高稀释比熔融-X射线荧光光谱法分析硅酸盐岩石样品中18种组分

doi:10.13686/j.cnki.dzyzy.2021.06.014

摘要
图/表
参考文献
相关文章 (4)

全文: PDF (870 KB) HTML (1 KB)
输出: BibTeX | EndNote (RIS)

摘要选取土壤、水系沉积物、岩石、超基性岩、黏土等标准物质，应用混合溶剂与样品质量比为14：1的高稀释比方法熔融制备测试样品，拟合校准曲线，建立X射线荧光光谱（XRF）同时测定硅酸盐岩石样品中18种组分（SiO₂、Al₂O₃、TFe₂O₃、MgO、CaO、K₂O、Na₂O、TiO₂、BaO、MnO、P₂O₅、Cr₂O₃、V₂O₅、Rb、Sr、Zr、Cu、Ni）的快速分析方法.应用帕纳科Eagon2全自动高频电感熔样机，称取7.0000 g（45Li₂B₄O₇+10LiBO₂+5LiF）混合溶剂与0.5000 g样品混合均匀，分别加入氧化剂饱和硝酸铵溶液2滴，脱模剂饱和溴化锂溶液4滴，于700℃先预氧化4 min，再1 120℃熔融9 min制备样片，自然冷却至室温.此熔样方法能保证样品中待测组分熔化完全，并制得表面光滑平整的样片.用国家标准物质验证，测试结果的准确度和精密度均符合《地质矿产实验室测试质量管理规范》（DZ/T 0130-2006）要求.

	服务

	把本文推荐给朋友
	加入我的书架
	加入引用管理器
	E-mail Alert
	RSS
	作者相关文章
	卜道露
	邱海
	龚仓
	帅林阳
	丁洋

关键词 ：高稀释比, 熔融制样, X射线荧光光谱法, 硅酸盐

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).

Key words： high dilution ratio fusion sample preparation X-ray fluorescence spectrometry silicate

收稿日期: 2021-01-12

PACS:

P585.2

基金资助:自然资源部项目"甘肃阳山金矿岩金普查"（DD20191028）.

作者简介: 卜道露(1986-),男,硕士,工程师,现从事岩石矿物分析测试工作,通信地址四川省成都市郫都区唐元镇长林大道19号,E-mail//budaolu509@163.com

引用本文:

卜道露, 邱海, 龚仓, 帅林阳, 丁洋. 高稀释比熔融-X射线荧光光谱法分析硅酸盐岩石样品中18种组分[J]. 地质与资源, 2021, 30(6): 740-746.
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. GEOLOGY AND RESOURCES, 2021, 30(6): 740-746.

链接本文:

http://manu25.magtech.com.cn/Jweb_dzyzy/CN/10.13686/j.cnki.dzyzy.2021.06.014 或 http://manu25.magtech.com.cn/Jweb_dzyzy/CN/Y2021/V30/I6/740

[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. 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)
[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. 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.
[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. 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.
[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. 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.
[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. Chen Y M, Chen X F. Argentine Mina Pirquitas 1:250000 geochemistry dataset[J]. Geology in China, 2018, 45(S2):83-92, 107-118.
[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. 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.
[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. 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.
[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. 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.
[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. 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.
[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. 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.
[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. 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.
[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. 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.
[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. 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.
[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. 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.
[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. 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.
[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. 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.
[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. Luo L Q, Zhan X C, Li G H. X-ray fluorescence spectrometry[M]. 2nd ed. Beijing:Chemical Industry Press, 2015:130-135.
[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. 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.
[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. 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.
[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. 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.