甲苯磺酸异构体的气相色谱分析

GAS CHROMATOGRAPHY OF ISOMERS OF TOLUENE SULFONIC ACID

为克服在甲苯磺酸异构体定量分析结果中重复性和准确性差的问题,从多种色谱固定液中选出合适固定液,以正二十一烷作为内标物,优化了色谱条件,对气相色谱法研究甲苯磺酸乙酯异构体中的诸多影响因素进行了比较,确定了汽化室温度对于邻、间、对甲苯磺酸乙酯异构体准确测定的影响作用。

Precision and accuracy of GC determination of isomers of toluene sulfonic acid was evidently improved by choosing a more feasible stationary liquid (QF-1) and using n-heneicosane as internal standard. Through study was made on the conditions of preparation of toluene sulfoinc acid under different temperatures, and on the method of quantitative analysis of ethyl esters of toluenesulfonic acid produced by its esterification. The chromatographic parameters, i.e. the flow-rate of carrying gas, the length of column, the column temperatare, the temperature of the vaporization chamber, the retention time and etc., were optimized. Under the optimum conditions, even the compound pair, m-TsOEt and p-TsOEt, which is hard to separate, can be effectively separated. The ratio of amount of ortho-, meta- and para- isomers produced in the sulfonation of toluene was characterized by the ratio of the amount of the corresponding isomers of ethyl esters of toluene sulfonic acid determined by the method proposed.