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《化学分析计量》 2022年第07期
DOI:10.3969/j.issn.1008-6145.2022.07.003
柱前衍生气相色谱法测定氯乙酰氯中二氯乙酰氯
闫元春,冯云霞,马丹
郑州原理生物科技有限公司,郑州 450000 
Determination of dichloroacetyl chloride in chloroacetyl chlorideby gas chromatography with pre-column derivatization
YAN Yuanchun, FENG Yunxia, MA Dan
Zhengzhou Yuanli Biological Technology Co., Ltd., Zhengzhou 450000, China 
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0.999 5,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。 
Abstract: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 coef ficient was 0.999 5, 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 
Keywords:gas chromatography; chloroacetyl chloride; dichloroacetyl chloride; pre-column derivatization 
基金:郑州市重大科技创新专项(2020CXZX0074) 
本文引用格式:
闫元春,冯云霞,马丹.柱前衍生气相色谱法测定氯乙酰氯中二氯乙酰氯[J].化学分析计量,2022,31(7):9.
YAN Yuanchun,FENG Yunxia,MA Dan. Determination of dichloroacetyl chloride in chloroacetyl chloride by gas chromatography with pre-column derivatization[J]. Chemical Analysis and Meterage,2022,31(7):9. 

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