作者：徐聪1, 赵婷1, 池海涛1, 李琴梅1,2, 成永霞3, 赵小学3, 刘伟丽1,2, 高峡1,2
作者单位：1. 北京市理化分析测试中心, 北京 100094;
2. 有机材料检测技术与质量评价北京市重点实验室, 北京 100094;
3. 河南省土壤重金属污染监测与修复重点实验室, 河南 济源 459000
关键词：电感耦合等离子体质谱法;微波消解;土壤;重金属;小麦
摘要：
建立微波消解-电感耦合等离子体质谱（ICP-MS）法同时测定土壤及对应耕作物小麦中8种重金属元素（Cr、Ni、Cu、Zn、As、Cd、Hg、Pb）含量的方法，比较不同的酸消解体系对土壤消解效果的影响。通过优化仪器参数、选择103Rh作单一内标元素校正土壤基体的干扰及仪器信号漂移，并编辑校正方程消除质谱干扰等，实现对土壤、小麦籽粒及小麦粉中重金属元素的准确测定。结果表明：以HNO3-H2O2-HF （5∶2∶2）为消解液体系微波消解土壤时，样品消解完全且效果最佳；各元素均呈现良好的线性关系，相关系数（r2）≥0.999 5；检出限在0.005~0.15 μg/L之间。土壤标准物质GBW07454（GSS-25）和小麦标准物质GSB10046（GSB-24）的测定值与标准值吻合，加标回收率在93.4%~103.6%范围内，方法精密度和准确度高。实际样品结果显示，土壤中Cd、Pb达到3级中污染水平；对应小麦籽粒和小麦粉中重金属元素与土壤存在一定的同源性，重金属元素更易富集于小麦籽粒中，其中Cd污染最严重。
Determination of eight kinds of heavy metal elements in cultivated soil and the wheat by microwave digestion-ICP-MS method
XU Cong1, ZHAO Ting1, CHI Haitao1, LI Qinmei1,2, CHENG Yongxia3, ZHAO Xiaoxue3, LIU Weili1,2, Gao Xia1,2
1. Beijing Center for Physical & Chemical Analysis, Beijing 100094, China;
2. Organic Material Testing Technology and Quality Evaluation of the Key Laboratory of Beijing, Beijing 100094, China;
3. Key Laboratory for Monitoring and Remediation of Heavy Metal Polluted Soils of Henan Province, Jiyuan 459000, China
Abstract: A method was established to determine eight kinds of heavy metal elements (Cr, Ni, Cu, Zn, As, Cd, Hg, Pb) in soil and the wheat by microwave digestion-inductively coupled plasma mass spectrometry (ICP-MS), and the effects of different acid digestion reagent systems on soil digestion were investigated. The heavy metal elements in soil, the wheat grains and the wheat flour were accurately determined by optimizing instrument parameters, selecting 103Rh as interior standard to correct the matrix interference and instrument signal drift, and editing correction equation to eliminate mass spectrum interference. The results indicated that the samples was dissolved completely with best effects when using HNO3-H2O2-HF (5:2:2) as digestion reagent system. Each element presented a good linear relationship with correlation coefficient (r2) ≥ 0.999 5, and the detection limit was between 0.005-0.15 μg/L. The method has high precision and accuracy because the determination results of GBW07454 (GSS-25) and GSB10046 (GSB-24) were consistent with the standard values and the recovery ranged between 93.4%-103.6%. The practical sample results showed that Cd, Pb reached the 3 level pollution in soil and the heavy metals in the soil were homologous with the corresponding wheat grains and wheat flour, and which are more likely to be enriched in wheat grain, among which the pollution of Cd was the most serious.
Keywords: inductively coupled plasma mass spectrometry method;microwave digestion;soil;heavy metal;wheat
2019, 45(5):85-92 收稿日期: 2019-01-17;收到修改稿日期: 2019-03-03
基金项目: 河南省土壤重金属污染监测与修复重点实验室开放基金资助项目（2017205）
作者简介: 徐聪(1990-),女,山西河津市人,硕士,研究方向光谱质谱分析
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