双色散-双聚焦X射线光谱仪研制与特性研究

doi:10.3964/j.issn.1000-0593(2024)10-2827-07

Abstract
References
Related Citation (15)

Download: PDF (6558 KB)
Export: BibTeX | EndNote (RIS)

Abstract X-ray emission spectroscopy is an in situ non-destructive method to obtain chemical species of elements, and the development of laboratory-type XES devices worldwide is still in the exploratory stage. Energy-Dispersive X-Ray Fluorescence Spectrometer (EDXRF) and Wavelength-Dispersive X-Ray Fluorescence Spectrometer (WDXRF) are widely used in geological, environmental and archaeological fields. However, although EDXRF has a simple structure and can realize rapid, non-destructive detection of multiple elements, the resolution is not ideal, the spectral line interference is serious, and the detection limit is poor. Although WDXRF can distinguish most elements with spectral overlapping characteristics in conventional applications, the structure and cost are complicated. To explore the development of laboratory-type XES devices, this study synthesizes the performance advantages of the Dual Dispersions and Dural Focuses X-Ray Spectrometer (DDF-XRS) design concept and successfully develops the principle prototype. The experimental data and analysis results show that this DDF-XRS spectrometer combines the advantages of both micro EDXRF and WDXRF with a simple structure, good signal-to-noise ratio, high resolution, and low detection limit characteristics. Through the wavelength-energy double dispersion technology, X-rays are firstly diffracted by the crystal to undergo wavelength dispersion, thus obtaining monochromatic light, and at the same time, the energy dispersion of the silicon drift detector can be used to observe the degree of monochromaticity, reduce the risk of misjudgment of spectral line interference, and improve the accuracy and reliability of the analysis results, which overcomes the limitations of the complex structure for WDXRF and the insufficient energy resolution of the EDXRF, and highlights the necessity and superiority of the double dispersion. This technology overcomes the limitations of WDXRF multi-element peak determination and EDXRF energy resolution, emphasizing the necessity and superiority of double dispersion. At present, the resolution of the DDF-XRS spectrometer is 45 eV, which can reduce the spectral line overlap of transition metal K_β to K_α peaks; at the same time, it significantly reduces the background of the continuum spectrum, and the optimal signal-to-noise ratio is >1 000; and the detection limit of Cr in the determination of geologic samples can be up to 0.26 mg·kg^-1. With the application of DDF-XRS, the transition metal K_α1 and K_α2 spectral lines can be resolved to a certain extent, and it is expected that the resolution can be further improved by combining with linear or two-dimensional array detectors to realize the determination of X-ray emission fingerprint spectra to obtain the chemical forms of the analyzed elements. Since the current crystal properties cannot fully resolve the overlapping spectral lines of transition metals, the search for curved crystals with high fractionation capacity and diffraction intensity will be the next research focus.

Key words：X-ray fluorescence; Bent crystal; Curved crystal; Resolution; Detection limit; Wavelength dispersion; Energy dispersion

Received: 2023-08-11 Accepted: 2024-01-23

ZTFLH:

O657.34

Corresponding Authors: LUO Li-qiang E-mail: luoliqiang@cags.ac.cn

Cite this article:

SHEN Ya-ting,HAN Ling-yun,CHEN Jun-ru, et al. Research and Characterization of Laboratory Dual Dispersions and Dural Focuses X-Ray Fluorescence Spectrometer Instrument Development[J]. SPECTROSCOPY AND SPECTRAL ANALYSIS, 2024, 44(10): 2827-2833.

