氢载气气质联用测定聚合级丙烯中微量磷烷和砷烷  

Determination of trace amount of phosphine and arsine in polymer grade propylene by GC-MS using hydrogen as carrier gas

作　　者：陈松[1] Chris Harvey 耿珂 王小伟 姜健准[1] Chen Song;Chris Harvey;Geng Ke;Wang Xiaowei;Jiang Jianzhun(Sinopec Beijing Research Institute of Chemical Industry,Beijing 100013,China;Peak Scientific InstrumentsShanghai Ltd.,Shanghai 201203,China;Beijing GASTK Analytical Technology Co.,Ltd.,Beijing 100012,China)

机构地区：[1]中国石化北京化工研究院,北京100013 [2]毕克气体仪器贸易(上海)有限公司,上海201203 [3]北京集思泰科分析技术有限公司,北京100012

出　　处：《石油化工》2022年第4期427-431,共5页Petrochemical Technology

基　　金：中国石油化工股份有限公司资助项目(CHG21009)。

摘　　要：以氢气为载气,采用闪蒸气化进样系统和动态气体稀释定量系统,建立了聚合级丙烯原料中微量磷烷、砷烷的气质联用分析方法。实验结果表明,当磷烷、砷烷含量在0.005~0.995 mL/m^(3)时,外标校正曲线相关系数为0.999,加标回收率在95.8%~103.8%之间,相对标准偏差小于4.0%,最低检出限小于0.010 mL/m^(3)。经实际试样检验,该方法可满足丙烯原料中磷烷、砷烷含量监测和分析要求。为聚合级丙烯原料中μL/m^(3)级别磷烷、砷烷的分析提供了一种低成本的分析方法。Trace amount of phosphine and arsine in polymer grade propylene has been determined by GC-MS using hydrogen as carrier gas with liquid evaporator and gas dynamic dilution system.The results show that the correlation coefficient of standard curve is 0.999,while the recoveries being around 95.8%-103.8%,the relative standard deviation being less than 4.0%and the determination limit being less than 0.010 mL/m^(3) when the condition of phosphine and arsine content in propylene ranges from 0.005-0.995 mL/m^(3).Several industrial propylene samples containing phosphine and arsine have been further analyzed to verify the method described above,of which the results indicate that this method has supplied a low cost solution for the determination and analysis of trace amount of phosphine and arsine in propylene even when the content is low toμL/m^(3) level.

关 键 词：氢气 丙烯 气质联用 磷烷 砷烷 

分 类 号：TQ221.21[化学工程—有机化工]