X射线荧光光谱法测定纯镁中7种杂质元素  

Determination of 7 impurity elements in pure magnesium by X-ray fluorescence spectrometry

作　　者：瞿媛媛 白万里 QU Yuanyuan;BAI Wanli(Chinalco Test Science and Technology(Zhengzhou)Co.,Ltd.,Zhengzhou 450041,China)

机构地区：[1]中铝检测科技(郑州)有限公司,河南郑州450041

出　　处：《冶金分析》2024年第4期31-39,共9页Metallurgical Analysis

基　　金：国家标准制定项目(20220732-T-610)。

摘　　要：纯镁中杂质元素含量较低,主要包括Si、Fe、Cu、Al、Mn、Zn、Pb等,应用化学湿法测定时程序繁琐、测试周期长,应用火花放电原子发射光谱法虽可快速测定,但多类金属交叉测试时存在污染风险。试验采用铣床制备样品后快速测定,确立了X射线荧光光谱法(XRF)测定纯镁中Si、Fe、Cu、Al、Mn、Zn、Pb的分析方法。经标准样品分析,各元素测定值与标准值相吻合,有效解决了化学湿法分析测试周期长的问题和火花放电原子发射光谱法测定多类金属时交叉污染的问题。经实际样品分析及实验室间结果比对,0.0010%级别以上元素测定结果的相对标准偏差(RSD)在7%以下,方法具有良好重现性和广泛适用性。The impurity elements in pure magnesium mainly include Si,Fe,Cu,Al,Mn,Zn and Pb with low contents.The wet chemical method has some shortcomings such as complicated determination procedures and long test period.Although the spark discharge atomic emission spectrometry can be used for rapid determination,there is a risk of contamination when a variety of metals are cross-tested.In this study,the samples were prepared using milling machine followed by rapid determination.The analytical method for the determination of Si,Fe,Cu,Al,Mn,Zn and Pb in pure magnesium by X-ray fluorescence spectrometry(XRF)was established.The standard sample analysis results showed that the measured values of each element were consistent with the certified values.This method effectively solved the problem of long test period of wet chemical method as well as cross contamination in the determination of various metals by spark discharge atomic emission spectrometry.The actual sample analysis and inter-laboratory comparison results indicated that the relative standard deviation(RSD)of the determination results for elements with content above 0.0010% was less than 7%.The proposed method had good reproducibility and wide applicability.

关 键 词：纯镁 X射线荧光光谱法(XRF) 杂质元素 铣床 放置时间 实验室间比对 

分 类 号：O657.34[理学—分析化学]