气相色谱法分析丙烯聚合催化剂中内给电子体的含量

Determination of Internal Electron Donors in Propylene polymerization Catalysts by GC Method

通过采用程序升温和梯度流量相结合的方式,建立了气相色谱快速分析丙烯聚合催化剂中二醚类、邻苯二甲酸酯类、二醇酯类等10种内给电子体定量分析方法。采用邻苯二甲酸二戊酯作为内标物,10种内给电子体的内标曲线的线性关系良好,相关系数大于0.9995,采用内标法测定内给电子体含量时,低水平添加回收率在94.40%~105.40%之间,高水平添加回收率在95.25%~103.67%,测定结果的相对标准偏差均小于3.0%,具有良好的精密度和准确度。

A GC method for the quick determination of 10 internal electron donors in Propylene polymerization catalysts was developed with programmable temperature and progressive flow. The extraction conditions and instrument parameters were optimized using dipentyl phthalate as internal standard and the calibration curves of the 10 internal electron donors were established. The investigation showed that The calibration curves of the 10 internal electron donors were with the correlation coefficients(R2) more than 0. 9995. The recoveries of the samples ranged from 94.40%~105.40% with the standard addition of 5mg and 95.25%~103.67% with the standard addition of 15mg. All the relative standard deviations for the determination were less than 3%,which indicated good accuracy and repro ducibility.