微波消解–电感耦合等离子体质谱法测定土壤中总镉、铅、铬含量的不确定度评定  

Uncertainty evaluation of the determination of Cd,Pb and Cr in soil by microwave digestion-inductively coupled plasma mass spectrometry

作　　者：胡春 孙永兴 许凯歌 常立群 张静 HU Chun;SUN Yong-Xing;XU Kai-Ge;CHANG Li-Qun;ZHANG Jing(The Analysis and Test Center of Ningxia of North Minzu University,Yinchuan 750020,China;Ningxia Agricultural Institute of Survey and Design,Yinchuan 750002,China;Quality Standards and Testing Institute of Agricultural Technology,Yinchuan 750002,China)

机构地区：[1]北方民族大学宁夏分析测试中心,银川750020 [2]宁夏农业勘查设计院,银川750002 [3]宁夏农产品质量标准与检测技术研究所,银川750002

出　　处：《实验室检测》2024年第10期82-86,共5页Laboratory Testing

基　　金：宁夏农林科学院科技创新引导基金项目(NKYG–24–13)

摘　　要：目的评估微波消解–电感耦合等离子体质谱法(ICP-MS)测定土壤中总镉(Cd)、铅(Pb)、铬(Cr)含量时的不确定度。方法为确保检测结果准确可靠,采用微波消解–电感耦合等离子体质谱法(ICP-MS)测定土壤中总镉(Cd)、铅(Pb)、铬(Cr)含量的不确定度,并依据JJF1059.1—2012《测量不确定度评定与表示》,计算合成不确定度,得出扩展不确定度。结果影响检测结果的不确定度来源主要有标准溶液配制过程、样品重复测量和标准曲线拟合,对Cd、Pb、Cr含量不确定度的贡献率分别为50.4%~60.3%、18.7%~26.1%、12.1%~20.4%,样品称量和消解定容对不确定度的影响很小,贡献率在1.5%~2%之间,可忽略不计。结论提出了有效控制不确定度的措施,保证实验数据的可靠性,为准确表述土壤样品中重金属含量提供了参考。Objective To evaluate the uncertainty of determination of total cadmium(Cd),lead(Pb)and chromium(Cr)in soil by microwave digestion and inductively coupled plasma mass spectrometry(ICP-MS).Methods To ensure the accuracy and reliability of the detection results,the uncertainty of total cadmium(Cd),lead(Pb)and chromium(Cr)in soil was determined by microwave digestion and inductively coupled plasma mass spectrometry(ICP-MS)and according to JJF1059.1-2012 Evalution and Expression of Uncertainty in Measurement the synthetic uncertainty was calculated and the extended uncertainty was obtained.Results The main sources of uncertainty were the standard curve preparation the repeatability measurement of samples and the standard curve fitting the contribution rates to the uncertainty of Cd,Pb and Cr were 50.4%~60.3%,18.7%~26.1%and 12.1%~20.4%.The influence of sample weighing and resolution volume for the uncertainty was small and the contribution rate was between 1.5%~2%,which could be ignored.Conclusion The effective measures to control uncertainty were put forward,which ensured the reliability of the experimental data and provided the reference for the accurate representation of the heavy metal content in soil.

关 键 词：不确定度 电感耦合等离子体质谱法 微波消解 土壤 

分 类 号：X833[环境科学与工程—环境工程] O657.63[理学—分析化学]