Determination of major and minor components in medium-low grade bauxite and high-sulfur bauxite by wavelength dispersive X-ray fluorescence spectrometry
Abstract：There is a great variety of medium-low grade bauxite. The content of Al2O3 is low and the composition of other components is complicated. It usually contains rich Fe2O3, CaO, MgO and S. During the determination of samples containing rich Fe2O3 and S by X-ray fluorescence spectrometry (XRF) after fusion sample preparation, the platinum-gold crucible can be corroded in sample melting. Moreover, the flowability of sample is poor and the volatilization of S at high temperature is serious. NH4NO3 was used as oxidizing agent for fusion sample preparation. The simultaneous determination method of Al2O3, SiO2, Fe2O3, CaO, TiO2, K2O, Na2O, MgO, P2O5 and S in medium-low grade bauxite and high-sulfur bauxite by wavelength dispersive X-ray fluorescence spectrometry was established. In order to broaden the content range of components such as Fe2O3 and S, the calibration curve was plotted using the national standard substances and samples after chemical analysis. The dilution ratio of sample and flux was 1∶20. In experiments, 1.0g of NH4NO3 was used as oxidizing agent and 0.5mL of LiBr solution was used as release agent. After fusion at 1050℃ for 8min, the transparent sample pellet with high vitrifaction degree could be prepared. The detection limits of components ranged from 27.7μg/g to 259μg/g. The relative standard deviations (RSD, n=12) of determination results were all less than 3%. The actual sample was analyzed and the found results were consistent with those obtained by other methods. The proposed study effectively solved the sample preparation problem for Fe2O3 and S-rich medium-low grade bauxite and high-sulfur bauxite as well as the problem that the content of S was difficult to be accurately determined. The proposed method was applicable for the analysis of bauxite samples with S content less than 15%.
陆安军, 苏梦晓. 波长色散X射线荧光光谱法测定中低品位铝土矿和高硫铝土矿中主次组分[J]. 冶金分析, 2019, 39(4): 53-59.
LU An-jun, SU Meng-xiao. Determination of major and minor components in medium-low grade bauxite and high-sulfur bauxite by wavelength dispersive X-ray fluorescence spectrometry. , 2019, 39(4): 53-59.
陈滨,肖利,唐娴敏.中低品位贵州铝土矿石灰拜尔法溶出工艺[J].中南大学学报:自然科学版,2014,45(5):1397-1402.CHEN Bin,XIAO Li,TANG Xian-min.Digestion technology of Guizhou diasporic bauxite with low and medium grades by lime Bayer process[J].Journal of Central South University:Science and Technology,2014,45(5):1397-1402.
[2]
梁汉轩,鹿爱莉,李翠平,等.我国铝土矿贫矿资源的开发利用条件及方向[J].中国矿业,2011,20(7):10-13.LIANG Han-xuan,LU Ai-li,LI Cui-ping,et al.Conditions and directions for utilization of low-grade bauxite in China[J].China Mining Magazine,2011,20(7):10-13.
[3]
王鹏,魏徳洲.高硫铝土矿脱硫技术[J].金属矿山,2012(1):108-110.WANG Peng,WEI De-zhou.Desulfuration technique research of high-sulfur bauxite[J].Metal Mine,2012(1):108-110.
[4]
文加波,李克庆,向忠宝,等.电感耦合等离子体原子发射光谱法同时测定铝土矿中40种组分[J].冶金分析,2011,31(12):43-49.WEN Jia-bo,LI Ke-qing,XIANG Zhong-bao,et al.Simultaneous determination of forty elements in bauxite by inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2011,31(12):43-49.
[5]
王琰,孙洛新,张帆,等.电感耦合等离子体发射光谱法测定含刚玉的铝土矿中硅铝铁钛[J].岩矿测试,2013,32(5):719-723.WANG Yan,SUN Luo-xin,ZHANG Fan,et al.Determination of Si,Al,Fe and Ti in bauxite by inductively coupled plasma-atomic emission spectrometry[J].Rock and Mineral Analysis,2013,32(5):719-723.
[6]
邓赛文,梁国立,方明渭,等.X射线荧光光谱快速分析铝土矿的方法研究[J].岩矿测试,2001,20(4):305-308.DENG Sai-wen,LIANG Guo-li,FANG Ming-wei,et al.A rapid in site method for bauxite analysis by XRF[J].Rock and Mineral Analysis,2001,20(4):305-308.
[7]
张莉娟,曾江萍.超细制样粉末压片法测定铝土矿中主量元素的含量[J].轻金属,2014(7):6-9.ZHANG Li-juan,ZENG Jiang-ping.Determination of main elements of bauxite by pressed ultrafine powder pellet[J].Light Metals,2014(7):6-9.
