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探索了从环境样品中提取甲基汞的方法,并通过对环境样品中的甲基汞分析方法的研究,对比用ICP-MS、FIMS和GC-ECD 3种分析仪器检测环境样品中的甲基汞。实验优化了溶剂萃取种类、溶剂浓度和各种辅助萃取条件。选用2 mol/L盐酸溶液作为溶剂萃取环境样品的甲基汞,然后采用ICP-MS、FIMS和GC-ECD分别测定甲基汞的含量。水质样品中的检出限分别为0.012、0.009 6和0.004μg/L;土壤样品中的检出限为0.04,0.02,0.02μg/L,相对标准偏差小于8%,基体加标回收率在85%～95%。3种分析方法对甲基汞的分析都能满足实际样品的分析测试需要。但ICP-MS对样品的前处理溶液可以直接上机检测,元素干扰少,适应批量样品的分析;而GC-MS对样品前处理溶液需要进行有机溶剂转换,增加了操作的复杂性;FIMS分析时,当有机物含量高时,干扰明显,影响汞的还原效率。
The method of extracting methylmercury from environmental samples was explored. By comparing methylmercury analysis method in environmental samples, the methyl groups in environmental samples were detected by ICP-MS, FIMS and GC-ECD HG. The experimental optimization of solvent extraction, solvent concentration and various auxiliary extraction conditions. Methylmercury was extracted from environmental samples using 2 mol / L hydrochloric acid as solvent, and the content of methylmercury was determined by ICP-MS, FIMS and GC-ECD respectively. The detection limits of water samples were 0.012,0.009 6 and 0.004μg / L, respectively. The detection limits of soil samples were 0.04,0.02,0.02μg / L, the relative standard deviations were less than 8%, and the recoveries were 85 % ~ 95%. Three kinds of analytical methods for the analysis of methylmercury can meet the actual sample analysis and testing needs. However, ICP-MS pretreatment of the sample solution can be directly on the machine test, the element less interference, to adapt to batch sample analysis; and GC-MS sample pretreatment solution requires organic solvent conversion, increasing the complexity of the operation; FIMS analysis When the organic content is high, the interference is obvious, affecting the reduction efficiency of mercury.