摘要
利用GC-MS联用技术建立了快速检测Ziegler-Natta催化剂中内给电子体含量的分析方法,优化了前处理条件和仪器参数,建立了二醇酯类、邻苯二甲酸酯类、二醚类、单酯类等17种内给电子体的标准曲线.表征结果显示,对催化剂进行前处理时,适宜的溶剂为乙酸乙酯,提取方式为摇床振荡.最佳的色谱条件为：HP-5MSUI色谱柱,柱初温50℃,保持1 min,以10℃/min的速率升温至280℃,恒温5 min.17种内给电子体标准曲线的线性关系良好,相关系数大于0.998,利用标准曲线测试内给电子体含量时,低水平添加的回收率在85.91％ ～ 121.70％之间,高水平添加的回收率在86.08％～98.84％之间,相对标准偏差在1.02％～ 10.88％之间,显示了良好的准确性和重现性.该方法可应用于Ziegler-Natta催化剂中内给电子体含量的定性定量测试.
A GC-MS method for the quick determination of 17 internal electron donors in Zeigler- Natta catalysts was developed. The extraction conditions and instrument parameters were optimized and the calibration curves of the 17 internal electron donors were established. The investigation showed that the catalysts should be pretreated with ethyl acetate and shaking table oscillation. The optimal chroma- tographic conditions were as follows： HP-5MSUI chromatographic column, initial temperature 50 ℃ for 1 rain, 10℃/min temperature programmed to 280 ℃, and then constant temperature for 5 rain. The calibration curves of the 17 internal electron donors were in the linear range of 1 - 10 mg/L with the correlation coefficients（R2） more than 0. 998. The recoveries of the samples ranged from 85.91 % to 121.70% with the standard addition in the range of 5 -20 g/kg. All the relative standard deviations for the determination were between the 1.02% - 10. 88%, which indicated good accuracy and reproducibility.
出处
《石油化工》
CAS
CSCD
北大核心
2015年第4期511-516,共6页
Petrochemical Technology
