气相色谱法测定水中氯乙酸的研究

Study on Determination of Chloroacetic Acid in Water by Gas Chromatography

[目的 ]建立一种简便、准确、适于基层使用的测定水中氯乙酸方法。 [方法 ]用酸、甲醇酯化氯乙酸 ,15 %DEGS填充色谱柱分离 ,电子捕获检测器检测。 [结果 ]氯乙酸最佳酯化条件 :温度 60℃ ,时间 60min ,浓硫酸 0 4ml,甲醇0 8ml。色谱最佳测试条件 :15 %DEGS色谱柱分离 ,柱温 10 5℃ ,气化室温度 190℃ ,检测室温度 190℃。该法线性范围较宽 ,一氯乙酸线性范围在 2 5～ 40 0 μg/ml(r=0 993 9) ,三氯乙酸线性范围在 0 2 5～ 1 0 μg/ml(r =0 9940 ) ,回收率在 95 %～ 10 5 %之间 ,CV均小于 5 % ,显示出良好的精密度和准确度。 [结论 ]本法具有快速、灵敏、准确等优点 。

To establish a simple and accurate method for detecting chloroacetic acid in water. Chloroacetic acid was esterified by acid and methanol,separated by 15% DMGS column,determined by gas chromatography. The best derivatizative conditions:60℃,10 min,concentrated sulfuric acid 0 4 ml,methanol 0 8 ml. The best chromatographic condition:15% DMGS column was used,the column temperature 105℃,injector temperature 190℃,detector temperature 190℃. The method has wider linear dependence. The linear range of monochloroacetic acid is from 25 to 400 μg/ml( r =0 993 9),and that of trichloroacetic acid is also from 0 25 to 1 0 μg/ml( r =0 994 0). The recovery rate is 95%～105%( CV <5%). [Conclusion] The results showed that the method is rapid,simple,sensitive and accurate.