摘要
目的 建立一种大体积进样离子色谱方法同时测定生活饮用水中的氟离子、氯离子、硝酸盐、硫酸盐、溴酸盐、亚氯酸盐、氯酸盐、二氯乙酸、三氯乙酸和草甘膦的含量.方法 水样经0.22 μm滤膜过滤,200μl大体积进样分析,利用淋洗液发生装置实现流动相KOH溶液梯度淋洗,并探究2种不同梯度淋洗模式的检测效果,流速为1.0 ml/min,通过IonPac AS19分析柱分离,电导检测器检测.结果 氟离子、氯离子、硝酸盐、硫酸盐、草甘膦在0.05 mg/L～10.0 mg/L,溴酸盐、亚氯酸盐、氯酸盐在0.005 mg/L～0.2 mg/L,二氯乙酸、三氯乙酸在0.01 mg/L～0.2 mg/L浓度内线性相关系数均＞0.999 0,加标回收率为90.2％～116.1％,相对标准偏差均＜2.75％(n=5),方法检出限为0.2 μg/L～5.3 μg/L(S/N=3).该方法能有效分离生活饮用水中的10种阴离子,满足实际样品的检测需求.结论 本方法操作简单、灵敏度高、准确性好,可用于生活饮用水中氟离子、氯离子、硝酸盐、硫酸盐、溴酸盐、亚氯酸盐、氯酸盐、二氯乙酸、三氯乙酸和草甘膦的测定.
Abstract
Objective This paper aims to establish a method for the simultaneous determination of fluoride,chloride,nitrate,sulfate,bromate,chlorite,chlorate,dichloroacetic acid,trichloroacetic acid and glyphosate concentrations in drinking water by ion chromatography with large volume injection.Methods Drinking water samples were filtered through 0.22 μm filter mem-brane and mass injection of 200 μl was adopted for analysis.Gradient leaching of mobile phase KOH solution was realized by a leach generation device,and the detection effect of two different gradient leaching modes was explored.The flow rate was 1.0 ml/min,which was separated by IonPac AS19 analysis column and detected by conductivity detector.Results The corre-lation coefficients(r)were greater than 0.999 0 and the recoveries were within 90.2％-116.1％when fluoride,chloride,nitrate,sulfate and glyphosate were in the range of 0.05 mg/L-10.0 mg/L,bromate,chlorite,chlorate were in the range of 0.005 mg/L-0.2 mg/L,and dichloroacetic acid and trichloroacetic acid were in the concentrations of 0.01 mg/L-0.2 mg/L.The relative standard deviations(RSD)were all less than 2.75％(n=5).The detection limits were within 0.2 μg/L-5.3 μg/L(S/N=3).This method could effectively isolate ten anions and meet the requirements for practical sam-ple testing.Conclusion The method is simple,sensitive,and accurate.It can be used for the detection of fluoride,chloride,nitrate sulfate,bromate,chlorite,chlorate,dichloroacetic acid,trichloroacetic acid,glyphosate in drinking water.
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维普
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