Determination of Six Extractable Heavy Metals in Soil by ICP-MS
摘 要
为测定土壤中铜、铅、锌、镉、铬、镍等6种重金属可提取态的含量,采集农田区土壤样品,经风干、压碎、磨细、过筛等步骤制得粒度小于2 mm的分析样品。取此样品10.00 g,加入0.01 mol·L-1氯化钙溶液100 mL作提取剂(土液比为1:10),在密封状态下于(20±2)℃振荡提取120 min,所得悬浮液经离心分离,用带滤膜(0.45 μm)的针筒抽取溶液10 mL,加入硝酸两滴,供电感耦合等离子体质谱法分析。同时做空白试样。在质谱分析中,采用碰撞池模式,以流量4 mL·min-1的氦气为反应气体,从而消除了大部分质谱干扰。在制作标准曲线时,采用基体匹配法并在线加入103Rh(5.0 μg·L-1)和185Re(10 μg·L-1)混合标准溶液作为内标,有效地解决了基体效应等非质谱干扰。结果表明:所测定的6种重金属元素的质量浓度在一定范围内与其对应的信号强度之间呈线性关系,其检出限(3s)在0.002~0.012 mg·kg-1之间。应用此方法分析了两个标准样品(ASB-S2和ESS-EC-1)中上述6种重金属可提取态的含量,所得结果与认定值相符,测定值的相对标准偏差(n=6)在1.2%~6.8%之间。
Abstract
Aiming to the determination of 6 extractable heavy metals in soil, sample of soil was collected from field of farm-region, and treated by air-drying, crushing, grinding and sieving to prepare a portion of analytical sample having sizes less than 2 mm. 10.00 g of the prepared soil sample were extracted with 100 mL of 0.01 mol·L-1 CaCl2 solution (keeping the soil to solution ratio of 1 to 10) in a tightly-sealed polyethylene (PE) flask at (20±2)℃ for 120 min under constant shaking. An aliquot of 10 mL of clear solution was taken from the suspension with a filtering-syringe attached with 0.45 μm filtering membrane. Two drops of conc. HNO3 were added to the solution, and mixed well. This solution is ready for use in ICP-MS analysis. A blank solution should be prepared simultaneously by the same procedure. The mode of collision cell with He gas at a flow-rate of 4 mL·min-1 as reacting gas was used in MS, to eliminate most of the mass spectral interferences, and mixed standard solution of 103Rh (5.0 μg·L-1) and 185Re (10 μg·L-1) was added to overcome non-MS interferences, such as matrix effect and etc. Linear relationships were obtained between values of the signal intensities and the respective mass concentrations of the 6 heavy metal elements, values of detection limit (3s) were found in the range of 0.002-0.012 mg·kg-1. Two standard samples (ASB-S2 and ESS-EC-1) were analyzed by the proposed method, giving values of extractable contents of the 6 heavy metals in consistency with the certified values, and values of RSDs (n=6) found were in the range of 1.2%-6.8%.
中图分类号 O657.63 DOI 10.11973/lhjy-hx201907019
所属栏目 专题报道(电感耦合等离子体质谱法)
基金项目 广西科学研究与技术开发计划项目(桂科AD18126020);中国有色桂林矿产地质研究院有限公司创新基金项目(KDY2017007)
收稿日期 2019/1/15
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备注唐碧玉,高级工程师,硕士,主要从事电感耦合等离子体质谱法和电感耦合等离子体原子发射光谱法的应用研究,187354191@qq.com
引用该论文: TANG Biyu,SHI Yihua,QIU Li,YANG Zhaohong,GU Xingqian,TANG Rongsheng. Determination of Six Extractable Heavy Metals in Soil by ICP-MS[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2019, 55(7): 846~852
唐碧玉,施意华,邱丽,阳兆鸿,古行乾,唐荣盛. 电感耦合等离子体质谱法测定土壤中6种重金属可提取态的含量[J]. 理化检验-化学分册, 2019, 55(7): 846~852
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参考文献
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【3】PUEYO M, LÍPEZ-SÁNCHEZ J F, RAURET G. Assessment of CaCl2, NaNO3 and NH4NO3 extraction procedures for the study of Cd, Cu, Pb and Zn extractability in contaminated soils[J]. Analytica Chimica Acta, 2004,504(2):217-226.
【4】李亮亮,张大庚,李天来,等.土壤有效态重金属提取剂选择的研究[J].土壤, 2008,40(5):819-823.
【5】荆延德,何振立,杨肖娥,等.稻菜轮作制下土壤有效态汞提取剂和提取条件研究[J].水土保持通报, 2012,32(4):185-189.
【6】宋伟娇,代世峰,赵蕾,等.微波消解-电感耦合等离子体质谱法测定煤中的硼[J].岩矿测试, 2014,33(3):327-331.
【7】唐碧玉,施意华,杨仲平,等.灰化酸溶-电感耦合等离子体质谱法测定煤炭中的镓锗铟[J].岩矿测试, 2018,37(4):371-378.
【8】FOTEEVA L S, MATCZUK M, PAWLAK K, et al. Combination of ICP-MS, capillary electrophoresis, and their hyphenation for probing Ru(Ⅲ) metallodrug-DNA interactions[J]. Analytical and Bioanalytical Chemistry, 2017,409(9):2421-2427.
【9】YANG B, ZHANG Y, CHEN B B, et al. Elemental-tagged immunoassay combined with inductively coupled plasma mass spectrometry for the detection of tumor cells using a lead sulfide nanoparticle label[J]. Talanta, 2017,167:499-505.
【10】潘春燕,张频,宋寅生,等.电感耦合等离子体质谱法测定血浆和血清中12种微量元素[J].理化检验-化学分册, 2018,54(3):355-359.
【11】周莉,石贵勇,付宇,等.广州市大气颗粒物PM2.5显微形貌特征和来源解析[J].岩矿测试, 2016,35(3):302-309.
【12】马金晶,罗雯,张龙旺,等.微波消解-电感耦合等离子体质谱法测定人面果树中的重金属元素[J].分析试验室, 2012,31(7):32-35.
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【15】蒙华毅,梁书怀,吴祖军,等.碰撞反应池-电感耦合等离子体质谱法同时测定甘蔗中的9种重金属元素[J].理化检验-化学分册, 2015,51(9):1240-1243.
【16】BRINKHAUS S G, BORNHORST J, CHAKRABORTY S, et al. Elemental bioimaging of manganese uptake in C. elegans[J]. Metallomics, 2014,6(3):617-621.
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