气相色谱法测定2-甲基-4-氯苯酚反应液中6种组分含量

Determination of six components in 2-methyl-4-ch lorophenol reaction solution by gas chromatography

采用气相色谱法测定2-甲基-4-氯苯酚反应液中6种组分的含量。通过优化色谱条件,样品中6种待测组分经TG 1701MS毛细管柱分离,使用氢火焰离子化检测器(FID)检测,以对甲酚为内标物,采用内标法定量,2-氯-6-甲基苯酚、邻甲酚(原料)、对甲酚(内标)、2,4-二氯-6-甲基苯酚、2-甲基-3-氯苯酚、2-甲基-4-氯苯酚(产物)、2-甲基-5-氯苯酚与相邻色谱峰分离较好,在测定浓度下有良好的线性关.系,线性相关系数r均大于0.999;方法的回收率为97%~105%,相对标准偏差RSD<3%,符合分析方法的要求。该分析方法操作简便、准确度高,可为2-甲基-4-氯苯酚的工艺优化和中控分析提供有效数据。

A gas chromatographic method was used to determine the contents of six components in the reaction solution of 2-methyl-4-chlorophenol.By optimizing the chromatographic conditions,the six components to be measured in the sample were separated by TG-1701MS capillary column and detected by hydrogen flame ionization detector(FID)and quantified by internal standard method with p-cresol as the internal standard substance.2-chloro-6-methylphenol,o-cresol(raw material),p-cresol(internal standard substance),2,4-dichloro-6-methylphenol,2-methyl-3-chlorophenol,2-methyl-4-chlorophenol(product),2-methyl-5-chlorophenol were well separated from adjacent chromatographic peaks,with good linearity at the measured concentrations and linear correlation coefficients r greater than 0.999;the recoveries of the method ranged from 97%to 105%with the relative standard deviations RSD<3%,which met the requirements of the analytical method.The analysis method is simple and accurate,and can provide effective data for process optimization and intermediate control analysis of 2-methyl-4-chlorophenol.