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全自动蒸馏前处理-ID/GC-ICP-MS测定海水中痕量甲基汞
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作者单位
冷金慧,王立军,刘亮,高亚倩,林忠胜,王华 1.大连海洋大学水产与生命学院2.国家海洋局近岸海域生态环境重点实验室国家海洋环境监测中心3.辽宁师范大学化学化工学院 
基金项目:国家自然科学基金项目(21577028);辽宁省高等学校创新人才支持计划;辽宁省教育厅科学研究项目(L201603);生态环境及其信息图谱福建省高等学校重点实验室开放课题(ST17001)
中文摘要:建立了基于自动蒸馏前处理,气相色谱-电感耦合等离子质谱联用(GC-ICP-MS),同位素稀释法(ID)测定海水中痕量甲基汞的分析方法。结果表明,自动蒸馏仪在45 min内即可完成海水样品的蒸馏,采用BrCl溶液能有效消除蒸馏管路中甲基汞的残留,降低实验空白;同位素稀释剂的添加量对甲基汞的测定结果明显影响,样品中总汞质量浓度低于1.0 μg·L-1时,因操作产生的甲基汞量可忽略不计。海水中甲基汞的加标回收率为98.2%~122%,天然海水及加标海水中甲基汞的相对标准偏差(RSD)分别为16%和5.4%,方法检出限为0.009 ng·L-1。以大连湾表层海水为实际样品,测得水样中甲基汞的质量浓度的平均值为(0.103±0.036) ng·L-1,方法可满足近岸海水中痕量甲基汞的分析要求。
中文关键词:气相色谱-电感耦合等离子质谱  同位素稀释  海水  甲基汞  全自动蒸馏仪
 
Determination of Trace of Methylmercury in Seawater by Isotope Dilution/Gas Chromatography-Inductively Coupled Plasma Mass Spectrometry with an Automatic Distillation
Abstract:An isotope dilution/gas chromatography-inductively coupled plasma mass spectrometric(ID/GC-ICP-MS)method was developed for the separation and determination of trace of methylmercury(MeHg)in seawater after an automatic distillation.Results showed that the distillation pretreatment for the seawater samples could be completed in 45 min using an automatic distillation apparatus,and BrCl solution was very efficient in removing the MeHg residues in the distillation ware,which could result in the procedural blank lowering markedly.The artificial MeHg during the distillation process might be negligible if the total mercury mass concentration in the sample was lower than 1.0 μg·L-1.The spiked recoveries for MeHg in seawater ranged from 98.2% to 122%,with RSDs for MeHg in natural seawater and spiked seawater of 16% and 5.4%,respectively,and the detection limits were 0.009 ng·L-1.The method was applied in the analysis of MeHg in the surface seawater collected from Dalian Bay with average MeHg concentration of (0.103±0.036) ng·L-1,and it could meet the requirements for analysis of trace methylmercury in coastal water.
Key Words:gas chromatography-inductively coupled plasma mass spectrometry(GC-ICP-MS)  isotope dilution  seawater  methylmercury  automatic distillation apparatus
引用本文:冷金慧,王立军,刘亮,高亚倩,林忠胜,王华.全自动蒸馏前处理-ID/GC-ICP-MS测定海水中痕量甲基汞[J].分析测试学报,2018,37(9):1071-1075.
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