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#26610114α-H1Hα-H1H1H1Hα-Hα-H1%±0.22005-07-112005-11-18No.LS-04-KJZX-1411234KOH56α-H1Hα-H22.1AVANCE400400MHz5mmBBONPG16-16-HDA.RARCOSEGA.RBASF14-14-BDDDAA.RTPAIPAOPAnAdASeACDCl3DMSO-D6TMSC.P.SA.R33857280632.22.2.1100mL150～190℃102℃210～250℃10～16h2.2.211HNMRδ5δ6.53420065FENXIHUAXUEChineseJournalofAnalyticalChemistry5695～69821H1H60～80Hz1%1%13C1H11HFig.1Pulsesequenceofreversedgateddecouplingin1Hnuclearmagneticreso-nanceNMR13C13C1H1H13C11H3α-H1H15s15s1.5s2.2.3α-Hα-H7nOHmmol=0.5nStA∂-H/AStnOH%%OHAα-H1Hα-HASt1HnSt0.5OHα-HCH2%%OHVOH=56.11nOH/MsVOHKOHmg/gnOH%%OHMsg33.1α-H141Hα-HHOCH%%2%%RCH%%2%%%%%%OOCR'COOCH%%2%%RCH2%%n%%OH1#2#2#α-H1#CH22#CH211H1#2#Table1Chemicalshiftsofpeak1#andpeak2#in1HNMRSampleNo.Compositionδ1#10-6δ2#10-6SampleNo.Compositionδ1#10-6δ2#10-61Ethyleneglycol/terephthalicacidEG/TPA3.984.508EG/adipicacidAdA3.814.202EG/isophthalicacidIPA4.054.53914-butanedio14-BD/AdA3.684.093EG/o-phthalicaicdOPA3.834.341016-hexanediol16-HD/AdA3.644.074EG/14-cyclohexanediacidCHDA3.794.1711NeopentylglycolNPG/AdA3.464.035EG/sebacylicacidSeA3.824.2012NPG/CHDA3.303.886EG/succinicaicdSuA3.794.2513NPG/TPA3.474.207EG/dodecanedioicacidDDA3.814.2014NPG/IPA3.444.21α-Hα-H696343.23.2.121H21HTable2Hydroxylvalueresultsofseveralalkylalcoholby1HNMRmethodSampleSampleweightmgPeakareaofsampleInternalstandardweightmgPeakareaofinternalstandardMeasuredhydroxylvaluemg/gAveragevaluemg/gTheoreticalvaluemg/gRelativeerror%Neopentyleneglycol2.0661.000023.1162.80521074.22.8321.000022.9622.03551073.01.8741.000023.0783.08901073.91073.71079.00.51-Pentanol13.4941.000022.5620.7133631.413.3261.000022.6650.7260631.110.6591.000022.6320.9060631.3631.3636.50.81-Dodecanol16.5371.000022.6991.2341299.619.0591.000022.6161.0665299.714.3921.000022.5941.4115299.6299.6301.10.51-Octadecanol12.5631.000022.6872.3478207.210.9411.000022.6552.6933207.113.8321.000022.6732.1290207.4207.2207.40.11%3.2.23385728063331%3.3DIC543Table3QuantitativeresultsofpolyesterstandardsSampleNo.SampleweightmgPeakareaofsampleInternalstandardweightmgPeakareaofinternalstandardMeasuredhydroxylvaluemg/gAveragevaluemg/gTheoreticalvaluemg/gRelativeerror%3381.0801.000022.44416.904331.11.1641.000022.40515.679330.71.0921.000022.39216.696330.8330.9332.00.35721.7001.000022.40618.165195.51.6191.000022.51619.182195.31.5971.000022.47319.369195.7195.5196.20.48061.6391.000022.40626.607138.41.7191.000022.51625.494138.41.6971.000022.47325.812138.2138.3139.20.63.4Ⅲ6±0.2%79654Table4TheMeasuredresultsofpolyesterhydroxylvaluesbydifferentmethodsSampleNo.SampleweightmgPeakareaofsampleInternalstandardweightmgPeakareaofinternalstandardMeasuredhydroxylvaluemg/gAveragevaluemg/gResultsmeasuredbychemicalmethodKOHmg/gⅠ74.11.000022.30.4873166.472.01.000022.00.4924167.182.11.000022.10.4342166.9167168Ⅱ65.41.000022.60.950697.960.11.000022.41.029697.591.21.000022.20.667698.297.998.7Ⅲ69.41.000022.81.559456.870.11.000022.81.529857.375.11.000022.41.400657.457.258.6Ⅳ70.51.000022.23.674823.974.91.000022.23.369423.794.51.000022.42.647024.023.923.6V76.31.000022.46.757511.783.81.000022.15.824412.267.61.000022.37.467311.911.911.2References1ZhangZhixianZhangRuihao.QuantitativeAnalysisofOrganicFunctionalgroup.BeijingChemicalIndustryPress199065～712WuLichuanYuAifangChenLiban.GuangzhouChemistry200328246～523KranesALangeAEzrinM.PlasticsAnalysisGuide.NewYorkHanserPublishers1983136～1404HaslamJWillisHA.IdentificationandAnalysisofPlastics.LondonHeyden&Son1980234～2375FloydF-L.Anal.Chem.1973453603～6056KazuyukiYAkiraA.KokaiTokkyoKohoHP199711142～1497ChenZhaolianZengManling.HydroxylValueTestingofPolyesterPolyol.ChemicalIndustryStandardofthePeople'sRepublicofChina1996HG/T2709-95MeasurementofHydroxylValueforPolyesterby1HNuclearMagneticResonance-InternalStandardMethodWuAiqin#YuJingZhuangJianNingQiangQingdaoDinipponInkChemicalFineChemicalsCo.Ltd.Qingdao266101AbstractFourteenkindsofpolyestersweresynthesizedwhichistostudythecharacteristicsofterminalhydroxylα-Hofpolyesterin1HnuclearmagneticresonanceNMRspectra.Utilizingtheresultsthatthepeakofterminalhydroxylα-Hofpolyesterdoesnotinterferebyotherpeaksofpolyesteranewsimpleandsensitivemethodtodeterminethehydroxylvalueofpolyesterby1HNMRwasestablished.Inthismethodamodified1HNMRpulsesequenceandimprovedparameterswereadoptedandstyrenewasaddedastheinternalstandard.Theinvestigatedresultsshowthattherelativeerroroftheoreticavaluesandmeasuredvaluewinthismethodislowerthan1%andtheprecisionis±0.2.Thismethodischaracterizednotonlybysimplicityandrapiditybutalsobyhighprecision.KeywordsNuclearmagneticresonancepolyesterinternalstandardhydroxylvalueReceived11July2005accepted18November200589634