国产顺序扫描式波长色散X射线荧光光谱仪在铁基合金分析中的应用  

Application of domestric sequential scanning wavelength dispersive X-ray fluorescence spectrometer in analysis of iron-based alloy

作　　者：刘明博 王英倩 倪子月 李冬玲[1,2] 沈学静 王海舟[1,2] LIU Mingbo;WANG Yingqian;NI Ziyue;LI Dongling;SHEN Xuejing;WANG Haizhou(Central Iron and Steel Research Institute Co.,Ltd.,Beijing 100081,China;NCS Testing Technology Co.,Ltd.,Beijing 100081,China)

机构地区：[1]钢铁研究总院有限公司,北京100081 [2]钢研纳克检测技术股份有限公司,北京100081

出　　处：《冶金分析》2023年第1期1-7,共7页Metallurgical Analysis

基　　金：国家重点研发计划基础科研条件与重大科学仪器设备研发专项(2022YFF0707300)。

摘　　要：为了拓展自主研发的顺序扫描式波长色散X射线荧光光谱仪(WDXRF)在铁基合金检测领域的应用,通过对测试条件、谱线干扰方法、强度表征方法、基体校正方法等的研究,开发了覆盖多种类型铁基合金样品,可以对16种常用元素成分进行直接快速分析的方法。实验采用铣床对样品进行表面处理,对各待测元素设定合适的条件并进行所有样品的测试,然后在软件中分别用经验系数法和Alpha系数法进行工作曲线绘制,并采用估计标准误差(SEE)作为曲线质量评定依据,通过SEE值的大小确定各元素的基体校正方法,最后选取典型样品进行了方法重复性和正确度的考察。结果显示,无论对于常量元素Fe、Cr、Ni、Mn,还是微量元素Al、Si、P、S、Ti、V、Co、Cu、Zr、Nb、Mo、W,实验方法都有较好的正确度、精密度以及检出限,并有较宽的测试范围。研究表明,在铁基合金分析领域,实验方法能够满足日常测试分析的需求。In order to expand the application of self-developed sequential scanning wavelength dispersive X-ray fluorescence spectrometer in testing of iron-based alloys,the method for direct and rapid analysis of 16 common elements was developed.The proposed method could cover various types of iron-based alloy samples.The measurement conditions,spectral interference correction,intensity characterization and matrix correction methods were investigated.The surface of sample was treated in experiments using milling machine.Proper conditions were set for each element in the analysis of samples.Then the working curves were prepared in software by experiential coefficient method and Alpha coefficient method,respectively.The standard error of estimate(SEE)was adopted as the evaluation basis of curve quality.The matrix correction methods of elements were confirmed through the values of SEE.Finally,the repeatability and trueness were investigated by selecting typical samples.The results showed that the proposed method had good trueness,precision and limit of detection whether for major elements(Fe,Cr,Ni and Mn)or minor elements(Al,Si,P,S,Ti,V,Co,Cu,Zr,Nb,Mo and W).Moreover,the determination range was wide.The experimental results indicated that the proposed method could meet the requirements of routine testing in the analysis field of iron-based alloys.

关 键 词：波长色散X射线荧光光谱(WDXRF) 铁基合金 Alpha系数法 经验系数法 估计标准误差(SEE) 

分 类 号：O657.34[理学—分析化学] TF125.13[理学—化学]