液-液萃取、衍生化气相色谱法测定饮用水中卤乙酸

Determination of haloacetic acids in drinking water by liquid-liquid extraction,derivatization with acidic methanol and gas chromatography with electron-capture detection

目的 :建立液 -液萃取、衍生化气相色谱法测定饮用水中卤乙酸的检测方法。方法 :通过各种条件实验确立色谱的实验条件 ;并对方法学中的线性、精密度和准确度等参数进行实验。结果 :选用中等极性毛细管柱 ,样品经MTBE萃取、甲醇衍生化后 ,用带有电子捕获检测器的气相色谱进行测定 ,同时可以分析MCAA、DCAA、TCAA、MBAA和DBAA5种化合物 ,16min内完成全部物质的测定 ,并且获得了较好的分离效果 ;0 5 μg/L～ 5 0 μg/L 浓度范围 ,5种物质工作曲线具有较好的直线线性 ,相关系数 (r)在 0 99～ 0 999之间 ;精密度测定结果RSD为 2 7%～ 10 0 % ;准确度回收率测定结果为 74 4%～ 12 0 %。结论 :该方法安全 ,简便 ,易于操作 ,技术参数符合方法检测的要求。

Objective:To obtained a method for determination of haloaceticacids(HAAs)in drinking water by liquid-liquid extraction,derivatization procedure and gas chromatography with electron-capture detection Methods:Some experimental conditions of gas chromatography and other parameters of the method were established by test Results:After extract with methyl-tert-butyl ether and methyl esters with methanol,the compounds of MCAA,MBAA,DCAA,TCAA and DBAA were analyzed in 16 min by capillary GC using an electron-capture detection The correlation coefficient of the method was 0 99～0 999 between 2 μg/L and 50 μg/L The recovery and the relative standard deviation were 74 4%～120% and 2 7%～10 0%,respectively Conclusion:The method is safe,simple and suitable for determination of HAAs in drinking water [