基于气相色谱-质谱联用的乙烯和丙烯中痕量砷烷和磷烷的测定方法  

Determination method of trace amount of arsine and phosphine in ethylene and propylene based on gas chromatography-mass spectrometry

作　　者：霍达 陈菲 来锦波 史得军 王春燕 曹青 HUO Da;CHEN Fei;LAI Jin-bo;SHI De-jun;WANG Chun-yan;CAO Qing(Analysis&Characterization Research Division,Petrochemical Research Institute,PetroChina,Beijing 102206,China;Process Engineering Research Division,Petrochemical Research Institute,PetroChina,Beijing 102206,China;Fundamental Science&Advanced Technology Research Division,Petrochemical Research Institute,PetroChina,Beijing 102206,China)

机构地区：[1]中国石油石油化工研究院分析表征研究所,北京102206 [2]中国石油石油化工研究院工艺工程研究所,北京102206 [3]中国石油石油化工研究院基础前沿技术研究所,北京102206

出　　处：《合成橡胶工业》2025年第1期29-33,共5页China Synthetic Rubber Industry

基　　金：国家重点研发计划项目(2022YFF0609700-2022YFF0609703)。

摘　　要：基于气相色谱-质谱联用开发了一种同时测定乙烯和丙烯中痕量砷烷和磷烷含量的测定方法,考察了此方法的检出限、线性范围、回收率和重复性。结果表明,此方法对砷烷的检出限可低至0.682μL/m3,在4.955~99.100μL/m3体积浓度范围内峰面积与体积浓度的相关性系数为0.9995,不同浓度样品检测值与实际值的差值均在7%内,3次测定结果的相对标准偏差为1.14%;此方法对磷烷的检出限可低至0.677μL/m3,在5.000~100.000μL/m3体积浓度范围内峰面积与体积浓度的相关性系数为0.9997,不同浓度样品检测值与实际值的差值均在10%内,3次测定结果的相对标准偏差为1.20%。本方法所用色谱柱系统简单、检出限低,测定过程方便快捷,可为聚合级乙烯和丙烯单体的质量监控提供新的分析手段。A method for simultaneous determination of trace amount of arsine and phosphine in ethylene and propylene was developed based on gas chromatography-mass spectrometry,and the limit of detection,linear range,recovery rate and repeatabi-lity of the method were investigated.The results showed that the limit of detection of this method for arsine could be as low as 0.682μL/m3 and the correlation coefficient between peak area and volume concentration was 0.9995 within the volume concentration range of 4.955-99.100μL/m3,the deviations between the test value and the actual value of samples with different concentrations were all within 7%and the relative standard deviation of the three measurement results was 1.14%.The limit of detection of this method for phosphine could be as low as 0.677μL/m3 and the correlation coefficient between peak area and volume concentration was 0.9997 within the volume concentration range of 5.000-100.000μL/m3,the deviations between the test value and the actual value of samples with different concentrations were all within 10%and the relative standard deviation of the three measurement results was 1.20%.The chromatographic column system used in this method was simple,the limit of detection was low and the determination process was convenient and fast,and this method could provide a new analytical means for the quality monitoring of polymerization-grade ethylene and propylene monomers.

关 键 词：乙烯 丙烯 痕量 砷烷 磷烷 气相色谱-质谱联用 检出限 

分 类 号：TQ330.3[化学工程—橡胶工业]