乙烯和丙烯中痕量砷烷和磷烷的测定

Determination of trace amount of arsine and phosphine in ethylene and propylene

通过联用气相色谱-原子发射光谱检测器开发了一种同时分析乙烯、丙烯产品中痕量砷烷和磷烷的方法,优化了色谱分析条件,考察了该方法的检测限、线性范围、加标回收率和重复性。结果表明,本方法对砷烷的检测限低至0.02 mL/m^(3),在砷烷的体积浓度为0.02~2090 mL/m^(3)时的相关性系数大于0.999,加标回收率为87.60%,3次平行测定结果的相对标准偏差为1.83%;对磷烷的检测限低至0.03 mL/m^(3),在磷烷的体积浓度为0.03~3010 mL/m^(3)时的相关性系数大于0.999,加标回收率为106.13%,3次平行测定结果的相对标准偏差为3.39%。本方法可以作为控制乙烯、丙烯产品中痕量砷烷和磷烷的分析方法。

A method was developed for the simultaneous analysis of trace arsine and phosphine in ethylene and propylene products by gas chromatography-atomic emission spectroscopy detector and the chromatographic analysis conditions were optimized,and the detection limit,linear range,recovery rate and repeatability of the method were investigated.The results showed that the detection limit of the method for arsine was as low as 0.02 mL/m3,the linear correlation coefficient was more than 0.999 in the volume concentration range of 0.02~2090 mL/m3,the recovery rate was 87.60%and the relative standard deviation of the 3 parallel measurements was 1.83%.The detection limit of phosphine was as low as 0.03 mL/m3,the correlation coefficient was greater than 0.999 in the volume concentration range of 0.03~3010 mL/m3,the recovery rate was 106.13%and the relative standard deviation of the 3 parallel measurements was 3.39%.The method can be used as a control analysis method for trace arsine and phosphine in ethylene and propylene products.