气相色谱-质谱联用法分析齐格勒-纳塔催化剂中的8种内给电子体

Determination methods of eight internal donors in ziegler-natta catalyst by gas chromatography-mass spectrometry

建立了齐格勒一纳塔催化剂中2－羟基苯甲酸乙酯、苯甲酸乙酯、邻苯二甲酸二异丁酯、邻苯二甲酸二丁酯、2－异丙基－2－异戊基－1，3－二甲氧基丙烷、2－氰基－2，3－二并丙基丁二酸二乙酯、2，4－戊二醇二苯甲酸酯和3，5－庚二醇二苯甲酸酯内给电子体的气相色谱－质谱联用分析方法。样品经水分散，乙酸乙酯萃取后，气相色谱一质谱法测定。8种内给电子体化合物含量在1～10mg／L范围内线性关系良好（R^2〉0．998），苯甲酸乙酯、邻苯二甲酸二丁酯、邻苯二甲酸二异丁酯检出限（S/N=3）为0．05g/kg，2一羟基苯甲酸乙酯、2一异丙基－2－异戊基－1，3－二甲氧基丙烷、2一氰基－2，3－二异丙基丁二酸二乙酯、2，4－戊二醇二苯甲酸酯、3，5－庚二醇二苯甲酸酯检出限（影Ⅳ=3）为0．1g/kg；添加水平为5g/kg的加标回收率为90．2％～120．9％，添加水平为20g／kg的加标回收率为92．0％～98．8％，相对标准偏差（RSD，n=3）小于11％。方法有效减小催化剂基质的干扰，为齐格勒一纳塔催化剂内给电子体的研发和产品质量控制提供科学数据。

A method was established for the determination of ethyl 2-hydroxybenzoate, ethyl benzoate, phthalmic acid diisobutyl ester, benzenedicarboxylic acid dibutyl ester, 2-iso propy 1-2-isopentyl-1,3-dimethoxypropane, dialkyl 2, 3-diisopropyl-2-cyanosuccinate, 2,4-pentadiol dibenzoate and 3,5-heptandiol dibenzoate internal donors in Zeigler-Natta catalysts by gas chromatography-mass spectrometry. The catalysts were dispersed in water, and shook up, then extracted with ethyl acetate. The sample was detected by gas chromatography-mass spectrometry under selected ion monitoring mode and external standard method. The calibration curves of eight internal electron donors were linear in the range of 1 - 10 mg/L with correlation coefficients （ R2 ） higher than 0. 9998. The limits of detection （ S/N = 3 ） were in the 0. 05 g/kg to 0. 1 g/kg levels. The recoveries of the samples ranged from 90.2% to 120.9% and 92.0% -98.8% , with the two standard addition levels of 5 g/kg and 20 g/kg. The relative standard deviations （RSD） of eight donors were below 10. 88%. This method was rapid, sensitive and simple for internal donors＇ research and provided scientific data for production quality control in Zeigler-Natta catalysts.