URL:

https://www.gpxygpfx.com/EN/10.3964/j.issn.1000-0593(2024)10-2827-07 OR https://www.gpxygpfx.com/EN/Y2024/V44/I10/2827

[1] Boman J, Langer M, Pei X, et al. X-Ray Spectrometry, 2023, 52(6): 447.
[2] Chubarov Victor M, Maltsev Artem S, Amosova Alena A, et al. X-Ray Spectrometry, 2023, doi: 10.1002/XYS.3384.
[3] Lilek Nataša, Kandolf Borovšak Andreja, Bertoncelj Jasna, et al. X-Ray Spectrometry, 2022, 51(3): 186.
[4] Rotich Nelson K, Gatari Michael J, Kareru Patrick, et al. X-Ray Spectrometry, 2023, 52(2): 83.
[5] Bábek Ondǐej, Fačevicová Kamila, Žídek Martin, et al. Journal of Geochemical Exploration. 2022, 243: 107106.
[6] DUAN Wen，SHI You-chang(段文, 石友昌). Rock and Mineral Analysis(岩矿测试)，2023，42(1): 72.
[7] Gong Yuwu, Xiong Yingfei, Wang Enyuan, et al. X-Ray Spectrometry, 2023, 52(2): 62.
[8] Wolfs Sandra, Dekkers Rob. X-Ray Spectrometry, 2023, 52(2): 52.
[9] Arora H, Abhilash S R, Umapathy G R, et al. Vacuum, 2022, 201: 111052.
[10] LIU Mei(刘妹). Rock and Mineral Analysis(岩矿测试)，2023，42(3): 445.
[11] FANG Peng-da, ZHANG Li-juan, WANG Jia-song, et al(方蓬达，张莉娟，王家松，等). Rock and Mineral Analysis(岩矿测试)，2023，42(2): 411.
[12] Tambuzzi Stefano, Bonizzoni Letizia, Francesco Di Paola, et al. X-Ray Spectrometry, 2024, 53(2): 112.
[13] Carapelle Alain, Lejeune Gary, Morelle Mathieu, et al. X-Ray Spectrometry, 2022, 51(4): 388.
[14] LUO Li-qiang, ZHAN Xiu-chun, LI Guo-hui(罗立强，詹秀春，李国会). X-Ray Fluorescence Spectrometry(X射线荧光光谱分析). 3rd Edition)（第3版）. Beijing: Chemical Industrial Press(北京：化工出版社)，2023.
[15] Li Xiaoli, Yu Zhaoshui, Xu Jinli, et al. X-Ray Spectrometry, 2023, 52(1): 2.
[16] Seidler G T, Mortensen D R, Remesnik A J, et al. Rev. Sci. Instrum., 2014, 85(11): 113906.
[17] Afshari M, Krumey P, Menn D, et al. Structural Dynamics, 2020, 7: 014301.
[18] Jahrman Evan P, Seidler Gerald T, Sieber John R. Analytical Chemistry, 2018; 90(11): 6587.
[19] Honkanen Ari-Pekka, Ollikkala Sami, Ahopelto Taru, et al. Rev. Sci. Instrum., 2019, 90(3): 033107.
[20] Jahrman Evan P, Holden William M, Ditter Alexander S, et al. Rev. Sci. Instrum., 2019, 90(2): 024106.
[21] Kowalska Joanna K, Lima Frederico A, Pollock Christopher J, et al. Israel Journal of Chemistry，2016，56(9-10): 803.
[22] Nowak S H, Armenta R, Schwartz C P, et al. Rev. Sci. Instrum., 2020, 91(3): 033101.
[23] Szlachetko J, Nachtegaal M, De Boni E, et al. Rev. Sci. Instrum., 2012, 83(10): 103105.
[24] Owens Alan. Journal of Synchrotron Radiation, 2006, 13(2): 143.
[25] Lechner P, Pahlke A, Soltau H. X-Ray Spectrometry, 2004, 33(4): 256.
[26] Kavčič M, Budnar M, Mühleisen A, et al. Rev. Sci. Instrum., 2012, 83(6): 069901.
[27] LUO Li-qiang, SHEN Ya-ting, MA Yan-hong, et al(罗立强，沈亚婷，马艳红，等). Spectroscopy and Spectral Analysis(光谱学与光谱分析), 2017, 37(4): 1003.