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[X射线荧光光谱法同时测定大气颗粒物样品中的多种元素]

[Simultaneous determination of multiple elements in airborne particulate samples by X-ray fluorescence spectrometry].

作者信息

Takada T, Hitosugi M, Kadowaki T, Kudo M

出版信息

Sangyo Igaku. 1983 Jul;25(4):235-44. doi: 10.1539/joh1959.25.235.

DOI:10.1539/joh1959.25.235
PMID:6663820
Abstract

An energy dispersive X-ray fluorescence spectrometer (EDX) has been applied to determine multielements in the workplace air. The standards for X-ray fluorescence analysis were prepared by the chelate precipitation method on polyvinyl chloride (PVC) membrane filter. And, the specimens were prepared to deposit various metal compounds of different chemical forms by the suspension method on PVC membrane filter, and they were determined with EDX and atomic absorption spectrometer (AAS). The results obtained were as follows. Though there is a difference by each element, an amount less than 3 microgram/cm2 per unit area makes it possible to undergo multielement analysis, that is, is has no influence on fine particle effect (particle size; under 5 microns). Then, effects of the X-ray intensity by different chemical forms are negligible. At the presence the neighboring element and other elements this technique showed greater precision by carrying out on corrective treatment, etc. The coefficient of variation of this technique was in the range of 2.5-6.5% at DDTC-Cu of 0.5-5.0 micrograms/cm2, with the limit of detection for As : 0.002 microgram/cm2, Zn : 0.003 microgram/cm2, Pb : 0.003 microgram/cm2, Cu : 0.004 microgram/cm2, Ni : 0.003 microgram/cm2, Fe : 0.005 microgram/cm2, Mn : 0.008 microgram/cm2, Cr : 0.013 microgram/cm2, respectively. Aerosols collected at the workplace were analyzed with EDX and AAS, and the obtained results showed good agreement with such regression line as y = 1.04 chi + 0.04, the coefficient of correlation being r = 0.995. From these results, this technique was found to be a very excellent method for monitoring of multielements in the workplace air.

摘要

能量色散X射线荧光光谱仪(EDX)已被用于测定工作场所空气中的多种元素。通过在聚氯乙烯(PVC)膜滤器上采用螯合沉淀法制备X射线荧光分析标准物质。并且,通过悬浮法在PVC膜滤器上制备标本,以沉积不同化学形式的各种金属化合物,然后用EDX和原子吸收光谱仪(AAS)进行测定。得到的结果如下。尽管每种元素存在差异,但单位面积小于3微克/平方厘米的量使得进行多元素分析成为可能,也就是说,对细颗粒效应(粒径;小于5微米)没有影响。然后,不同化学形式对X射线强度的影响可以忽略不计。在存在相邻元素和其他元素的情况下,通过进行校正处理等,该技术显示出更高的精度。在二乙基二硫代氨基甲酸钠-铜含量为0.5-5.0微克/平方厘米时,该技术的变异系数在2.5-6.5%范围内,砷的检测限为0.002微克/平方厘米,锌为0.003微克/平方厘米,铅为0.003微克/平方厘米,铜为0.004微克/平方厘米,镍为0.003微克/平方厘米,铁为0.005微克/平方厘米,锰为0.008微克/平方厘米,铬为0.013微克/平方厘米。对在工作场所收集的气溶胶用EDX和AAS进行分析,得到的结果与y = 1.04x + 0.04这样的回归线显示出良好的一致性,相关系数r = 0.995。从这些结果来看,该技术被发现是一种用于监测工作场所空气中多种元素的非常出色的方法。

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