Determination of Major and Rare Earth Elements in Rare Earth Ores by X-ray Fluorescence Spectrometry with Fusion Sample Preparation

Wei ZHOU; Meng ZENG; Jian WANG; Lei ZHANG; Ying-chun LI

doi:10.15898/j.cnki.11-2131/td.201706280113

2018 Vol. 37, No. 3

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Article navigation > Rock and Mineral Analysis > 2018 > 37(3): 298-305

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Wei ZHOU, Meng ZENG, Jian WANG, Lei ZHANG, Ying-chun LI. Determination of Major and Rare Earth Elements in Rare Earth Ores by X-ray Fluorescence Spectrometry with Fusion Sample Preparation[J]. Rock and Mineral Analysis, 2018, 37(3): 298-305. doi: 10.15898/j.cnki.11-2131/td.201706280113

Citation:

Wei ZHOU, Meng ZENG, Jian WANG, Lei ZHANG, Ying-chun LI. Determination of Major and Rare Earth Elements in Rare Earth Ores by X-ray Fluorescence Spectrometry with Fusion Sample Preparation[J]. Rock and Mineral Analysis, 2018, 37(3): 298-305. doi: 10.15898/j.cnki.11-2131/td.201706280113

Determination of Major and Rare Earth Elements in Rare Earth Ores by X-ray Fluorescence Spectrometry with Fusion Sample Preparation

1.
National Research Center for Geoanalysis, Beijing 100037, China
2.
Ganxibei Geological Brigade, Jiangxi Bureau of Exploration & Development of Geology & Mineral Resources, Jiujiang 336017, China

More Information

Corresponding author: Ying-chun LI, liyingchun@cags.ac.cn

Received Date: 10 April 2017

Revised Date: 09 January 2018

Accepted Date: 07 May 2018

Abstract

Abstract

BACKGROUND The analysis of ore samples by X-ray Fluorescence Spectrometry (XRF) has the advantages of quantitative accuracy, less reagent and good reproducibility. However, due to the lack of rare earth standard materials at present, the accurate quantitative requirements for complex rare earth ore samples cannot be met. BAOBJECTIVES To establish the analysis method for XRF determination of 25 major elements and rare earth elements in rare earth ores and mineralized samples. METHODS The use of artificial standard samples solved the problem of lack of standard materials. The linear ranges of La, Ce and Y were extended by adding high purity rare earth oxides La₂O₃, CeO₂ and Y₂O₃. A calibration line was produced using artificial standard samples, existing standard materials of rare earth and carbonate. The major elements were calibrated by a theoretical alpha coefficient method, whereas the rare earth elements were calibrated by an empirical coefficient method. Interference correction was used for elements with overlapping spectral lines. RESULTS The relative standard deviations (RSD, n=13) of most major elements were less than 1.5%, whereas the RSDs of rare earth elements were 0.69%-6.94% when their concentrations were above 300 μg/g. CONCLUSIONS The method was evaluated by unknown samples and the sums of major elements, rare earth elements and loss of ignition were 99.41%-100.63%. The method satisfies the first criterion of Geology and Minerals Laboratory Testing Quality Management Standards.
- rare earth ore /
- X-ray Fluorescence Spectrometry /
- matrix effect /
- artificial standard substances

