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中国无机分析化学:2022,12(3):24-30
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微波/电热板组合消解-电感耦合等离子体质谱(ICP-MS)法测定土壤中重金属元素
(浙江省温州生态环境监测中心)
Determination of Heavy Metals in Soil by ICP-MS Combined with Microwave/Electric Heating Plate Digestion
TAO Zhen-yan1, WANG Shen1, YE Shaozuo2
(1.Zhejiang Province Wenzhou Ecological Environment Monitoring Center;2.Zhejiang Province Wenzhou Ecological Environment Monitoring Center,)
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投稿时间:2021-08-09    修订日期:2021-08-23
中文摘要: 为提高土壤检测的重金属得率,采用了微波消解/电热板组合预处理-电感耦合等离子体质谱法(ICP-MS)测定土壤重金属含量。分析了硝酸(HNO3)、氢氟酸(HF)、高氯酸(HClO4)和盐酸(HCl)组合消解液及赶酸温度对土壤预处理影响。结果显示:在硝酸和盐酸混合消解液中,硝酸占比越高,铬(Cr)、钴(Co)、铜(Cu)、镉(Cd)得率更高;消解液体系中加入氢氟酸可使消解更加彻底,提高铬与铜的得率。最优预处理消解条件为硝酸 6ml+ 氢氟酸 2ml消解液组合进行微波消解,1ml 高氯酸于155℃电热板上赶酸。经土壤标准样品GBW07401(GSS-1)和GBW07452(GSS-23)实际应用,预处理条件优化后测试准确度和稳定性均显著提高。此外使用元素铑(Rh)作为内标物时,其方法稳定性和准确性高于内标物钪(Sc)和锗(Ge)。可为相关国家土壤重金属测定标准的修制订提供方法学参考。
Abstract:In order to improve the yield of heavy metals in soil digestion pretreatment, the content of heavy metals in soil was determined by microwave digestion/electrothermal plate combined inductively coupled plasma mass spectrometry (ICP-MS). The effects of combined digestion solution and temperature on microwave pretreatment were analyzed. The results show that the higher the proportion of HNO3 in the digestion solution, the higher the yield of Cr, Co, Cu, CD and other heavy metals; HF can remove the residue and improve the Cr and Cu yield. The optimal pretreatment digestion conditions were microwave digestion with HNO3 6ml + HF 2ml, and 1ml HClO4 was removed on 155℃ electrothermal plate. The practical application of national certified reference materials of soil GBW07401(GSS-1)and GBW07452(GSS-23) shows that the accuracy and stability of the test are improved significantly after the optimization of the pretreatment conditions. In addition, when Rh is used as internal standard, the stability and accuracy of the method are higher than that of SC and Ge. It provides a reference for the revision of the soil heavy metal determination national standards.
文章编号:     中图分类号:X833;O657.63    文献标志码:
基金项目:温州市基础性社会发展科技项目(No.S2020014)
引用文本:
陶甄彦,王珅,叶绍佐.微波/电热板组合消解-电感耦合等离子体质谱(ICP-MS)法测定土壤中重金属元素[J].中国无机分析化学,2022,12(3):24-30.
TAO Zhen-yan,WANG Shen,YE Shaozuo.Determination of Heavy Metals in Soil by ICP-MS Combined with Microwave/Electric Heating Plate Digestion[J].Chinese Journal of Inorganic Analytical Chemistry,2022,12(3):24-30.

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