作者：闫学全

作者单位：青海省海东市环境监测站, 青海 海东 810600

关键词：自动石墨消解;ICP-MS;工业区;土壤;方法

摘要：

建立电感耦合等离子体质谱法监测工业区土壤样品中砷、汞、硒、锑4种微量元素残留的分析方法。利用全自动石墨消解仪消解工业园区土壤样品，盐酸-硝酸-氢氟酸体系作为消解酸体系，按照程序设置进行密闭消解，消解液用3%稀硝酸定容，电感耦合等离子体质谱仪定量检测砷、汞、硒、锑4种元素残留量。4种元素质量浓度在0.02~10 g/L范围内线性关系良好，相关系数（r2）0.995；4种元素加标回收率范围为84.5%~107.2%；检出限：砷0.001 8 g/L、汞0.003 4 g/L、硒0.007 4 g/L、锑0.001 0 g/L；精密度相对标准偏差RSD（n=6）在1.35%~3.51%之间，重复性相对标准偏差RSD（n=6）在2.47%~4.89%之间。结果表明，该方法具有前处理快速、检出限低、重复性好、检测结果准确可靠等优点，适用于工业园区土壤中微量元素残留的检测。

Automatic graphite digestion-ICP-MS method for detection of arsenic, mercury, selenium and antimony elements in industrial soil

YAN Xuequan

Haidong Environmental Monitoring Station of Qinghai Province, Haidong 810600, China

Abstract: A ICP-MS method for detection residues of 4 microelements (arsenic, mercury, selenium and antimony) of industrial soil samples was established. Automatic graphite digestion instrument was used to digest industrial soil samples, HCl-HNO₃-HF system was selected as digestion solution system, samples were digested enclosing and digestion solution was diluted with 3% HNO₃ to a constant volume. Then residues of 4 microelements were tested quantitatively by ICP-MS. Concentration of 4 microelements showed good linear relationships in the range 0.02-10 μg/L, with the correlation coefficients were above 0.995. The recoveries of 4 microelements were between 84.5%-107.2%. The detection limits were as follows: arsenic 0.001 8 μg/L, mercury 0.003 4 μg/L, selenium 0.007 4 μg/L, antimony 0.001 0 μg/L. The relative standard deviation of precision (n=6) were between 1.35%-3.51%. Relative standard deviation of reproducibility (n=6) were in the range 2.47%-4.89%.The results showed that this method has the advantages of quick pre-treated, low detection, good reproducibility with accuracy and reliable results, which can apply to detection of microelements of industrial soil.

Keywords: automatic graphite digestion;ICP-MS;industrial area;soil;method

2018, 44(11): 77-80  收稿日期: 2018-07-15;收到修改稿日期: 2018-08-22

基金项目: 

作者简介: 闫学全(1979-),男,青海海东市人,高级工程师,主要从事环境监测工作

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