能量色散X射线荧光光谱仪测定PM_(2.5)中重金属方法的建立与应用
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摘要
由于商品化的空气颗粒物薄膜标准样品较少,限制了X射线荧光技术在PM_(2.5)中金属分析的应用。为建立能量色散X射线荧光光谱法(EDXRF)分析PM_(2.5)中金属元素(Al、K、Ti、Mn、Fe、Ni、Cu、Zn和Pb)的实验方法,采集一系列不同浓度的PM_(2.5)实际样品作为标准样品,消解后上ICP-MS分析,以其测得结果为标准值,建立EDXRF校准曲线,各元素线性相关系数r为0.9577～0.9986。EDXRF方法检出限为5～64ng/cm~2,重复测定RSD为0.1%～2.0%。最后用建立的方法测定实际样品,并和ICP-MS的结果比较,两种仪器的结果相对偏差为0%～12%。本实验提供了一种简单易得的标准样品获取方法,以此建立的EDXRF分析方法快速可靠。
The scarcity of commercial air particulate filter standards limits the application of X-ray fluorescence in the determination of metals in PM_(2.5). To establish a method for determination of metal elements(Al, K, Ti, Mn, Fe, Ni, Cu, Zn and Pb) in PM_(2.5) using Energy dispersive X-ray fluorescence spectroscopy(EDXRF), serial filter samples of different concentration are used as standards. Correlation coefficients of calibration are 0.9577～0.9986. Detection limits of EDXRF are 5～64 ng/cm~2, and RSDs of replication are 0.1 %～2.0 %. After the method is established, a few more samples are collected, analyzed by EDXRF and ICP-MS, the relative deviations of the two methods are 0 %～12 %. The study offers an easy way of standard acquisition, which is practical and reliable for X-ray fluorescence analysis.
The scarcity of commercial air particulate filter standards limits the application of X-ray fluorescence in the determination of metals in PM_(2.5). To establish a method for determination of metal elements(Al, K, Ti, Mn, Fe, Ni, Cu, Zn and Pb) in PM_(2.5) using Energy dispersive X-ray fluorescence spectroscopy(EDXRF), serial filter samples of different concentration are used as standards. Correlation coefficients of calibration are 0.9577～0.9986. Detection limits of EDXRF are 5～64 ng/cm~2, and RSDs of replication are 0.1 %～2.0 %. After the method is established, a few more samples are collected, analyzed by EDXRF and ICP-MS, the relative deviations of the two methods are 0 %～12 %. The study offers an easy way of standard acquisition, which is practical and reliable for X-ray fluorescence analysis.
引文
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[2]刘旭辉,郭建娥,马利刚,等.2016年太原市空气PM2.5中重金属元素来源分析[J].预防医学论坛,2017,23(8):564-567.
[3]赵莉斯,于瑞莲,徐玲玲,等.厦门海沧区PM2.5中金属元素污染评价及来源分析[J].环境科学,2017,38(10):4061-4070.
[4]中华人民共和国国家环境保护标准.HJ 829-2017.环境空气颗粒物中无机元素的测定能量色散X射线荧光光谱法及其编制说明[S].北京:中华人民共和国环境保护部.2017.
[5]何文权,叶伯明.能量色散X射线荧光光谱分析大气颗粒中多种元素[J].岩矿测试,2002,21(4):301-303.
[6]吉昂,郑南,王河锦,等.高能偏振能量色散-X射线荧光光谱法测定PM10大气颗粒物的组成[J].岩矿测试,2011,30(5):528-535.