X射线荧光光谱法测定纯镁中7种杂质元素

doi:10.13228/j.boyuan.issn1000-7571.012304

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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,0.001 0%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。

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	瞿媛媛
	白万里

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

Abstract：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 0.001 0% was less than 7%. The proposed method had good reproducibility and wide applicability.

Key words： pure magnesium X-ray fluorescence spectrometry(XRF) impurity element milling machine placement time inter-laboratory comparison

收稿日期: 2023-08-21

ZTFLH:

O657.34

基金资助:国家标准制定项目(20220732-T-610)

通讯作者: 白万里(1986-),男,高级工程师,硕士,主要从事冶金材料分析工作;E-mail:zyy_bwl@rilm.com.cn

作者简介: 瞿媛媛(1996-),女,工程师,硕士,主要从事冶金分析及材料性能表征工作;E-mail:18811633606@163.com

引用本文:

瞿媛媛, 白万里. X射线荧光光谱法测定纯镁中7种杂质元素[J]. 冶金分析, 2024, 44(4): 31-39. QU Yuanyuan, BAI Wanli. Determination of 7 impurity elements in pure magnesium by X-ray fluorescence spectrometry. , 2024, 44(4): 31-39.

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http://yjfx.chinamet.cn/CN/10.13228/j.boyuan.issn1000-7571.012304 或 http://yjfx.chinamet.cn/CN/Y2024/V44/I4/31

[1] 吴国华,陈玉狮,丁文江.镁合金在航空航天领域研究应用现状与展望[J].载人航天,2016,22(3):281-292.
WU Guohua,CHEN Yushi,DING Wenjiang.Current research,application and future prospect of magnesium alloys in aerospace industry[J].Manned Spaceflight,2016,22(3):281-292.
[2] 康鸿跃,陈善华,马永平,等.镁合金在军事装备中的应用[J].金属世界,2008(1):61-64.
KANG Hongyue,CHEN Shanhua,MA Yongping,et al.Applications of magnesium alloys in military equipment[J].Metal World,2008(1):61-64.
[3] 刘世杰,唐伟能.镁合金在轨道交通领域的应用[J].金属制品,2023,49(3):67-72.
LIU Shijie,TANG Weineng.Application of magnesium alloy in rail transit[J].Metal Products,2023,49(3):67-72.
[4] 谭军,王芳磊,蒋斌,等.镁合金结构材料应用现状与展望[J].自然杂志,2023,45(2):93-105.
TAN Jun,WANG Fanglei,JIANG Bin,et al.Application status and prospects of magnesium alloy structural materials[J].Chinese Journal of Nature,2023,45(2):93-105.
[5] 杨成选.合金铸铁的X射线荧光光谱分析[J].光谱实验室,1998,15(3):70-74.
YANG Chengxuan.XRF analysis of alloy cast iron[J].Chinese Journal of Spectroscopy Laboratory,1998,15(3):70-74.
[6] 师世龙.XRF法测定锌合金中的铝[J].光谱实验室,2006,23(1):96-98.
SHI Shilong.Determination of aluminum in zinc alloy by XRF[J].Chinese Journal of Spectroscopy Laboratory,2006,23(1):96-98.
[7] 王广西,葛良全,罗良红,等.波长色散X 射线荧光光谱法快速测定铂铑合金中铂和铑的含量[J].核技术,2016,39(1):17-22.
WANG Guangxi,GE Liangquan,LUO Lianghong,et al.Rapid determination of platinum and rhodium in Pt-Rh alloy by wavelength dispersive X-ray fluorescence spectrometry[J].Nuclear Techniques,2016,39(1):17-22.
[8] 张文诚,曹吉祥,张爽.X 射线荧光光谱法测定易切削不锈钢中铅碲铋[J].冶金分析,2019,39(3):38-43.
ZHANG Wencheng,CAO Jixiang,ZHANG Shuang.Determination of lead,tellurium and bismuth in free-cutting stainless steel by X-ray fluorescence spectrometry[J].Metallurgical Analysis,2019,39(3):38-43.
[9] 李辉,张庸,刘喜山.金属材料分析国内外标准中波长色散X射线荧光光谱法的应用[J].理化检验(化学分册),2020,56(3):363-372.
LI Hui,ZHANG Yong,LIU Xishan.On the application of wavelength-dispersive X-ray fluorescence spectrometry to some domestic and foreign standards for metal analysis[J].Physical Testing and Chemical Analysis(Part B:Chemical Analysis),2020,56(3):363-372.
[10] 周素莲,黄肇敏,崔萍萍.X射线荧光光谱法测定铝合金及纯铝中痕量元素[J].理化检验(化学分册),2009,45(4):474-475,479.
ZHOU Sulian,HUANG Zhaomin,CUI Pingping.XRFS determination of trace elements in aluminum alloys and pure aluminum[J].Physical Testing and Chemical Analysis(Part B:Chemical Analysis),2009,45(4):474-475,479.
[11] 童晓民,韩菲,朱智,等.铸造铝合金样品的X射线荧光光谱分析[J].岩矿测试,2003,22(4):303-306.
TONG Xiaomin,HAN Fei,ZHU Zhi,et al.Analysis of ZL205A alloy by X-ray fluorescence spectrometry[J].Rock and Mineral Analysis,2003,22(4):303-306.
[12] 张祥,陆晓明,张毅.X射线荧光光谱法测定变形铝合金中合金元素的影响因素探讨[J].冶金分析,2023,43(5):10-16.
ZHANG Xiang,LU Xiaoming,ZHANG Yi.Discussion on influencing factor on determination of alloying element in wrought alloy by X-ray fluorescence spectrometry[J].Metallurgical Analysis,2023,43(5):10-16.
[13] DE Boer.Fundamental parameters for X-ray fluorescence analysis[J].Spectrochimica Acta,1989,44B(11):1171-1190.
[14] 吉昂,陶光仪,卓尚军,等.X射线荧光光谱分析[M].北京:科学出版社,2003:227.
[15] 国家质量监督检验检疫总局,中国国家标准化管理委员会.GB/T 13748.10—2013镁及镁合金化学分析方法第10部分:硅含量的测定钼蓝分光光度法[S].北京:中国标准出版社,2013.
[16] 国家质量监督检验检疫总局,中国国家标准化管理委员会.GB/T 13748.20—2009镁及镁合金化学分析方法第20部分:ICP-AES测定元素含量[S].北京:中国标准出版社,2009.
[17] 王勇,李子敬,刘林,等.微波消解-电感耦合等离子体原子发射光谱法测定钛及钛合金中19种元素[J].冶金分析,2023,43(5):86-94.
WANG Yong,LI Zijing,LIU Lin,et al.Determination of 19 elements in titanium and titanium alloy by microwave digestion-inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2023,43(5):86-94.