丙烯中微量丙二烯及甲基乙炔的测定方法优化

Optimization of determination method of trace propylene diene and methyl acetylene in propylene

本文通过选择适宜的色谱柱、柱温、载气流量、进样量等条件,实现了碳一到碳六19个烃类组分的良好分离,并使丙二烯、甲基乙炔的检出限达到了0.01mL/m~3,完全满足了茂金属催化剂体系对丙烯原料杂质监控的技术要求,弥补了丙烯国家标准中无法检测10级别杂质的空白。通过对标准样品的多次重复测定,其相对标准偏差小于10%,精密度良好,回收率在100%-112%之间,测定结果准确可靠。该方法操作简单、分析快速、检出限低,能够有效地为茂金属聚丙烯装置提供丙烯原料组成分析的监控手段。

In this paper, by selecting suitable chromatographic column, column temperature, carrier gas flow,sample volume and other conditions, the good separation of 19 hydrocarbon components from carbon one to carbon six was achieved, and the detection limit of propylene and methyl acetylene reached 0.01mL/m3, which fully met the technical requirements of metal locene catalyst system for the monitoring of propylene raw material impurities. It makes up for the blank of 10-9 impurity level which cannot be detected in propylene national standard. The RSD is less than 10% and the recovery rate is between 100% and 112%. The results are accurate and reliable. The method is simple in operation, rapid in analysis and low in detection limit. It can effectively provide a monitoring method for the composition analysis of propylene raw materials in metallocene polypropylene plant.