二氟甲烷磺酰氯的气相色谱分析方法研究

Study on Analysis Method of Difluoromethanesulphonyl Chloride by Gas Chromatography

建立了检测二氟甲烷磺酰氯含量的气相色谱分析法。DB-WAX气相色谱柱,氯苯为内标物,进行定性分析和定量分析。结果表明,该方法在0.615~15.36 g/L的浓度范围之内呈良好线性关系(r=0.999 82),相对标准偏差为0.39%,加标回收率在96.73%~104.37%之间。该方法简便、快速,具有良好的精密度和准确度,可用于合成样品中二氟甲烷磺酰氯含量的测定。

A gas chromatography method was established to detection the content of difluoromethanesulphonyl chloride.The method selected a DB-WAX gas chromatography column with chlorobenzene as the internal standard for qualitative and quantitative analysis.The results showed that this method had a good linear relation(r=0.99982)in a concentra-tion range from 0.615 g/L to 15.36 g/L with an average RSD of 0.39%and a recovery rate range from 96.73%to 104.37%.This method has been proved to be simple,rapid with good accuracy and reliability,which could be applica-ble in detecting of difluoromethanesulphonyl chloride in the samples taking from the preparation reaction.