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References

[1]	Simandl G J.Geology and market-dependent significance of rare earth element resources[J].Mineralium Deposita, 2014, 49(8):889-904. doi: 10.1007/s00126-014-0546-z CrossRef Google Scholar
[2]	Jordens A, Cheng Y P, Waters K E.A review of the beneficiation of rare earth element bearing minerals[J].Minerals Engineering, 2013, 41(1):97-114. Google Scholar
[3]	Simandl G J, Fajber R, Paradis S.Portable X-ray fluore-scence in the assessment of rare earth element-enriched sedimentary phosphate deposits[J].Geochemistry Exploration Environment Analysis, 2014, 14(2):161-169. doi: 10.1144/geochem2012-180 CrossRef Google Scholar
[4]	Xie F, Zhang T A, Dreisinger D, et al.A critical review on solvent extraction of rare earths from aqueous solutions[J].Minerals Engineering, 2014, 56(2):10-28. Google Scholar
[5]	李小莉, 张勤.粉末压片-X射线荧光光谱法测定土壤、水系沉积物和岩石样品中15种稀土元素[J].冶金分析, 2013, 33(7):35-40. Google Scholar Li X L, Zhang Q.Determination of fifteen rare earth elements in soil, stream sediment and rock samples by X-ray fluorescence spectrometry with pressed powder pellet[J].Metallurgical Analysis, 2013, 33(7):35-40. Google Scholar
[6]	张文娟, 谢玲君, 刘鸿.ICP-AES法测定氟碳铈矿中低含量稀土总量[J].有色金属科学与工程, 2016, 7(6):141-146. Google Scholar Zhang W J, Xie L J, Liu H.Determination of low content total rare earth in bastnaesite by ICP-AES[J].Nonferrous Metals Science and Engineering, 2016, 7(6):141-146. Google Scholar
[7]	罗立强, 詹秀春, 李国会.X射线荧光光谱仪[M].北京:化学工业出版社, 2008. Google Scholar Luo L Q, Zhan X C, Li G H.X-ray Fluorescence Spectrometer[M].Beijing:Chemical Industry Press, 2008. Google Scholar
[8]	Claisse F, Blanchette J S B(著). 卓尚军(译). 硼酸盐熔融的物理与化学[M]. 上海: 华东理工大学出版社, 2006. Google Scholar Claisse F, Blanchette J S B (Authors). Zhuo S J (Translator). Physics and Chemistry of Borate Melting[M]. Shanghai: East China University of Science and Technology Press, 2006. Google Scholar
[9]	Parra L M M, Greaves E D, Paz J L, et al.Simultaneous determination of rare earths by X-ray fluorescence spectrometry using a fundamental parameters method[J].X-Ray Spectrometry, 1993, 22(5):362-367. doi: 10.1002/(ISSN)1097-4539 CrossRef Google Scholar
[10]	黄肇敏, 周素莲.X射线荧光光谱法测定混合稀土氧化物中稀土分量[J].光谱学与光谱分析, 2007, 27(9):1873-1877. Google Scholar Huang Z M, Zhou S L.Method for determination of RE₂O₃ by X-ray fluorescence spectrometry[J].Spectroscopy and Spectral Analysis, 2007, 27(9):1873-1877. Google Scholar
[11]	李可及, 肖颖.熔融制样-X射线荧光光谱法测定氟碳铈矿流程样品[J].稀土, 2016, 37(2):144-148. Google Scholar Li K J, Xiao Y.Determination of bastnaesite process samples by fusion X-ray fluorescence spectrometry[J].Chinese Rare Earths, 2016, 37(2):144-148. Google Scholar
[12]	Legkodymov A A, Kuper K E, Nazmov V P, et al.Applying hard X-rays to determination of the minimum detection levels of rare earth element by the XRFA-SR method[J].Bulletin of the Russian Academy of Sciences Physics, 2015, 79(1):103-108. doi: 10.3103/S1062873815010207 CrossRef Google Scholar
[13]	于丽丽, 汤玉河, 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. Google Scholar Yu L L, Tang Y H, Xiao F Y, 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. Google Scholar
[14]	冯丽丽, 张庆建, 丁仕兵, 等.X射线荧光光谱法测定锆矿中10种主次成分[J].冶金分析, 2014, 34(7):51-55. Google Scholar Feng L L, Zhang Q J, Ding S B, et al.Determination of ten major and minor components in zirconium ore by X-ray fluorescence spectrometry[J].Metallurgical Analysis, 2014, 34(7):51-55. Google Scholar
[15]	罗学辉, 苏建芝, 汤宇磊, 等.高倍稀释熔融制样-X射线荧光光谱法测定镍矿石中主次成分[J].冶金分析, 2017, 37(9):52-56. Google Scholar Luo X H, Su J Z, Tang Y L, et al.Determination of major and minor components in nickel ore by X-ray fluorescence spectrometry with fusion sample preparation of high dilution[J].Metallurgical Analysis, 2017, 37(9):52-56. Google Scholar
[16]	李迎春, 周伟, 王健, 等.X射线荧光光谱法测定高锶高钡的硅酸盐样品中主量元素[J].岩矿测试, 2013, 32(2):249-253. Google Scholar Li Y C, Zhou W, Wang J, et al.Determination of major elements in silicate samples with high content strontium and barium by X-ray fluorescence spectrometry[J].Rock and Mineral Analysis, 2013, 32(2):249-253. Google Scholar
[17]	沈亚婷, 李迎春, 孙梦荷, 等.波长与能量色散复合式X射线荧光光谱仪特性研究及矿区土壤分析[J].光谱学与光谱分析, 2017, 37(7):2216-2224. Google Scholar Shen Y T, Li Y C, Sun M H, et al.Studies on characteristics on a combined wavelength and energy dispersion X-ray fluorescence spectrometer and determinations of major, minor and trace elements in soils around a mining area[J].Spectroscopy and Spectral Analysis, 2017, 37(7):2216-2224. Google Scholar
[18]	李国会, 李小莉.X射线荧光光谱分析熔融法制样的系统研究[J].冶金分析, 2015, 35(7):1-9. Google Scholar Li G H, Li X L.Systematic study on the fusion sample preparation in X-ray fluorescence spectrometric analysis[J].Metallurgical Analysis, 2015, 35(7):1-9. Google Scholar
[19]	詹秀春, 陈永君, 郑妙子, 等.地质样品X射线荧光分析中的背景相关曲线及其应用[J].岩矿测试, 2003, 22(3):161-164. Google Scholar Zhan X C, Chen Y J, Zheng M Z, et al.Background-related curve in the X-ray fluorescence spectrometric analysis of geological materials and its application[J].Rock and Mineral Analysis, 2003, 22(3):161-164. Google Scholar