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生态环境监测工作中应用AAS/AFS和XRF法测定土壤重金属数据质量评价 预览

Evaluation of Data Quality on the Detection of Heavy Metals in Soils by Atomic Absorption Spectrometry or Atomic Fluorescence Spectrometry and X-ray Fluorescence Spectrometry in Ecological Environment Monitoring
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摘要 当前我国生态环境监测工作中,测定土壤重金属等无机元素全量所采用的标准方法主要为原子吸收光谱法(AAS)、原子荧光光谱法(AFS)和波长色散X射线荧光光谱法(WDXRF)等。为掌握AAS、AFS和WDXRF等方法测试结果的有效性和可比性,本文选取了20个来自全国不同区域、不同类型的实际土壤样品,通过盲样方式插入国家土壤环境监测任务样品批次中,分发至3~5个实验室,采用AAS/AFS、WDXRF和便携式X射线荧光光谱法(p-XRF)平行测定Cr、Ni、Cu、Zn、As、Hg、Cd、Pb、V和Mn十个元素全量。结果表明:元素含量水平分布均匀(在≤1.0、1.0~2.0、2.0~10.0及>10.0水平均有分布);85%以上样品Cr、Ni、Cu、Zn和Pb元素WDXRF方法的实验室间相对偏差(RD)更理想,60%样品As元素AFS方法的RD更优,元素含量对WDXRF方法的RD有更明显影响。总体上,AAS/AFS和WDXRF两类方法实验室间精密度控制水平均较高,WDXRF法更理想。进一步分析AAS/AFS和WDXRF方法间平行性(以这两类方法测试结果的相对偏差RD’进行评价),Cr、Ni、Cu和Zn元素的RD’基本低于20%,As和Pb元素80%以上的RD’低于20%,Pearson相关性和线性关系分析表明这两类方法有较高的可比性;另外,Cr、Ni、Cu、Zn、Pb和As元素的p-XRF与AAS/AFS方法测试结果也有较理想的可比性。本研究认为,AAS/AFS和WDXRF两类方法具有等同测试效果,实际监测工作中Cd、Hg等含量较低元素宜选择检出限较低的AAS/AFS法;因WDXRF方法的前处理过程简单易控,大批量土壤分析中使用该方法更加高效,在特定实验条件下p-XRF方法也有可接受的定量效果。 BACKGROUND: In current ecological environmental monitoring, the standard methods used to determine the total contents of inorganic elements, such as heavy metals in soil, include atomic absorption spectrometry(AAS), atomic fluorescence spectrometry(AFS) and wavelength dispersive X-ray fluorescence spectrometry(WDXRF).OBJECTIVES: To evaluate the quality, validity and mutual comparability of the results obtained by different analytical methods.METHODS: Twenty actual soil samples of different types from different regions in China were selected and inserted into the national soil environmental monitoring sample batch blind, and sent to 3-5 laboratories. AAS/AFS, WDXRF and portable X-ray fluorescence spectrometry(p-XRF) were used to determine the total amount of Cr, Ni, Cu, Zn, As, Hg, Cd, Pb, V and Mn in parallel.RESULTS: The content of these elements was equally distributed at levels of ≤1.0, 1.0-2.0, 2.0-10.0, and 10.0. The results show that 85% samples had better inter-laboratory relative deviation(RD) of the WDXRF method in terms of Cr, Ni, Cu, Zn and Pb. On the other hand, 60% samples had better RD using AFS method for the As determination. Element content had more obvious effect on RD for WDXRF method. Generally, the inter-laboratory precision control was good for both AAS/AFS and WDXRF methods, and the WDXRF method was more desirable. Through further analysis of the parallelism between AAS/AFS and WDXRF methods(evaluated as the relative deviation RD’ of the analytical results of these two methods), it showed that almost all the RD’ of Cr, Ni, Cu and Zn was less than 20%, and more than eighty percent RD’ of As and Pb was less than 20%. The results of Pearson correlation and linear relationship analysis also show that the analytical results of two methods were highly comparable. Additionally, there was also good comparability between the results of AAS/AFS and p-XRF methods for determination of Cr, Ni, Cu, Zn, Pb and As.CONCLUSIONS: AAS/AFS method and WDXRF method have equivalent test results. In actual
作者 田志仁 封雪 姜晓旭 李宗超 李妤 夏新 TIAN Zhi-ren;FENG Xue;JIANG Xiao-xu;LI Zong-chao;LI Yu;XIA Xin(State Environmental Protection Key Laboratory of Quality Control in Environmental Monitoring, China National Environmental Monitoring Centre, Beijing 100012, China;University of Science and Technology Beijing, Beijing 100083, China)
出处 《岩矿测试》 CAS CSCD 北大核心 2019年第5期479-488,共10页 Rock and Mineral Analysis
基金 国家重点研发计划项目“土壤高精度多参数现场快速检测系统集成与应用示范”(2017YFF0108204).
关键词 土壤 重金属元素 原子吸收光谱法 原子荧光光谱法 波长色散X射线荧光光谱法 便携式X射线荧光光谱法 相对偏差 soil heavy metal elements atomic absorption spectrometry atomic fluorescence spectrometry wavelength dispersive X-ray fluorescence spectrometry portable X-ray fluorescence spectrometry relative deviation
作者简介 田志仁,硕士,工程师,从事土壤环境监测工作。E-mail:1731427795@qq.com;通信作者:夏新,博士,研究员,从事土壤环境监测工作。E-mail:13811875524@163.com。
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