPurityValueof2-EthylhexanolByGasChromatography1

ThisstandardisissuedunderthefixeddesignationD5008;thenumberimmediatelyfollowingthedesignationindicatestheyearoforiginaladoptionor,inthecaseofrevision,theyearoflastrevision.Anumberinparenthesesindicatestheyearoflastreapproval.Asuperscriptepsilon(e)indicatesaneditorialchangesincethelastrevisionorreapproval.

1.Scope

1.1Thistestmethodcoversthedeterminationofethylmethylpentanolcontentandpurityvalueof2-ethylhexanol.

1.2WaterandacidcannotbedeterminedbythistestmethodandmustbedeterminedinaccordancewithTestMethodsD1613andE203andthoseresultsusedtonormalizethechromatographicdata.

1.3Forpurposesofdeterminingconformanceofanob-servedoracalculatedvalueusingthistestmethodtorelevantspecifications,testresult(s)shallberoundedoff“tothenearestunit”inthelastright-handdigitusedinexpressingthespecificationlimit,inaccordancewiththerounding-offmethodofPracticeE29.

1.4ThevaluesstatedinSIunitsaretoberegardedasstandard.Nootherunitsofmeasurementareincludedinthisstandard.

1.5Forhazardinformationandguidance,seethesupplier'sMaterialSafetyDataSheet.

1.6Thisstandarddoesnotpurporttoaddressallofthesafetyconcerns,ifany,associatedwithitsuse.Itistheresponsibilityoftheuserofthisstandardtoestablishappro-priatesafety,health,andenvironmentalpracticesanddeter-minetheapplicabilityofregulatorylimitationspriortouse.Foraspecifichazardstatement,see6.1.1.

1.7Thisinternationalstandardwasdevelopedinaccor-dancewithinternationallyrecognizedprinciplesonstandard-izationestablishedintheDecisiononPrinciplesfortheDevelopmentofInternationalStandards,GuidesandRecom-mendationsissuedbytheWorldTradeOrganizationTechnicalBarrierstoTrade(TBT)Committee.

1ThistestmethodisunderthejurisdictionofASTMCommitteeD01onPaintandRelatedCoatings,Materials,andApplicationsandisthedirectresponsiblityof

SubcommitteeD01.35onSolvents,Plasticizers,andChemicalIntermediates.

CurrenteditionapprovedJan.1,2022.PublishedJanuary2022.Originallyapprovedin1989.Lastpreviouseditionapprovedin2012asD5008-07(2012)whichwaswithdrawnJanuary2021andreinstatedinJanuary2022.DOI:10.1520/D5008-22.

2.ReferencedDocuments

2.1ASTMStandards:2

D1613TestMethodforAcidityinVolatileSolventsand

ChemicalIntermediatesUsedinPaint,Varnish,Lacquer,

andRelatedProducts

E29PracticeforUsingSignificantDigitsinTestDatato

DetermineConformancewithSpecifications

E203TestMethodforWaterUsingVolumetricKarlFischer

Titration

3.SummaryofTestMethod

3.1Arepresentativespecimenisintroducedontoacapillarycolumn.The2-ethylhexanolisseparatedfromtheethylmethylpentanolandotherimpuritieswhilethecomponentsaretrans-portedthroughthecolumnbyaninertcarriergas.Theseparatedcomponentsaremeasuredintheeffluentbyaflameionizationdetectorandtheareasforthepeaksaredeterminedbyasuitableintegrationtechnique.Thedataareinterpretedbyapplyingcomponentdetectorresponsefactorstothepeakareas,andtherelativeconcentrationsaredeterminedbyrelat-ingtheindividualpeakresponsestothetotalpeakresponse.AcidityandwateraremeasuredbyTestMethodsD1613andE203,respectively,andtheresultsareusedtonormalizethevaluesobtainedbygaschromatography.Aninternalstandardprocedureisalsoincludedasanalternativecalculationtech-nique.Withthisprocedure,allimpuritiesaredeterminedrelativetotheinternalstandardandthepurityvalueisdeterminedbysubtractingthesumoftheimpurities,water,andacidfrom100.

4.SignificanceandUse

4.1Thistestmethodisusedtodeterminethepurityvalueandethylmethylpentanolcontentof2-ethylhexanol.

2ForreferencedASTMstandards,visittheASTMwebsite,

,or

contactASTMCustomerServiceatservice@ForAnnualBookofASTM

Standardsvolumeinformation

,

refer

tothestandard'sDocumentSummarypageontheASTMwebsite.

Copyright◎ASTMInternational,100BarrHarborDrive,POBoxC700,WestConshohocken,PA19428-2959.UnitedStates

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5.Apparatus

5.1Chromatograph—Anygaschromatographdesignedormodifiedforusewithcapillaryorwide-borecapillarycolumns.Thegaschromatographshouldbeequippedwithaflameionizationdetectororotherdetectorcapableofoperatingwiththesecolumnsandcapableofdetectingimpuritiesatalevelof

0.01weight%withasignaltonoiseratioofatleast5:1.

