半密闭酸溶-电感耦合等离子体质谱(ICP-MS)法测定化探样品中的铬、镍、铜、锌、镉、铅等6种重金属  

Determination of Chromium, Nickel, Copper, Zinc, Cadmium, Lead in Geological Samples by Inductively Coupled Plasma Mass Spectrometry(ICP-MS) with Semi-closed Acid Solution

作　　者：孙孟华 金倩 陈庆芝 李晓敬 朱永晓 王文娟 SUN Menghua;JIN Qian;CHEN Qingzhi;LI Xiaojing;ZHU Yongxiao;WANG Wenjuan(Hebei Research Center for Geoanalysis,Baoding,Hebei 071051,China;Hebei Provincial Key Laboratory of Mineral Resources and Ecological Environment Monitoring,Baoding,Hebei 071051,China)

机构地区：[1]河北省地质实验测试中心,河北保定071051 [2]河北省矿产资源与生态环境监测重点实验室,河北保定071051

出　　处：《中国无机分析化学》2023年第4期318-325,共8页Chinese Journal of Inorganic Analytical Chemistry

基　　金：保定市科技计划项目(2140ZZ034)。

摘　　要：通过采用半密闭酸溶消解法处理样品,选择离线校正的方式校正了Sn对Cd的同量异位素的干扰,增加积分时间和读数次数提高了Cd的准确度和精密度,对前处理方法和仪器的参数条件进行优化,建立了电感耦合等离子体质谱(ICP-MS)法测定化探样品中Cr、Ni、Cu、Zn、Cd、Pb等6种重金属元素的方法。结果表明,半密闭体系可达到回流的目的,样品分解完全且无污染现象,在最优的实验条件下,标准曲线的相关系数均不小于0.999 7,检出限为0.019~1.65μg/g,测定下限为0.057~4.95μg/g。按照实验方法对岩石、水系沉积物和土壤国家标准物质中Cr、Ni、Cu、Zn、Cd、Pb平行测定12次,各元素的测定结果与认定值基本一致,相对偏差均不大于3.6%,相对误差均不大于10.3%。对土壤样品进行分析,测定结果与四酸溶解-电感耦合等离子体发射光谱(ICP-OES)法测定Cr、Ni、Cu、Zn、Pb,火焰-石墨炉原子吸收光谱法测定Cd的结果基本吻合。The interference of Sn on the same amount of ectopic element of Cd was corrected by using the semi-closed acid digestion method to treat the sample.The accuracy and precision of Cd were improved by increasing the integration time and the number of readings.After optimizing the preprocessing method and instrument parameter conditions, a method for the determination of Cr, Ni, Cu, Zn, Cd and Pb in geological samples by inductively coupled plasma mass spectrometry(ICP-MS) was established.The results showed that the semi-closed system could achieve the purpose of reflux, complete sample decomposition and no pollution phenomenon.Under optimal experimental conditions, the correlation coefficient of the standard curve was no less than 0.999 7 with the limit of detection ranged from 0.019 to 1.65 μg/g and the limit of quantification ranged from 0.057 to 4.95 μg/g.According to the experimental method, Cr, Ni, Cu, Zn, Cd and Pb in the national standard materials of rocks, water system sediments and soil were tested for 12 times.The determination results of each element were basically consistent with the certified values, where the relative deviations were no more than 3.6% and the relative error were no more than 10.3%.Then, the soil samples were analyzed and the results were basically consistent with those of the determination of Cr, Ni, Cu, Zn, Pb by tetra-acid dissolution-ICP-OES and the determination of Cd by flame-graphite furnace atomic absorption method.

关 键 词：化探样品 半密闭酸溶 电感耦合等离子体质谱 重金属 

分 类 号：O657.63[理学—分析化学]