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目的建立液液萃取气相色谱法测定饮用水和水源水中9种卤代乙酸和2种除草剂共11种卤代酸的方法。方法采用甲基叔丁基醚为萃取溶剂,1,2-二溴丙烷为内标溶剂,在酸性条件下加氯化钠萃取水中的卤代酸。取甲基叔丁基醚层加入硫酸酸化的甲醇溶液,在酸性条件下,50℃酯化反应1 h,采用气相色谱法进行检测。结果方法的线性范围为2.0μg/L~100.0μg/L,线性相关系数为0.999 0~0.999 9,检出限为0.09μg/L~0.65μg/L;在2.0μg/L、20.0μg/L、100.0μg/L 3个添加水平范围内的平均加标回收率分别为83.5%~106.2%、89.0%~104.1%、87.1%~99.3%;相对标准偏差(RSD)为0.36%~6.23%。结论该方法在测定饮用水和水源水中的11种卤代酸时,具有操作简单、干扰少、快速、准确可靠等特点,适合用于居民生活饮用水和水源水的日常监控。
OBJECTIVE To establish a method for the determination of 11 haloacid acids and 2 kinds of herbicides in drinking water and drinking water by liquid-liquid extraction and gas chromatography. Methods Methyl tert-butyl ether was used as extraction solvent and 1,2-Dibromopropane as internal standard solvent. Under acidic condition, sodium chloride was added to extract haloacid in water. Take methyl tert-butyl ether layer was added sulfuric acid solution of methanol, under acidic conditions, 50 ℃ esterification reaction 1 h, using gas chromatography detection. Results The linear range of the method was 2.0μg / L ~ 100.0μg / L, the linear correlation coefficient was 0.999 0 ~ 0.999 9, the detection limit was 0.09μg / L ~ 0.65μg / L; And 100.0 μg / L respectively. The average recoveries were 83.5% -106.2%, 89.0% -104.1% and 87.1% -99.3%, respectively. The relative standard deviations (RSDs) ranged from 0.36% to 6.23%. Conclusion The method has the characteristics of simple operation, less interference, quickness, accuracy and reliability when measuring 11 kinds of halogenated acids in drinking water and source water. It is suitable for daily monitoring of drinking water and water source water of residents.