5.2Column—Anycolumncapableofresolving2-ethylhexanolfromethylmethylpentanolandotherimpuri-tiesthatmaybepresent.Thepeaksshouldberesolvedquantitativelywithinapracticalelapsedtime.ColumnsthatmeettherequirementofthistestmethodarelistedinTable1.Othercolumnsmaybeused,providedtheuserestablishesthatacolumngivestherequiredseparations.

5.3SpecimenIntroductionSystem—Anysystemcapableofintroducingarepresentativespecimenintothegaschromato-graphmaybeused.A1-μLsyringehasbeenusedsuccessfully.

5.4ComputingIntegrator—Anycomputingintegratorca-pableofaccuratelydeterminingthepeakareasgeneratedduringthisanalysis.

5.5AnalyticalBalance—Theinternalstandardtechniquerequiresananalyticalbalancecapableofmeasuring0.1mg.

6.ReagentsandMaterials

6.1CarrierGas—Helium,purifiednitrogen,orhydrogenaresuitable.Thecarriergasshouldhaveaminimumpurityof99.95mol%.

6.1.1Warning—Ifhydrogenisused,takespecialsafetyprecautionstoensurethatthechromatographicsystemisfreefromleaks.

6.2DetectorGases—Hydrogenandairareusedfortheflameionizationdetector.Ifamake-upgasisused,heliumornitrogenaresuitable.

6.3StandardsforCalibrationandIdentification—Standardsamplesforallidentifiablecomponentspresentareneededforidentificationbyretentiontime,andforcalibrationforquanti-tativemeasurements.Inthecaseoftheinternalstandardmethod,pure(99.0+%)2-ethyl-1-butanolisspecifiedastheinternalstandard.Anyotherinternalstandardmaybeusedprovideditisnotpresentinthesampleanddoesn'tinterferewithanyotherchromatographicpeakwiththecolumnused.

7.CalibrationandStandardization

7.1Identification—Selecttheconditionsofcolumn,columntemperatureandcarrier-gaslowthatwillgivethenecessarycomponentresolution(seeTable1).Determinetheretentiontimeforeachcomponentbyinjectingsmallamountsofthecompoundeitherseparatelyorinmixtures.

7.2Standardization—Theareaundereachpeakgeneratedisconsideredaquantitativemeasureofthecorrespondingcom-pound.Therelativeareaisproportionaltoconcentrationifthedetectorrespondsequallytoallthesamplecomponents.Theresponsetodifferentcomponentsisgenerallysignificantlydifferentforflameionizationdetectors.Thisdifferenceindetectorresponsemaybecorrectedbyuseofrelativeresponsefactorsobtainedbyinjectingandmeasuringtheresponseofknownblends.Usingpurematerials,prepareacalibrationmixturewitheachcomponentpresentintheappropriateamount.Ifaninternalstandardcalculationtechniqueisused,includetheinternalstandardinthiscalibrationmixture.Ifpurecomponentsarenotavailableandinterferingcomponentsare

TABLE1ConditionsandRetentionTimes

CaselCasell

Casell

Column:

Material

fusedsilica

fusedsilica

fusedsilica

Length,m

10

10

30

Insidediameter,mm

0.53

0.53

0.32

Liquidphase

immobilizedpolydimethylsiloxane

immobilizedpolydimethylsiloxane

immobilizedpolyethyleneglycol

Filmthickness,μm

5

5

0.25

Injectionsystem:

directflashvaporzation

directflashvaporizaion

split

Injectionspecimensize,μLTemperatures:

0.1

0.1

1

Columntemperature,℃(isothermal)

85

85

120

Injectionporttemperature,℃

200

200

220

Detectotemperature,℃

200

200

220

Gases:

Carriergas

helium

helium

helium

Carriergasflowrate,mL/min

4

4

0.6

Carriergasvelocity,cm/s

30

30

20

Hydrogenflowrate(detector),mmin

30

30

30

Airflowrate(detector),mL/min

300

300

300

Make-upgas

none

none

helium

Make-upflowrate(detector),mL/min

none

none

30

Injectionsplitratio

A

A

50:1

Calculationtechnique:

normalization

internalstandard

normalization

Typicalretentiontime,min:

2-ethyl-2-butanol(internalstandard)

A

2.24

A

Ethylmethylpentanol

5.75

5.75

5.74

2-ethylhexanol

7.76

7.76

7.24

ANotapplicable.

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present,thenappropriateadjustmentsmustbemadeincalcu-latingtheweightsofthecomponentspresent.

7.2.1ChromatographicConditions—UsingasuitablemethodselectedfromTable1,analyzearepresentativespeci-menofthecalibrationmixture.

