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目的建立饮用水中微量丙烯腈的顶空气相色谱-氮磷检测器(HS-GC-NPD)测定方法。方法吸取10.00 ml水样,加入3.0 g氯化钠,加盖密封,经50℃平衡60 min,吸取顶空气体1.00 ml,进气相色谱分析,用HP-INNOWAX毛细管色谱柱程序升温分离,经NPD检测器分析,以保留时间定性,外标法定量。结果本试验方法测定饮用水中丙烯腈的检出限为0.002 mg/L。线性范围为0.04μg/ml~2.00μg/ml。样品加标回收率为87.0%~112.0%。8次平行测定结果的相对标准偏差(RSD)为2.16%~3.24%。结论该方法具备操作简单快速、灵敏度高、准确度及重现性好等优点,对检测饮用水中的丙烯腈具有一定的实用性和可操作性。
Objective To establish a method for determination of trace acrylonitrile in drinking water by headspace gas chromatography-nitrogen and phosphorus detector (HS-GC-NPD). Methods The water sample of 10.00 ml was taken and added with 3.0 g of sodium chloride. The mixture was sealed and sealed. After equilibrating at 50 ° C for 60 min, 1.00 ml of headspace gas was drawn in. The gas chromatographic analysis was carried out by using HP-INNOWAX capillary column chromatography. NPD detector analysis, retention time qualitative, external standard method of quantification. Results The detection limit of acrylonitrile in drinking water by this test method was 0.002 mg / L. The linear range was 0.04 μg / ml to 2.00 μg / ml. The recoveries of spiked samples ranged from 87.0% to 112.0%. The relative standard deviations (RSDs) of 8 replicates were 2.16% -3.24%. Conclusion The method has the advantages of simple and rapid operation, high sensitivity, good accuracy and reproducibility, and has some practicality and operability for the detection of acrylonitrile in drinking water.