Determination of stainless steel by mosaic sample preparation combined with standardless X-ray fluorescence spectrometry
AN Xiaojiao1, MA Xian1, LIU Tao1,2, WANG Jun1
1. Institute of Physical and Chemical Engineering of Nuclear Industry,Tianjin 300180,China; 2. Science and Technology on Particle Transport and Separation Labortory,Tianjin 300180,China
Abstract: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.
安晓娇, 马贤, 刘涛, 王筠. X射线荧光光谱镶嵌制样无标测定不锈钢[J]. 冶金分析, 2022, 42(2): 15-20.
AN Xiaojiao, MA Xian, LIU Tao, WANG Jun. Determination of stainless steel by mosaic sample preparation combined with standardless X-ray fluorescence spectrometry. , 2022, 42(2): 15-20.
[1] 罗立强,詹秀春,李国会. X射线荧光光谱分析 [M].2版.北京:化学工业出版社,2015:234-268. [2] 殷惠民,杜祯宇,任立军,等. 波长色散X射线荧光光谱谱线重叠和基体效应校正系数有效性判断及在土壤、沉积物重金属测定中的应用[J].冶金分析,2018,38(1):1-11. YIN Huimin,DU Zhenyu,REN Lijun,et al.Coefficient effectiveness judgment of overlapping line and matrix effect correction in wavelength dispersive X-ray fluorescence spectrometry and its application in determination of heavy metal elements in soil and sediment sample[J].Metallurgical Analysis,2018,38(1):1-11. [3] 李文翠,于湛,付玉,等. 应用XRF和ICP-MS研究陨石样品的元素分布[J].光谱学与光谱分析,2018,38(10):3261-3263. LI Wencui,YU Zhan,FU Yu,et al.Study on element distribution in meteorite samples by XRF and ICP-MS[J].Spectroscopy and Spectral Analysis,2018,38(10):3261-3263. [4] 王志刚,李凤全.城市灰尘中Pb的X射线荧光光谱半定量分析[J].光谱实验室,2007,24(4):652-655. WANG Zhigang,LI Fengquan.Semi-quantitative analysis Pb for urban dust by XRF[J].Chinese Journal of Spectroscopy Laboratory,2007,24(4):652-655. [5] 马成新,史小华,丁友明.基于无标样分析软件的X射线荧光光谱法测定金刚石刀头成分[J].冶金分析,2021,41(2):30-33. MA Chengxin,SHI Xiaohua,DING Youming.Determination of diamond knife head composition by X-ray fluorescence spectrometry based on analysis software without standard sample[J].Metallurgical Analysis,2021,41(2):30-33. [6] 张凯歌,谢福春,苏丹. X射线荧光光谱法无标分析测定不规则金属材料中主次量元素[J].吉林地质,2016,35(4):112-114. ZHANG Kaige,XIE Fuchun,SU Dan.Determination of major and minor elements in irregular metallic materials by X-ray fluorescence spectrometry[J].Jinlin Geology,2016,35(4):112-114. [7] 朱志秀,冯健,李晨,等.X射线荧光光谱无标样分析技术在出入境矿产品检验中的应用[J].理化检验(化学分册),2009,45(7):832-835. ZHU Zhixiu,FENG Jian,LI Chen,et al.Application of XRFS without using standard samples to inspection of mineral products in exits and entrances at customs[J].Physical Testing and Chemical Analysis(Part B:Chemical Analysis),2009,45(7):57-60. [8] 于丽丽,汤玉和,肖飞燕,等.X射线荧光光谱无标定量测定稀土矿石中五氧化二磷[J].冶金分析,2017,37(1):57-60. YU Lili,TANG Yuhe,XIAO Feiyan,et al.Determination of phosphorus pentoxide in rare earth ore by X-ray fluorescence spectrometry coupled with standard-less quantitative analysis[J].Metallurgical Analysis,2017,37(1):57-60. [9] 张红菊,张丁非,余大亮,等. X射线荧光光谱无标样分析在轻合金中的应用[J].分析试验室,2017,36(2):147-149. ZHANG Hongju,ZHANG Dingfei,YU Daliang,et al.Application of X-ray fluorescence spectrometer in the determination of light alloys[J].Chinese Journal of Analysis Laboratory,2017,36(2):147-149. [10] 苏丹.X射线荧光光谱法无标样分析测定粉煤灰中主次量元素[J].湖南有色金属,2016,32(3):76-78. SU Dan.Standardless analysis and determination of the major and minor elements in fly ash via X-ray fluorescence spectrometry[J].Hunan Nonferrous Metals,2016,32(3):76-78. [11] 窦怀智,洪华,王红卫,等.波长色散X射线荧光光谱无标分析法检测树脂中的铅[J].化学分析计量,2014,23(3):14-17. DOU Huaizhi,HONG Hua,WANG Hongwei,et al.Determination of lead in resin by wavelength dispersive X-ray fluorescence spectrometry with standard-sample-free quantitative analysis[J].Chemical Analysis and Meterage,2014,23(3):14-17.