微库仑法分析工业用乙烯和丙烯中的微量氯  

Analysis of Trace Chlorine in Ethylene and Propylene by Microcoulometry

作　　者：李思睿[1] 魏新宇[1] 张颖[1] 

机构地区：[1]中国石化北京化工研究院,北京100013

出　　处：《石油化工》2014年第6期703-706,共4页Petrochemical Technology

摘　　要：建立了一种测定工业用乙烯和丙烯中微量氯的微库仑法;优化了裂解炉温度、氩气(载气)流量、二次燃烧时氧气流量、气体进样速率和汽化装置等分析条件;考察了该方法的重复性和准确度,并确定了该方法的最低检出限。实验结果表明,微库仑法适宜的分析条件为:裂解炉温度1 050℃、氩气流量100 mL/min、二次燃烧时氧气流量100 mL/min、气体进样速率10 mL/min、汽化装置为闪蒸汽化装置。采用该方法分析乙烯和丙烯中的微量氯,回收率分别为109.34%,96.37%;试样重复测定5次的相对标准偏差分别为2.45%,0.35%;氯的最低检出限分别为0.59,0.46 mg/kg。该方法准确可靠,可满足工业用乙烯和丙烯产品中微量氯的测定。A microcoulometry for the analysis of trace chlorine in ethylene and propylene was established.The experimental conditions,including combustion oven temperature,flow rate of argon as carrier gas,flow rate of oxygen in the 2nd combustion,gas sample injection rate and vaporization device,were optimized.The accuracy and reproducibility of the method were verified and the detection limits of chloride in ethylene and propylene were determined.The experimental results showed that,under the optimal conditions of combustion oven temperature 1 050 ℃,flow rate of argon 100 mL/min,flow rate of oxygen in the 2nd combustion 100 mL/min,gas sample injection rate 10 mL/min and flash vaporization device,the recoveries of the chloride in ethylene and propylene were 109.37％ and 96.37％,the relative standard deviations were 2.45％ and 0.35％,and the limits of detection were 0.59 and 0.46 mg/kg,respectively.

关 键 词：微库仑法 微量氯 乙烯 丙烯 分析 

分 类 号：TQ207.4[化学工程—有机化工]