甲苯含量和杂质检测-ASTM-D6526-12中英文翻译

StandardTestMethodforAnalysisofToluenebyCapillaryColumnGasChromatography1（毛细柱）气相色谱法检测甲苯4.SummaryofTestMethod4.1Aportionofthesampleisinjectedintoagaschromatographusingamicrolitresyringeatthespecifiedconditionsofthetestmethod.Thetolueneandothercomponentsareseparatedastheyaretransportedthroughthecolumnbyaninertcarriergas.Thecomponentsintheeffluentaremeasuredbyaflameionizationdetector(FID).Theareaoftheimpuritypeaksandtolueneareelectronicallyintegrated.Thepeakareasarecorrectedwitheffectivecarbonnumber(ECN)4responsefactorsandnormalizedto100.0000%.4.检验方法综述4.1在检验方法中规定的适当条件下使用微量进样器注入气相色谱仪之中。使用惰性载气在色谱柱中分离甲苯和其他组分。这些组分流出后通过FID检测器可以进行测量。甲苯和杂质的峰面积采集整合后，峰面积通过ECN响应值调整归一化为100.0000%5.SignificanceandUse5.1Thistestmethodissuitablefordeterminingtheconcentrationsofknownimpuritiesinrefinedtolueneandforuseasanintegralqualitycontroltoolwheretolueneisproducedorusedinmanufacturing.5.2Toluenepurityisreported,butachromatographicanalysiscannotdetermineabsolutepurityifunknownorundetectedcomponentsarepresentinthesample.5.意义和应用5.1本试验方法适用于测定精制甲苯中已知杂质的浓度，作为生产或生产甲苯的整体质量控制工具。5.2甲苯纯度报告，但如果样品中存在未知或未检测到的成分，色谱分析不能确定绝对纯度。6.Interferences6.1Ifpresent,nonaromatichydrocarbonsof13carbonsorgreater,alcohols,ethers,andothersimilarorganiccompoundscaninterferewiththistestmethodbyco-elutingwiththearomatichydrocarbons.6.2CompoundsnotdetectedbyaFIDarenotdeterminedbythistestmethod.6.3Nonvolatilematerialisnotdetermined.6.干扰因素6.1如果存在13个碳或以上的非芳香烃，醇类、醚类和其他类似的有机化合物可以通过与芳香烃共洗脱来干扰本试验方法。6.2不能通过FID检测的组分无法用本检测方法检测6.3非挥发性物质不能用本方法检测7.Apparatus7.1GasChromatograph(GC)—anyGCbuiltforcapillarycolumnchromatography.Thesystemshallhavesufficientsensitivity,linearity,andrangetoobtainaminimumpeakheightresponsefor0.0010wt%impurityoftwicetheheightofthesignalbackgroundnoise,whilenotexceedingthefullscaleofeitherthedetectorortheelectronicintegrationforthemajorcomponent.Itshallhaveasplitinjectionsystemthatwillnotdiscriminateovertheboilingrangeofthesamplesanalyzed.ThesystemshouldbecapableofoperatingatconditionsgiveninTable1.7.仪器设备7.1气相色谱仪系统应该具有足够的灵敏度线性和检测范围，最小能检测杂质为0.0010%（该限度的杂质至少满足峰高是噪音的2倍）。主峰的峰高在仪器的检测范围内。任何沸点范围的化合物都可以使用仪器的分流进样系统。系统按照表一进行设定TABLE1TypicalInstrumentalParameters表一仪器参数Detector:Detectortemperature,°CColumn:TubingStationaryphaseFilmthickness,μmColumntemperature,°CCarrierGasLinearvelocityat70°C,Inlet:Injectionporttemperature,°CSplitratioSplitflow,mL/minSamplesize,μLFlameionization150°C50mby0.25mmFusedsilicaTCEP0.4070Heliumcm/s25Split150°C40551.0检测器检测器温度°C色谱柱管固定相膜厚度μm柱温°C载气70℃线速率进样进样口温度°C分流比分流流速mL/min样品量μLFID150°C50