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使用GC-ICP-MS法快速测定乙烯中的痕量磷化氢
引用本文:宋阳,张颖,魏新宇,陈松,赵亚婷,李思睿,黄文氢. 使用GC-ICP-MS法快速测定乙烯中的痕量磷化氢[J]. 石化技术与应用, 2014, 0(4): 350-354
作者姓名:宋阳  张颖  魏新宇  陈松  赵亚婷  李思睿  黄文氢
作者单位:中国石油化工股份有限公司北京化工研究院,北京100013
摘    要:采用直接进样,研究了气相色谱(GC)的载气流量、分流比和电感耦合等离子体质谱(ICPMS)的积分时间、载气流量、RF功率对磷化氢分析灵敏度或信噪比的影响,建立了定量分析乙烯中痕量磷化氢的GC-ICP-MS方法。结果表明,GC-ICP-MS法能够有效地避免乙烯和乙烷对磷化氢分析的干扰,具有简单快速、数据稳定性好、准确度高等优点,样本数为8时相对标准偏差小于7%,加标回收率为94%~106%,磷化氢的检出限为17μL/m3,适用于乙烯中痕量磷化氢的定量分析。

关 键 词:乙烯  磷化氢  气相色谱  电感耦合等离子体质谱  GC-ICP-MS

Quick determination of trace phosphine in ethylene by gas chromatography-inductively coupled plasma-mass spectroscopy
Affiliation:SONG Yang,ZHANG Ying,WEI Xin- yu,CHEN Song,ZHAO Ya- ting,LI Si- rui,HUANG Wen- qing ( Beijing Research Institute of Chemical Industry, SINOPEC, Beijing 100013, China)
Abstract:A gas chromatography inductively coupled plasma mass (GC ICP MS) spectro scopic analysis method was established for quantita tively determining trace phosphine in ethylene. The effect of GC parameters, such as carrier gas flow rate, split ratio, and ICP MS parameters, such as carrier gas flow rate,integration time and RF power, on the sensitivity or signal noise ratio of phosphine determination was investigated. The results showed that GC ICP MS method effectively eliminatedthe interference of ethylene and ethane of phos phine,so that trace phoshine in ethylene was deter mined quickly ,correctly. The relative standard devi ation was less than 7% ( n = 8) , recovery was be tween 94% and 106% and lowest detective limit of phoshine in ethylene was 17 μL/m3.
Keywords:ethylene  phosphine  gas chromato-graphy  inductively coupled plasma- mass spectros-copy  GC - ICP - MS
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