X射线荧光光谱镶嵌制样无标测定不锈钢  

Determination of stainless steel by mosaic sample preparation combined with standardless X-ray fluorescence spectrometry

作　　者：安晓娇[1] 马贤 刘涛[1,2] 王筠 AN Xiaojiao;MA Xian;LIU Tao;WANG Jun(Institute of Physical and Chemical Engineering of Nuclear Industry,Tianjin 300180,China;Science and Technology on Particle Transport and Separation Labortory,Tianjin 300180,China)

机构地区：[1]核工业理化工程研究院,天津300180 [2]粒子输运与富集技术国防科技重点实验室,天津300180

出　　处：《冶金分析》2022年第2期15-20,共6页Metallurgical Analysis

摘　　要：样品制备是X射线荧光光谱(XRF)分析测试的首要步骤,样品制备成功与否直接影响测试结果准确性。以不锈钢为例,对尺寸不满足直接进行XRF测试的样品,利用镶嵌法进行制样,并采用XRF无标定量方法分析不锈钢中Fe、Cr、Mn、Ni、Cu、Si、Co、V、Mo等元素。利用镶嵌法研究了样品尺寸对测试结果的影响,发现以测试主次成分Fe、Cr、Ni、Mn含量为主要目标时,样品覆盖光斑面积应达到25%以上,测试元素相对误差普遍低于1.5%,微量元素(除Si外)相对误差均在5.2%以内,满足测试要求。通过无标定量法测试不锈钢标准样品,发现方法对不锈钢中主次元素Fe、Cr、Ni均可实现准确测量,相对误差不大于1.6%,微量元素中Si和Cu元素的相对误差在5.0%以内。通过镶嵌法制样无标定量测定实际样品,并与化学法对比,进一步证实XRF可实现对非标准尺寸不锈钢样品的快速测量。镶嵌法制样XRF无标定量方法亦可推广到其他合金产品分析。Sample preparation is the first and key step for analysis and testing by X-ray fluorescence spectrometry(XRF).The success of sample preparation or not directly affects the accuracy of measurement results.Stainless steel was selected as an example in the study.For the sample with size that did not meet the requirements for direct XRF testing,the mosaic sample preparation was employed.The elements including Fe,Cr,Mn,Ni,Cu,Si,Co,V and Mo in stainless steel were quantitatively analyzed by standardless XRF.The influence of sample size on the testing results was studied by the mosaic method.It was found that for the main targets of major and minor components including Fe,Cr,Ni and Mn,when more than 25%of spot area was covered by the sample,the relative errors of testing elements were commonly less than 1.5%,and the relative errors of microelements(except for Si)were within 5.2%,which could meet the testing requirements.Through quantitative standardless analysis of standard sample of stainless steel,it was found that the major and minor elements of Fe,Cr and Ni in stainless steel could be accurately determined by the proposed method.The relative errors were not more than 1.6%.The relative errors of Si and Cu in microelements were within 5.0%.The actual samples were quantitatively determined by mosaic method without standards.Through the comparison with chemical method,it was further confirmed that the non-standard size stainless steel samples could be rapidly measured by XRF.The quantitative analysis method of mosaic sample preparation combined with X-ray fluorescence spectrometry without standards could be also extended to other alloy products.

关 键 词：X射线荧光光谱(XRF) 无标分析 镶嵌制样 不锈钢 样品尺寸 

分 类 号：O657.34[理学—分析化学] TF764.1[理学—化学]