DETERMINATION OF EIGHTEEN COMPONENTS IN SILICATE ROCKS BY X-RAY FLUORESCENCE SPECTROMETRY WITH HIGH DILUTION RATIO FUSION SAMPLE PREPARATION

BU Dao-lu; QIU Hai; GONG Cang; SHUAI Lin-yang; DING Yang

doi:10.13686/j.cnki.dzyzy.2021.06.014

2021 Vol. 30, No. 6

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BU Dao-lu, QIU Hai, GONG Cang, SHUAI Lin-yang, DING Yang. DETERMINATION OF EIGHTEEN COMPONENTS IN SILICATE ROCKS BY X-RAY FLUORESCENCE SPECTROMETRY WITH HIGH DILUTION RATIO FUSION SAMPLE PREPARATION[J]. Geology and Resources, 2021, 30(6): 740-746. doi: 10.13686/j.cnki.dzyzy.2021.06.014

Citation:

BU Dao-lu, QIU Hai, GONG Cang, SHUAI Lin-yang, DING Yang. DETERMINATION OF EIGHTEEN COMPONENTS IN SILICATE ROCKS BY X-RAY FLUORESCENCE SPECTROMETRY WITH HIGH DILUTION RATIO FUSION SAMPLE PREPARATION[J]. Geology and Resources, 2021, 30(6): 740-746. doi: 10.13686/j.cnki.dzyzy.2021.06.014

DETERMINATION OF EIGHTEEN COMPONENTS IN SILICATE ROCKS BY X-RAY FLUORESCENCE SPECTROMETRY WITH HIGH DILUTION RATIO FUSION SAMPLE PREPARATION

Applied Geology Research Center of China Geological Survey, Chengdu 611732, China

Received Date: 12 January 2021

Revised Date: 05 February 2021

Publish Date: 30 December 2021

Abstract

Abstract

The paper introduces a rapid analysis method of X-ray fluorescence spectrometry (XRF) to determine 18 components (SiO₂, Al₂O₃, TFe₂O₃, MgO, CaO, K₂O, Na₂O, TiO₂, BaO, MnO, P₂O₅, Cr₂O₃, V₂O₅, Rb, Sr, Zr, Cu and Ni) in silicate samples. Selecting the reference materials such as soil, stream sediments, rocks of national first-class standard material, ultrabasic rocks and clay, the method applies high dilution ratio (14:1) of mixed solvent to sample mass for fusion sample preparation and fits the calibration curve. Through Eagon2 automatic high frequency inductance fusion machine, 7.0000 g of mixed solvent (45Li₂B₄O₇+10LiBO₂+5LiF) and 0.5000 g of sample are mixed uniformly, adding 2 drops of saturated ammonium nitrate solution as oxidant and then 4 drops of saturated lithium bromide solution as release agent, followed by preoxidation at 700℃ for 4 min and fusion at 1120℃ for 9 min, and finally cooling naturally to room temperature for sample preparation. The above fusion method can ensure that the components to be measured are completely melted and the sample surface is smooth and flat. Verified by national standard substances, the accuracy and precision of test results are in line with the requirements of Quality Management Code for Laboratory Testing of Geology and Mineral Resources (DZ/T 0130-2006).
- high dilution ratio /
- fusion sample preparation /
- X-ray fluorescence spectrometry /
- silicate

