2023,32(1)福建分析测试FujianAnalysis&Testing电子制冷预浓缩-热解析-气相色谱质谱法测定废气中乙酸甲酯陈浩(漳州市古雷环境监测站,福建漳州363401)收稿日期:2022-10-13作者简介:陈浩(1989—),男,工程师,从事环境监测工作,Email:415087203@qq.com摘要:建立了气袋采样、电子制冷预浓缩-热解析-气相色谱质谱法测定废气中乙酸甲酯的方法。本方法用具有高度化学惰性的氟聚合物薄膜气袋采集固定源废气中的样品,样品经预浓缩系统冷冻浓缩、热解析后,进入气相色谱进行分离,根据保留时间、质谱特征离子定性,用质谱检测器检测,内标法定量测定废气中乙酸甲酯。实验进样体积为200mL时,检出限为0.1nmol/mol,实验标准曲线相关系数在0.99以上;精密度范围在7%以内,加标回收率范围在85.4%—105%。关键词:乙酸甲酯;电子制冷浓缩;热解析;气相色谱质谱中图分类号:O657.71文献标识码:A文章编号:1009-8143(2023)01-0045-04Doi:10.3969/j.issn.1009-8143.2023.01.09DeterminationofMethylAcetateinWasteGasbyMeansofElectronicRefrigerationPreconcentration-ThermalAnalysis-GasChromatography-massSpectrometry1ChenHao(ZhangzhouGulaiEnvironmentalMonitoringStation,Gulei,Fujian363215,China)Abstract:Amethodofgasbagsampling,electronicrefrigerationpreconcentration-thermalanalysis-gaschromatography-massspectrometrywasworkedoutinthispapertodeterminemethylacetateinwastegas.Bythismethod,samplesfromsta⁃tionarysourcewastegasarecollectedwithfluoropolymerfilmgasbagscharacterizedbyhighchemicalinertness.Afterthesamplesarefrozenandconcentratedthroughpre-concentrationsystemandthermallyanalyzed,theywillbeseparatedingaschromatography.Inviewofretentiontimeandcharacteristicionsofmassspectrometry,theyaredetectedbymassspectrom⁃etrydetector,andmethylacetateinwastegasisquantitativelydeterminedbyinternalstandardmethod.Whentheinjectionvolumeoftheexperimentwas200mL,thedetectionlimitwas0.1nmol/mol,andthecorrelationcoefficientofthestandardcurveoftheexperimentwasabove0.99.Theprecisioniswithintherangeof7%,andtheaddingstandardrecoveryrangesfrom85.4%to105%.Keywords:MethylAcetate;ElectronicRefrigerationConcentration;ThermalAnalysis;GasChromatography...