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李自强, 李小英, 钟琦, 苏文峰, 诸堃. 电感耦合等离子体质谱法测定土壤重金属普查样品中铬铜镉铅的关键环节研究[J]. 岩矿测试, 2016, 35(1): 37-41. DOI: 10.15898/j.cnki.11-2131/td.2016.01.007
引用本文: 李自强, 李小英, 钟琦, 苏文峰, 诸堃. 电感耦合等离子体质谱法测定土壤重金属普查样品中铬铜镉铅的关键环节研究[J]. 岩矿测试, 2016, 35(1): 37-41. DOI: 10.15898/j.cnki.11-2131/td.2016.01.007
Zi-qiang LI, Xiao-ying LI, Qi ZHONG, Wen-feng SU, Kun ZHU. Determination of Cr, Cu, Cd and Pb in Soil Samples by Inductively Coupled Plasma-Mass Spectrometry for an Investigation of Heavy Metal Pollution[J]. Rock and Mineral Analysis, 2016, 35(1): 37-41. DOI: 10.15898/j.cnki.11-2131/td.2016.01.007
Citation: Zi-qiang LI, Xiao-ying LI, Qi ZHONG, Wen-feng SU, Kun ZHU. Determination of Cr, Cu, Cd and Pb in Soil Samples by Inductively Coupled Plasma-Mass Spectrometry for an Investigation of Heavy Metal Pollution[J]. Rock and Mineral Analysis, 2016, 35(1): 37-41. DOI: 10.15898/j.cnki.11-2131/td.2016.01.007

电感耦合等离子体质谱法测定土壤重金属普查样品中铬铜镉铅的关键环节研究

Determination of Cr, Cu, Cd and Pb in Soil Samples by Inductively Coupled Plasma-Mass Spectrometry for an Investigation of Heavy Metal Pollution

  • 摘要: 土壤重金属普查样品的基质复杂、数量大、待测元素性质各异, 现有土壤中重金属的电感耦合等离子体质谱法(ICP-MS)存在样品分解方式不适宜、上机测定参数需优化等问题。本文采用电热板-酸分解样品, 研究了ICP-MS测定土壤中Cr、Cu、Cd、Pb四种主要重金属在分解和上机测定中的关键环节。结果表明采用"硝酸+盐酸+氢氟酸+50%硫酸"体系, 样品分解完全且待测元素无损失, 并使用工作曲线校准仪器可降低基体效应; 优选质谱测定同位素和采用碰撞反应池或数学校正可减少质谱干扰; 质谱积分驻留时间和重复次数对痕量元素Cd的精密度有较大影响, 宜设为0.4 s和3次。本方法对Cr、Cu、Cd、Pb的检出限分别为1.74、0.89、0.015、0.08μg/g, 为普查工作提供了一种可借鉴的分析手段。

     

    Abstract: The present methods for the determination of heavy metals in soil by Inductively Coupled Plasma-Mass Spectrometry(ICP-MS) have many disadvantages including an inappropriate decomposition process and the parameters of instruments requiring optimization.To address this inadequacy, soil samples for an investigation of heavy metal pollution have been characterized by complex matrices, large weights and different properties of measured elements.Combining acid decomposition on an electric heating plate with ICP-MS, the key to determination of four kinds of main heavy metal pollutants, Cr, Cu, Cd and Pb, in soil were explored and are presented in this study.The results show that the samples can be decomposed completely by a mixture of nitric acid, hydrochloric acid, hydrofluoric acid, and sulfuric acid(50%).The matrix effect is reduced effectively by the work curve and the mass spectrum interference is reduced effectively by both adopting collision/reaction cell technology and by mathematical correction.Integration time and repeated times of ICP-MS have significant influences on testing results of trace Cd, so the optimal parameters of them are 0.4s and 3 times, respectively.The detection limits of this method for Cr, Cu, Cd and Pb are 1.74, 0.89, 0.015 and 0.08μg/g, respectively.This study provides a rapid and accurate method for determining heavy metals in soil.

     

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