X射线荧光光谱法测定纯铜中微量杂质元素

X-ray fluorescence spectrometry for the determination of trace impurity elements in pure copper

对X射线荧光光谱法测定纯铜中微量杂质元素的实验条件,背景和光谱重叠干扰及校正进行研究。通过以纯铜标准样品绘制校准曲线,采用专用空白试样测量背景强度,多项式(多点)拟合计算峰底背景,专用的标准样品计算与分析线的重叠干扰量并加以校正,理论α系数法或基本参数法校正样品中元素间的吸收-增强效应,选择高反射率的人工晶体PX-10测定部分重金属痕量元素,成功地用X射线荧光光谱法测定纯铜中微量杂质元素。样品的分析结果与推荐值或火花源原子发射光谱的测定值符合,回收率在95%～102%范围,各元素的相对标准偏差(RSD)均小于5.0%。

A quantitative analysis method for the determination of trace impurity elements in pure copper by X-ray fluorescence spectrometry was established. In this study, the calibration curve was created with standard sample of pure copper. The peak base background was calculated with background strength of blank samples by multinomial （multiple-point） background method. The spectral overlapping interferences were calculated and corrected with special standard samples. The absorption and en- hancement effects among elements were corrected by using theoretical α coefficient method and fundamental parameter method. The artificial tens PX-10 with high reflection index was used to determine some trace heavy metal elements. The analytical results of this method were consistent with those of spark source atomic emission spectrometry. The recoveries were in the range of 95%-102%, and the relative standard deviations （RSD） were less than 5.0%.