mby0.25mm熔融石英管TCEP0.4070Heliumcm/s25Split150°C40551.07.2Recorder—electronicintegrationisrecommended.7.3CapillaryColumn—fusedsilicacapillarycolumnwith1,2,3-tris-2-cyano-ethoxypropane(TCEP)phaseisrecommended.Polyethyleneglycol(PEG)columnshavebeensuccessfullyused.Othercolumnsmaybeusedafterithasbeenestablishedthatsuchacolumniscapableofseparatingallmajorimpuritiesunderoperatingconditionsappropriateforthecolumn.7.4Microsyringe—capableofdelivering1μLofsample.7.2记录仪7.3毛细管柱：TCEP固定相的石英柱或者PEG色谱柱。如果可以确认其他色谱柱在适当条件下能够分离主要杂质，也可以应用。7.4微量进样器：能够进1uL的样品。8.Reagents8.1PurityofReagents—Reagentgradechemicalsshallbeusedinalltests.ItisintendedthatallreagentsshallconformtothespecificationsoftheCommitteeonAnalyticalReagentsoftheAmericanChemicalSociety,5wheresuchspecificationsareavailable,unlessotherwiseindicated.Othergradesmaybeused,provideditisfirstascertainedthatthereagentisofsufficientlyhighpuritytopermititsusewithoutlesseningtheaccuracyofthedetermination.8.2CarrierGas—Helium,99.99mole%minimum,isrecommended.8.试剂8.1试剂纯度：试剂级别的化学品可以用于检测。除另有说明外，所有试剂均应符合ACS5的规范。如果使用其他等级的试剂，需要保证其纯度不会影响检测的准确度。8.2载气：高纯度氦气（99.99%）8.3FID检测器气体8.3.1氢气：99.99%以上8.3.2空气：总烃和水不超过10ppm8.3FIDDetectorGases:8.3.1Hydrogen—99.99mole%minimum.8.3.2Air—lessthan10ppmeachoftotalhydrocarbonsandwater.9.Hazards9.1ConsultcurrentOSHAregulations,suppliers’MaterialSafetyDataSheets,andlocalregulationsforallmaterialsusedinthistestmethod.9.风险9.1请参阅现行的OSHA法规、供应商的材料安全数据表以及涵盖本测试方法中使用的所有材料的当地法规。10.SampleHandling10.1CollectthesamplesinaccordancewithPracticeD3437.10.2Topreservesampleintegrity(consistency)andpreventthelossofvolatilecomponents,whichmaybeinsomesamples,donotuncoversamplesanylongerthannecessary.10.样品处理10.1按照D3437惯例采集样品。10.2为了保证样品检测完整有效，避免损失组分，检测时间应该足够长，保证所有组分均被检测。11.PreparationofApparatus11.1Followthemanufacturer’sinstructionsformountingandconditioningthecolumninthechromatograph.11.2AdjusttheinstrumenttotheconditionsasdescribedinTable1togivetheproperseparations.Allowsufficienttimefortheinstrumenttoreachequilibriumasindicatedbyastablebaseline.SeePracticesE355andE1510foradditionalinformationongaschromatographypracticesandterminology.11.仪器准备11.1依据生产说明书装配仪器，配置色谱条件。11.2按照表一进行仪器参数设定，预热平衡仪器至基线平稳。更多信息参见E355和E1510关于色谱方法和术语的记录。12.Procedure12.1Injectanappropriateamountofspecimen,typically1.0μL,intothechromatograph.Alowpuritytoluenesamplechromatogram,whichshowstherelativeretentiontimeofcomponentstypicallyfoundincommercialtoluene,isillustratedinFig.1.NOTE1—SinceTCEPisanonbondedphase,significantretentiontimeshiftscanoccurwithcolumncondition.12.2Measurethea