Simultaneous determination of major and minor components in silicate and bauxite by X-ray fluorescence spectrometry with fusion sample preparation
GAO Zhi-jun1,2, CHEN Jing1,2, CHEN Hao-feng1,2, LI Jie1,2
1. Henan Province Rock and Mineral Testing Center, Zhengzhou 450012,China; 2. Key Laboratory of Ministry and Resources Analysis and Exploration of Precious Metals, Zhengzhou 450012,China
Abstract：The certified reference materials of soil, stream sediment, rock, iron ore and bauxite were prepared by fusion method for the fitting of calibration curve. The rapid analysis method for the simultaneous determination of major and minor components (SiO2, Al2O3, Fe2O3, TiO2, K2O, Na2O, CaO, MgO, P2O5 and MnO) in silicate and bauxite by X-ray fluorescence spectrometry(XRF) was established. The fusion conditions of samples were obtained as follows: the sample was uniformly mixed with lithium tetraborate-lithium metaborate (mass ratio of 67∶33) with the dilution ratio of 1∶10; then, 2 mL of 500 g/L NH4NO3 solution and 0.5 mL of 300 g/L NH4Br solution were added; the sample was pre-oxidized at 700 ℃ followed by fusion at 1 100 ℃. The proposed method solved the following problems: each ore sample required one set of analysis method; the geological samples with various types could not be determined simultaneously. The components in certified reference material of bauxite (GBW07178 and GBW07179) were determined by proposed method. The relative standard deviation (RSD, n=12) was less than 5%. The relative error (RE) was less than 10%. The proposed method was also applied to the determination of silicate and bauxite samples, and the found results were consistent with those obtained by wet method.
高志军,陈静,陈浩凤,李杰. 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 Zhi-jun,CHEN Jing,CHEN Hao-feng,LI Jie. Simultaneous determination of major and minor components in silicate and bauxite by X-ray fluorescence spectrometry with fusion sample preparation. , 2015, 35(7): 73-78.
李献华,刘颖,涂湘林.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 Xian-hua, LIU Ying, TU Xiang-lin, 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]. Geochemical,2002,31(3): 289-294.
[2]
周享春,汪福意.火焰原子吸收法测定硅酸盐中铁钙镁[J].理化检验:化学分册,1997,33(5):207-209. ZHOU Xian-chun, WANG Fu-yi. Determination of iron, calcium and magnesium in silicates by flame atomic absorption spectrometry[J]. Physical Testing and Chemical Analysis Part B: Chemical Analysis, 1997, 33(5):207-209.
朱忠平,李国会. 熔融制样—X射线荧光光谱法测定钛铁矿中主次组分[J]. 冶金分析,2013,33(6):32-36. ZHU Zhong-ping, LI Guo-hui. Determination of major and minor components in ilmenite by X-ray fluorescence spectrometry with fusion sample preparation[J]. Metallurgical Analysis ,2013,33(6):32-36.
[6]
张爱芬,马慧侠,李国会.X射线荧光光谱法测定铝矿石中主次痕量组分[J].岩矿测试,2005,24(4):307-310. ZHANG Ai-fen, MA Hui-xia, LI Guo-hui. Determination of major, minor and trace elements in bauxite by XRF spectrometry[J]. Rock and Mineral Analysis, 2005,24(4):307-310.
[7]
于波,严志远,杨乐山, 等. X射线荧光光谱法测定土壤和水系沉积物中碳和氮等36个主次痕量元素[J].岩矿测试, 2006,25(1):74-79. YU Bo, YAN Zhi-yuan , YANG Le-shan,et al. Determination of 36 major, minor and trace elements in soil and stream sediment samples by X-ray fluorescence spectrometry[J]. Rock and Mineral Analysis,2006,25(1):74-79.
[8]
赵恩好,岳明新,周国兴, 等.X射线荧光光谱法测定镁质耐火材料及其原料中10种成分[J]. 冶金分析,2013,33(7):62-67. ZHAO En-hao,YUE Ming-xin, ZHOU Guo-xing, et al. Determination of ten components in magnesia refractory materials and raw materials by X-ray fluorescence spectrometry[J]. Metallurgical Analysis, 2013,33(7):62-67.
[9]
张勤,樊守忠,潘宴山,等. X射线荧光光谱法测定多目标地球化学调查样品中主次痕量组分[J].岩矿测试,2004, 23(1):19-24. ZHANG Qin, FAN Shou-zhong, PAN Yan-shan, et al. Determination of 25 major , minor and trace elements in geochemical exploration samples by X-ray fluorescence spectrometry[J]. Rock and Mineral Analysis, 2004, 23(1):19-24.
[10]
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 Lun-ao. 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.
[11]
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. LI Guo-hui, BU Wei, FAN Shou-zhong. Determination of twenty major, minor and trace elements in silicate by XRF spectrometry[J]. Spectroscopy and Spectral Analysis, 1994, 14(1):105-110.
[12]
梁述廷, 刘玉纯, 胡浩. X射线荧光光谱法同时测定土壤样品中碳氮等多元素[J].岩矿测试, 2004,23(2):102-108. LIANG Shu-ting, LIU Yu-chun, HU Hao. Determination of C, N and other 36 elements in soil samples by XRF[J]. Rock and Mineral Analysis, 2004,23(2):102-108.
[13]
李小莉, 陈曦, 葛江洪, 等. 熔融制样—X射线荧光光谱法测定海洋沉积物中氯等元素[J].理化检验:化学分册,2011,47(12):1420-1423. LI Xiao-li, CHEN Xi, GE Jiang-hong,et al. XRFS determination of chlorine etc multi-elements in sead sediments with sample preparation by fusion[J]. Physical Testing and Chemical Analysis Part B: Chemical Analysis, 2011,47(12):1420-1423.
[14]
薛秋红, 李静, 丁玉龙, 等. 玻璃熔片制样X射线荧光光谱法测定矾土中主次量组分[J].岩矿测试, 2010,29(2):182-184. XUE Qiu-hong, LI Jing, DING Yu-long, et al. Determination of major and minor components in bauxite by X-ray fluorescence spectrometry with fusion sample preparation[J]. Rock and Mineral Analysis, 2010, 29(2):182-184.
[15]
Claisse F, Blanchette J S. Physics and Chemistry of Borate Fusion [M]. 卓尚军译. 上海: 华东理工大学出版社, 2006.
[16]
李清彩, 赵庆令. 粉末压片制样波长色散X射线荧光光谱法测定钼矿石中9种元素[J]. 岩矿测试, 2014,33(6):839-843. LI Qing-cai,ZHAO Qing-ling. Determination of 9 elements in molybdenum ore by wavelength dispersive X-ray fluorescence spectrometry with powder pelleting preparation[J]. Rock and Mineral Analysis, 2014,33(6):839-843.
[17]
于兆水, 张勤, 李小莉, 等. 高压粉末制样波长色散X射线荧光光谱法测定生物样品中23种元素[J].岩矿测试, 2014,33(6):844-848. YU Zhao-shui,ZHANG Qin,LI Xiao-li, et al. Determination of 23 elements in biological samples by wavelength dispersion X-ray fluorescence spectrometry with high pressure powder pelleting preparation[J]. Rock and Mineral Analysis, 2014,33(6):844-848.
