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目的对饮用水中卤乙酸的衍生-气相色谱测定法进行改进。方法对5种卤乙酸(一氯乙酸、一溴乙酸、二氯乙酸、三氯乙酸和二溴乙酸)的衍生-气相色谱测定法的前处理条件(五水硫酸铜及衍生化试剂酸化甲醇、硫酸钠水溶液、甲基叔丁基醚、饱和碳酸氢钠溶液加入量)进行改进,测定其对卤乙酸回收率的影响。结果优化实验方法后,在0.3～200.0μg/L线性范围内,5种卤乙酸的回归方程相关系数均在0.99以上,加标回收率为90.0%~103.2%,相对标准偏差为0.42%~2.76%,检出限分别为0.65、0.50、0.50、0.30、0.30μg/L。结论该方法具有较好的准确性、精密度和灵敏度,适用于饮用水中卤乙酸的测定。
Objective To improve the determination of haloacetic acid in drinking water by gas chromatography. Methods The derivatization of 5 haloacetic acids (monochloroacetic acid, monobromoacetic acid, dichloroacetic acid, trichloroacetic acid and dibromoacetic acid), the pretreatment conditions of GC (copper sulfate pentahydrate and derivatization reagent to acidify methanol, Sodium sulfate aqueous solution, methyl t-butyl ether, and saturated sodium bicarbonate solution) to improve the recovery of haloacetic acid. Results After the optimization of the experimental method, the correlation coefficients of the five haloacetic acids in the linear range of 0.3 ~ 200.0μg / L were all above 0.99 with the recoveries of 90.0% ~ 103.2% and the relative standard deviations of 0.42% ~ 2.76 %, The detection limits were 0.65,0.50,0.50,0.30,0.30μg / L. Conclusion The method has good accuracy, precision and sensitivity, and is suitable for the determination of haloacetic acid in drinking water.