[8]
钟代果.铝土矿中主成分的X射线荧光光谱分析[J].岩矿测试,2008,27(1):71-73.ZHONG Dai-guo.X-ray fluorescence spectrometric analysis of major components in bauxite samples[J].Rock and Mineral Analysis,2008,27(1):71-73.
[9]
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.
[10]
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 Zhi-jun,CHEN Jing,CHEN Hao-feng,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.
[11]
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 Cun-kuan,YUAN Yong-hai.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.
[12]
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.
[13]
刘江斌,段九存,党亮,等.X射线荧光光谱法同时测定铝土矿中主、次组分及3种痕量元素[J].理化检验:化学分册,2011,47(10):1211-1226.LIU Jiang-bin,DUAN Jiu-cun,DANG Liang,et al.XRFS determination of major,minor components and 3 trace elements in bauxites[J].Physical Testing and Chemical Analysis Part B:Chemical Analysis,2011,47(10):1211-1226.
[14]
谢静思,甘学锋.X射线荧光光谱法测定铝土矿中的主次量组分[J].广东化工,2013,40(24):149-150.XIE Jing-si,GAN Xue-feng.Determination of major and minor components in bauxite with X-ray fluorescence spectrometry[J].Guangdong Chemical Industry,2013,40(24):149-150.
[15]
彭南兰,华磊,秦红艳.X射线荧光光谱法测定文山地区铝土矿中多种组分[J].矿物学报,2013,33(4):530-534.PENG Nan-lan,HUA Lei,Q1N Hong-yan.Determination of multiple elements in Wenshan bauxite by XRF spectrometry[J].Acta Mineralogica Sinica,2013,33(4):530-534.
[16]
袁海燕.X射线荧光光谱法测定高铁铝土矿石中的主次量元素[J].化学工程师,2016(7):33-36.YUAN Hai-yan.Simultaneous determination of major and minor components in high-iron type bauxite by X-ray fluorescence spectrometry with fusion sample preparation[J].Chemical Engineer,2016(7):33-36.
[17]
钟坚海.熔融制样-X射线荧光光谱法测定铝矿中15种组分[J].冶金分析,2018,38(11):24-29.ZHONG Jian-hai.Determination of fifteen components in aluminum ore by X-ray fluorescence spectrometry with fusion sample prepaeation[J].Metallurgical Analysis,2018,38(11):24-29.
[18]
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.
[19]
普旭力,吴亚全,王鸿辉,等.X射线荧光光谱法同时测定铁矿石中主次量组分[J].岩矿测试,2008,27(5):353-356.PU Xu-li,WU Ya-quan,WANG Hong-hui,et al.Simultaneous determination of major and minor components in iron ore samples by X-ray fluorescence spectrometry[J].Rock and Mineral Analysis,2008,27(5):353-356.
[20]
廖海平,付冉冉,任春生,等.熔融制样-X射线荧光光谱法测定硫铁矿中主次成分[J].冶金分析,2014,34(12):29-32.LIAO Hai-ping,FU Ran-ran,REN Chun-sheng,et al.Determination of major and minor components in pyrite by X-ray fluorescence spectrometry with fusion sample preparation[J].Metallurgical Analysis,2014,34(12):29-32.
[21]
李小莉,安树清,徐铁民,等.熔片制样-X射线荧光光谱法测定煤灰样品中主次量组分[J].岩矿测试,2009,28(4):385-387.LI Xiao-li,AN Shu-qing,XU Tie-min,et al.Determination of major and minor components in coal ash samples by X-ray fluorescence spectrometry with fused bead sample preparation[J].Rock and Mineral Analysis,2009,28(4):385-387.
[22]
李国会.X射线荧光光谱法测定铬铁矿中主次量组分[J].岩矿测试,1999,18(2):53-56.LI Guo-hui.Determination of major and minor elements in chromite by X-ray fluorescence spectrometry[J].Rock and Mineral Analysis,1999,18(2):53-56.
[23]
张莉娟,徐铁民,李小莉,等.X射线荧光光谱法测定富含硫砷钒铁矿石中的主次量元素[J].岩矿测试,2011,30(6):772-776.ZHANG Li-juan,XU Tie-min,LI Xiao-li,et al.Quantification of major and minor components in iron ores with sulfur,arsenic and vanadium by X-ray fluorescence spectrometry[J].Rock and Mineral Analysis,2011,30(6):772-776.
[24]
Baker J W.Volatilization of sulfur in fusion techniques for preparation of discs for X-ray fluorescence analysis[J].Advances in X-ray Analysis,1982,25:91-94.