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References

[1]	《岩石矿物分析》编委会. 岩石矿物分析: 第2分册[M]. 4版. 北京: 地质出版社, 2011: 1-3. Google Scholar Editorial Board for Rock and Mineral Analysis. Analysis of rocks and minerals: Part 2[M]. 4th ed. Beijing: Geological Publishing House, 2011: 1-3. (in Chinese) Google Scholar
[2]	周存款, 袁永海. X射线荧光光谱法测定硅酸盐和高铁高钛铝土矿中主次组分[J]. 理化检验-化学分册, 2018, 54(3): 303-307. Google Scholar Zhou C K, Yuan Y H. Determination of major and minor components in silicate and bauxite with high content of iron and titanium by X-Ray fluorescence spectrometry[J]. Physical Testing and Chemical Analysis Part B-Chemical Analysis, 2018, 54(3): 303-307. Google Scholar
[3]	祁昌炜, 朱杰勇, 王佳音, 等. 便携式X射线荧光元素分析仪的应用[J]. 地质与资源, 2013, 22(1): 64-66. Google Scholar Qi C W, Zhu J Y, Wang J Y, et al. Application of the portable XRF analyzer in sample testing[J]. Geology and Resources, 2013, 22(1): 64-66. Google Scholar
[4]	李献华, 刘颖, 涂湘林, 等. 硅酸盐岩石化学组成的ICP-AES和ICP-MS准确测定: 酸溶与碱熔分解样品方法的对比[J]. 地球化学, 2002, 31(3): 289-294. Google Scholar Li X H, Liu Y, Tu X L, et al. Precise determination of chemical compositions in silicate rocks using ICP-AES and ICP-MS: A comparative study of sample digestion techniques of alkali fusion and acid dissolution[J]. Geochimica, 2002, 31(3): 289-294. Google Scholar
[5]	陈玉明, 陈秀法. 阿根廷米纳毕戈塔斯地区1: 250000地球化学数据集[J]. 中国地质, 2018, 45(S2): 83-92, 107-118. doi: 10.12029/gc2018Z210 CrossRef Google Scholar Chen Y M, Chen X F. Argentine Mina Pirquitas 1: 250000 geochemistry dataset[J]. Geology in China, 2018, 45(S2): 83-92, 107-118. doi: 10.12029/gc2018Z210 CrossRef Google Scholar
[6]	高志军, 陈静, 陈浩凤, 等. 熔融制样-X射线荧光光谱法测定硅酸盐和铝土矿中主次组分[J]. 冶金分析, 2015, 35(7): 73-78. Google Scholar Gao Z J, Chen J, Chen H F, et al. Simultaneous determination of major and minor components in silicate and bauxite by X-ray fluorescence spectrometry with fusion sample preparation[J]. Metallurgical Analysis, 2015, 35(7): 73-78. Google Scholar
[7]	李国会, 卜维, 樊守忠. X射线荧光光谱法测定硅酸盐中硫等20个主、次、痕量元素[J]. 光谱学与光谱分析, 1994, 14(1): 105-110, 104. Google Scholar Li G H, Bu W, Fan S Z. Determination of twenty major, minor and trace elements in silicate by XRF spectrometry[J]. Spectroscopy and Spectral Analysis, 1994, 14(1): 105-110, 104. Google Scholar
[8]	欧阳伦熬. X射线荧光光谱法测定多种铁矿和硅酸盐中主次量组分[J]. 岩矿测试, 2005, 24(4): 303-306. Google Scholar Ouyang L A. Determination of major and minor elements in iron ores and silicates by XRF spectrometry with fusion sample preparation technique[J]. Rock and Mineral Analysis, 2005, 24(4): 303-306. Google Scholar
[9]	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
[10]	袁伟哲, 田俊杰, 徐志坚, 等. X荧光光谱法测定硅酸盐中的主次量元素[J]. 吉林地质, 2015, 34(3): 116-119. Google Scholar Yuan W Z, Tian J J, Xu Z J, et al. Determination of primary and secondary elements in silicate by X fluorescence spectrometry[J]. Jilin Geology, 2015, 34(3): 116-119. Google Scholar
[11]	周存款, 潘炜燕, 乔小芳, 等. 熔融制样-X射线荧光光谱法测定硅酸盐样品中主量元素[J]. 矿产与地质, 2017, 31(5): 1004-1008. Google Scholar Zhou C K, Pan W Y, Qiao X F, et al. Determination of major elements in silicates by X-ray fluorescence spectrometry with fusion sample preparation[J]. Mineral Resources and Geology, 2017, 31(5): 1004-1008. Google Scholar
[12]	罗学辉. 熔融法-波长X射线荧光光谱法测定硅酸盐岩石中16种主次成份量[D]. 南昌: 东华理工大学, 2017: 18-19. Google Scholar Luo X H. Determination of 16 major and minor elements in silicate rock by wavelength X-ray fluorescence spectrometry with sample fusion[D]. Nanchang: East China University of Technology, 2017: 18-19. Google Scholar
[13]	张振华, 赵朔, 曹峰. X射线荧光光谱法熔融制样测定硅酸盐样品中的主、次成分[J]. 实验室科学, 2013, 16(2): 6-9. Google Scholar Zhang Z H, Zhao S, Cao F. Determination of major and minor elements in the samples of silicate rocks by XRF[J]. Laboratory Science, 2013, 16(2): 6-9. Google Scholar
[14]	周国兴, 赵恩好, 岳明新, 等. X射线荧光光谱法测试重晶石中的多元素[J]. 地质与资源, 2014, 23(3): 292-295. Google Scholar Zhou G X, Zhao E H, Yue M X, et al. Application of X-Ray fluorescence spectrometry in the multi-element test of barite[J]. Geology and Resources, 2014, 23(3): 292-295. Google Scholar
[15]	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
[16]	罗学辉, 苏建芝, 鹿青, 等. 高倍稀释熔融制样-X射线荧光光谱法测定铅锌矿中主次组分[J]. 冶金分析, 2014, 34(1): 50-54. Google Scholar Luo X H, Su J Z, Lu Q, et al. Determination of major and minor components in lead-zinc ores by X-ray fluorescence spectrometry with high dilution fusion sample preparation[J]. Metallurgical Analysis, 2014, 34(1): 50-54. Google Scholar
[17]	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: 130-135. Google Scholar Luo L Q, Zhan X C, Li G H. X-ray fluorescence spectrometry[M]. 2nd ed. Beijing: Chemical Industry Press, 2015: 130-135. Google Scholar
[18]	张勤, 李国会, 樊守忠, 等. X射线荧光光谱法测定土壤和水系沉积物等样品中碳、氮、氟、氯、硫、溴等42种主次和痕量元素[J]. 分析试验室, 2008, 27(11): 51-57. Google Scholar Zhang Q, Li G H, Fan S Z, et al. Study on determination of 42 major minor and trace elements in soil and stream sediment samples[J]. Chinese Journal of Analysis Laboratory, 2008, 27(11): 51-57. Google Scholar
[19]	中华人民共和国国家质量监督检验检疫总局, 中国国家标准化管理委员会. GB/T 14506.28-2010硅酸盐岩石化学分析方法——第28部分: 16个主次成分量测定[S]. 北京: 中国标准出版社, 2011: 1-7. Google Scholar General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China, Standardization Administration of the People's Republic of China. GB/T 14506.28-2010 Methods for chemical analysis of silicate rocks-Part 28: Determination of 16 major and minor elements content[S]. Beijing: Standards Press of China, 2011: 1-7. Google Scholar
[20]	中华人民共和国国土资源部. DZ/T 0130-2006地质矿产实验室测试质量管理规范[S]. 北京: 中国标准出版社, 2006: 31-39. Google Scholar Ministry of Land and Resources of the People's Republic of China. DZ/T 0130-2006 The specification of testing quality management for geological laboratories[S]. Beijing: Standards Press of China, 2006: 31-39. Google Scholar