7.2.2Ifacomputingintegratorisused,followthemanufac-turer'sinstructionmanualtocalculaterelativeresponsefactors.Ifmanualcalculationsareused,calculaterelativeresponsefactorsforeachcomponentasfollows:

R=(A×B)/(C×D)(1)

where:

R=responsefactorforcomponentofinterest,A=peakareaofreferencecomponent,

B=weightofcomponentofinterestincalibrationmixture,g,

C=peakareaforcomponentofinterestincalibrationmixture,and

D=weightofreferencecomponentincalibrationmixture,g.

NoTE1—Ifanormalizationcalculationtechniqueisused,2-ethylhexanolwillbethereferencecomponent.Ifaninternalstandardcalculationtechniqueisused,theinternalstandardwillbethereferencecomponent.

7.2.3Thecalibrationfactorgeneratedforethylmethylpentanolcanbeusedtocalculatetheconcentrationofanyunknownspresent.

8.Procedure

8.1NormalizationTechnique:

8.1.1Introducearepresentativespecimenintothechro-matograph.

8.1.2Usingthesameconditionsasforcalibrationandstandardization,determinetheareasforallpeaks.

8.2InternalStandardTechnique:

8.2.1Weigh0.1gofinternalstandardintoavial.Recordtheweighttothenearest0.1mg.

8.2.2Intothesamevial,weigh20.0gofarepresentativespecimen.Recordtheweighttothenearest0.1mg.Closethevialtightlyandmixwell.

8.2.3Introducearepresentativespecimenofthemixturein

8.2.2intothegaschromatograph.

8.2.4Usingthesameconditionsasforcalibrationandstandardization,determinetheareasforallpeaks.

9.Calculation

9.1NormalizationTechnique:

9.1.1Ifacomputingintegratorisused,followthemanufac-turer'sinstructionmanualtocomputethepercentofeachcomponentofinterest.

9.1.2Ifmanualcalculationsaremade,applytheappropriatedetectorresponsefactortoeachpeaktoobtainthecorrectedpeakresponse.Calculatetheweightpercent,W,ofeachcomponentofinterestasfollows:

W=(E/F)×(100-G)(2)

where:

E=correctedpeakresponseforcomponentofinterest,

F=sumofcorrectedpeakresponsesforallcomponents,

and

G=sumofwaterandacidasdeterminedbyTestMethodsD1613andE203.

9.2InternalStandardTechnique:

9.2.1Ifacomputingintegratorisused,followthemanufac-turer'sinstructionmanualtocomputethepercentofeachcomponentexceptthe2-ethylhexanol.

9.2.2Ifmanualcalculationsaremade,applytheappropriatedetectorresponsefactortoeachpeaktoobtainthecorrectedpeakresponse.CalculatetheweightpercentWofeachcomponent,exceptthe2-ethylhexanol,asfollows:

W=(H×1×100)/(J×K)(3)

where:

H=correctedpeakresponseforcomponentofinterest,I=weightofinternalstandardaddedtosample,g,

J=correctedpeakresponseforinternalstandard,andK=weightofsamplemixedwithinternalstandard,g.

9.2.3Calculatethepurityvalue,P,inweightpercentasshownbelow:

P=100-L(4)

where:

L=sumofwater,acid,andtheweightpercentofallcomponentsexcept2-ethylhexanol.

10.Report

10.1Reportthefollowinginformation:

10.1.1Theethylmethylpentanolcontenttothenearest

0.001weight%and

10.1.2Thepurityvaluetothenearest0.01weight%.

11.PrecisionandBias3

11.1Inaninterlaboratorystudyofthistestmethodinwhichoneoperatorintenlaboratoriestested2-ethylhexanolwithapurityvalueof99.653andwhichcontained0.203weight%ofethylmethylpentanol,thewithin-laboratorystandarddeviationandbetween-laboratorystandarddeviation,with9df,respectively,wereasfollows:

StandardDeviation,weight%

Within

Between

Laboratory

0.011

0.040

Ethylmethylpentanol2-Ethylhexanol

Laboratory

0.002

0.006

11.1.1Baseduponthesestandarddeviations,thefollowingcriteriashouldbeusedforjudgingtheacceptabilityofresultsatthe95%confidencelevel.

11.1.2Repeatability—Tworesults,eachthemeanofdupli-catesobtainedbythesameoperatorondifferentdays,shouldbeconsideredsuspectiftheydifferbymorethat0.02weight%absoluteforpurityvaluesor0.007weight%absoluteforethylmethylpentanol.

11.1.3Reproducibility—Tworesults,eachthemeanofdu-plicatesobtainedbyoperatorsindifferentlaboratories,shouldbeconsideredsuspectiftheydifferbymorethan0.13weight

3SupportingdatahavebeenfiledatASTMInternationalHeadquartersandmaybeobtainedbyrequestingResearchReportRR:D01-1118.ContactASTMCustomerServiceatservice@.

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%absoluteforpurityvaluesor0.036weight%absoluteforethylmethylpentanol.

11.2Bias—Thebiasofthistestmethodhasnotbeendeterminedbecauseasuitablereferencestandardisnotavail-abl