柱前衍生气相色谱法测定氯乙酰氯中二氯乙酰氯  

Determination of dichloroacetyl chloride in chloroacetyl chloride by gas chromatography with pre-column derivatization

作　　者：闫元春 冯云霞 马丹 YAN Yuanchun;FENG Yunxia;MA Dan(Zhengzhou Yuanli Biological Technology Co.,Ltd.,Zhengzhou 450000,China)

机构地区：[1]郑州原理生物科技有限公司,郑州450000

出　　处：《化学分析计量》2022年第7期9-12,共4页Chemical Analysis And Meterage

基　　金：郑州市重大科技创新专项(2020CXZX0074)。

摘　　要：建立柱前衍生气相色谱法测定氯乙酰氯中二氯乙酰氯的方法。以正丁醇为衍生试剂,在60℃水浴中对样品进行衍生处理30 min,溶液冷却后用氢氧化钠溶液滴定中和,取正丁醇层,以SE-30毛细管柱为色谱柱直接进样进行测定。二氯乙酰氯的质量浓度在0.8~2.4 mg/mL范围内与色谱峰峰面积线性关系良好,相关系数为0.9995,方法检出限为8.93μg/mL。样品测定结果的相对标准偏差为2.0%(n=6),加标回收率为103.29%~111.99%。该方法适用于氯乙酰氯中二氯乙酰氯含量的测定。A method for the determination of dichloroacetyl chloride in chloroacetyl chloride by pre-column derivatization gas chromatography was established.Took n-butanol as the derivatizing reagent,carried out derivatization treatment on the sample in 60℃water bath for 30 min.After being cooled,the solution was titrated and neutralized with sodium hydroxide solution.The solution of n-butanol layer was taken and injected directly,SE-30 capillary column as the chromatographic column for determination.The chromatographic peak area of dichloroacetyl chloride had a good linear relationship with the mass concentration in the range of 0.8–2.4 mg/mL,the correlation coefficient was 0.9995,and the detection limit of the method was 8.93μg/mL.The relative standard deviation of the determination results was 2.0%(n=6),and the recovery was 103.29%–111.99%.The method is suitable for the determination of dichloroacetyl chloride in chloroacetyl chloride.

关 键 词：气相色谱法 氯乙酰氯 二氯乙酰氯 柱前衍生 

分 类 号：O657.7[理学—分析化学]