作者：邱东平, 姚旭松, 赵丽, 巢彪

作者单位：四川省科源工程技术测试中心，四川 成都 610091

关键词：电感耦合等离子体质谱法;石墨仪消解;土壤;金属

摘要：

提出更高效的石墨消解仪预处理样品，电感耦合等离子体质谱法（ICP-MS）同时测定土壤中的9种金属元素的方法。分析样品前处理的酸度比列、处理时间、氢氟酸残余量、内标元素选择、干扰校正系数优化等指标对测定结果和仪器的影响。结果表明，当盐酸、硝酸、氢氟酸比例为3∶1∶2、消解时间90 min、内标元素同时选择Rh和Re时，数据结果稳定且氢氟酸残余量对进样系统无影响。方法检出限钒、铬、锰、钴、镍、铜、锌、镉、铅，分别为0.05，0.07，0.1，0.005，0.05，0.05，0.54，0.004，0.09 μg/g，精密度（RSD, n=12）为1.31 %~5.06%。方法经国家标准物质分析验证，测定值与标准值相对误差为–7.69%~6.45%。此法测定结果准确、稳定，操作简单，且易控制污染，建议在同行业中推广使用。

Discussion on detection method of 9 metals in soil by graphite instrument digestion-ICP-MS
QIU Dongping, YAO Xusong, ZHAO Li, CHAO Biao
Sichuan Keyuan Engineering Technology Testing Center, Chengdu 610091, China
Abstract: In this paper, a more efficient method of sample pretreatment by graphite digester and simultaneous determination of 9 metal elements in soil by inductively coupled plasma mass spectrometry (ICP-MS) was proposed. The influence of acidity ratio, treatment time, hydrofluoric acid residue, selection of internal standard elements and optimization of interference correction coefficient on the determination results and instruments were analyzed. The results showed that when the ratio of hydrochloric acid, nitric acid and hydrofluoric acid was 3∶1∶2, the digestion time was 90 minutes, and the internal standard elements Rh and Re were selected at the same time, the data results were stable and the residual amount of hydrofluoric acid had barely effect on the injection system. The detection limits of V, Cr, Mn, Co, Ni, Cu, Zn, Cd and Pb were 0.05, 0.07, 0.1, 0.005, 0.05,  0.05, 0.54, 0.004, 0.09 μg/g, respectively, and the precision (RSD, n = 12) was 1.31%-5.06%. This method has been verified by the analysis of national reference materials, and the relative error between the measured value and the standard value was –7.69%-6.45%. The method is accurate, stable, easy to operate and easy to control pollution. It is recommended to be used in the same industry.
Keywords: ICP-MS;graphite instrument digestion;soil;metal
2020, 46(11):70-75  收稿日期: 2020-02-26;收到修改稿日期: 2020-03-27
基金项目:
作者简介: 邱东平(1986-),男,四川犍为县人,工程师,主要研究方向为仪器分析检测
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