Determination of Chromium, Copper, Zinc, Cadmium, Lead and Nickel in Soil by ICP-MS with Microwave Digestion
摘 要
建立了微波消解-电感耦合等离子体质谱法(ICP-MS)测定土壤中铬、铜、锌、镉、铅、镍等含量的方法。土壤样品0.200 0 g在6 mL硝酸、2 mL盐酸和2 mL氢氟酸中微波消解;消解结束后,于150℃敞口赶酸至约2 mL,加入2 mL高氯酸继续赶酸至溶液呈不流动的黏稠状,用水溶解残渣,再用1%(体积分数)硝酸溶液定容至50 mL,采用ICP-MS对样品进行分析。结果显示:6种重金属元素标准曲线的线性范围均在50 μg·L-1以内,检出限(3s)为0.001~0.26 μg·L-1。对空白样品进行加标回收试验,回收率为94.3%~103%,测定值的相对标准偏差(n=6)为1.3%~2.8%。方法用于8处饮用水源地土壤样品的分析,以湖北省土壤背景值为参比,采用地积累指数对其进行评价,结果显示7处土壤未受到污染,1处土壤受到轻度污染。
Abstract
A method for the determination of chromium, copper, zinc, cadmium, lead and nickel in soil by inductively coupled plasma mass spectrometry (ICP-MS) with microwave digestion was developed. Soil sample of 0.200 0 g was digested by microwave in 6 mL of nitric acid, 2 mL of hydrochloric acid and 2 mL of hydrofluoric acid. After digestion, the solution was exposed to remove acid to about 2 mL at 150 ℃, and 2 mL of perchloric acid was added to continue to remove acid until the solution was stiff and viscous. The residues were dissolved in water, and 1% (φ) nitric acid solution was added to make its volume up to 50 mL. ICP-MS was used to analyze the sample. As shown by the results, linear ranges of the standard curves of 6 heavy metal elements were all within 50 μg·L-1, with detection limits (3s) in the range of 0.001-0.26 μg·L-1. Recovery test was made on blank samples by standard addition method, giving results in the range of 94.3%-103%, and RSDs (n=6) of the determined values ranged from 1.3% to 2.8%. This method was applied to the analysis of soil samples from 8 drinking water sources. The soil accumulation index was used to evaluate the soil samples with the soil background value of Hubei province as reference. The results showed that the soil samples of 7 places were not polluted, and the soil sample of 1 place was slightly polluted.
中图分类号 O657.63 DOI 10.11973/lhjy-hx202110012
所属栏目 工作简报
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收稿日期 2021/3/18
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备注徐雯,工程师,硕士,主要从事环境监测实验室分析工作,76242981@qq.com
引用该论文: XU Wen,FANG Qi,QI Liangliang. Determination of Chromium, Copper, Zinc, Cadmium, Lead and Nickel in Soil by ICP-MS with Microwave Digestion[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2021, 57(10): 923~927
徐雯,方琦,漆亮亮. 微波消解-电感耦合等离子体质谱法测定土壤中铬、铜、锌、镉、铅、镍的含量[J]. 理化检验-化学分册, 2021, 57(10): 923~927
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参考文献
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【6】李海峰, 王庆仁, 朱永官.土壤重金属测定两种前处理方法的比较[J].环境化学, 2006, 25(1):108-109.
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