Abstract：The determination of components in bauxite was very important to guide the actual production of steelmaking. The mixture of lithium tetraborate with mass fraction of 35.3% and lithium metaborate with mass fraction of 64.7% was used as mixed flux. The ammonium iodide solution was used as release agent. The bauxite sample was prepared as sample fused bead by fusion method in platinum-gold crucible. The absorption-enhancement effect was corrected by theoretical coefficient method and empirical coefficient method. Thus, a determination method of silicon dioxide, aluminum oxide and iron trioxide in bauxite was established by X-ray fluorescence spectrometry (XRF). The dilution ratio of sample to flux, the fusion temperature, the type and dosage of release agent were optimized. The results showed that the prepared sample slice was uniform and transparent without bubbles, which could meet the determination requirements, under the following conditions: the dilution ratio of sample to flux was 1∶10; 13-15 drops of 300g/L potassium iodide solution was selected as the release agent; the sample was fused at 1080℃ for 16min. In order to guarantee enough wide content range and proper content gradient of three components (silicon dioxide, aluminum oxide and iron trioxide) in calibration curves, three certified reference materials of alumina (YSS066-2013, YSS067-2013 and YSS068-2013) and the artificially synthesized calibration sample prepared with the above three certified reference materials according to certain mass ratio were employed to draw the calibration curve. The results showed that the linear correlation coefficients of calibration curves for test components were all higher than 0.998. The limit of detection of silicon dioxide, aluminum oxide and iron trioxide were 0.004%, 0.15% and 0.0026%, respectively. The proposed method was applied for the determination of silicon dioxide, aluminum oxide and iron trioxide in bauxite actual sample. The relative standard deviations (RSD, n=12) of determination results were between 0.41% and 1.2%. Two actual samples of bauxite and three artificially synthesized samples prepared with three certified reference materials (YSS066-2013, YSS067-2013 and YSS068-2013) according to certain mass ratio were determined according to the experimental method. The results were basically consistent with the theoretical values or those obtained by the titration method.
陈立平, 白旭, 杨亚茹, 宋文强. 熔融制样-X射线荧光光谱法测定铝矾土中二氧化硅、氧化铝和三氧化二铁[J]. 冶金分析, 2020, 40(3): 73-78.
CHEN Li-ping, BAI Xu, YANG Ya-ru, SONG Wen-qiang. Determination of silicon dioxide, aluminium oxide and iron trioxide in bauxite by X-ray fluorescence spectrometry with fusion sample preparation. , 2020, 40(3): 73-78.
胡璇,匡玉云,石磊.铬酸钡分光光度法测定高硫铝土矿中硫酸根[J].冶金分析,2018,38(12):59-63.HU Xuan,KUANG Yu-yun,SHI Lei.Determination of sulfate in high sulfur bauxite by barium chromate spectrophotometry[J].Metallurgical Analysis,2018,38(12):59-63.
[3]
崔俊燕.火焰原子吸收分光光度计测定铝土矿中氧化钾和氧化钠[J].山西建筑,2018,44(10):66-67.CUI Jun-yan.Determination of K2O,Na2O in bauxite using flame atomic absorption[J].Shanxi Architecture,2018,44(10):66-67.
[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仪同时测定铝土矿中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.Simul-taneous 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.
谢静思,甘学峰.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 Chemistry,2013,40(24):149-150.
[10]
严家庆,唐宇峰.X射线荧光光谱法快速测定铝土矿中的主组分[J].光谱实验室,2012,29(6):3690.YAN Jia-qing,TANG Yu-feng.Rapid determination of principal components in bauxite by X-ray fluorescence spectrometry[J].Chinese Journal of Spectroscopy Laboratory,2012,29(6):3690.
[11]
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):307-309.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):307-309.
[12]
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):531-534.PENG Nan-lan,HUA Lei,QIN Hong-yan.Determination of multiple elements in Wenshan bauxite by XRF spectrometry[J].Acta Mineralogica Sinica,2013,33(4):531-534.
[13]
黎红波,陈兵,张代云,等.X射线荧光光谱同时测定铝土矿石主次量组分[J].云南地质,2013,32(1):102-105.LI Hong-bo,CHEN Bing,ZHANG Dai-yun,et al.The synchronic testing of major and minor composition of bauxite with X-ray fluorescent spectrometry[J].Yunnan Geology,2013,32(1):102-105.
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.Simultneous 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.
[16]
王云霞,张健,庞玲,等.X射线荧光光谱法测定铝土矿中的主成分[J].理化检验:化学分册,2006,42(7):542-543.WANG Yun-xia,ZHANG Jian,PANG Ling,et al.XRFS determination of main components in bauxite[J].Physical Testing and Chemical Analysis Part B:Chemical Analysis,2006,42(7):542-543.
[17]
刘江滨,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):1211-1213.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):1211-1213.
[18]
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.
[19]
刘恒杰,贾海峰,谭清月.探究铝土矿中主成分的X射线荧光光谱分析[J].广东化工,2019,46(22):127-128.LIU Heng-jie,JIA Hai-feng,TAN Qing-yue.X-ray fluorescence spectroscopic analysis of main components in bauxite[J].Guangdong Industry,2019,46(22):127-128.
[20]
王贵.X射线荧光光谱在检验铝土矿石主成分中的应用[J].中国新技术新产品(China New Technologies and Products),2010(15):22-23.
[21]
袁汉章,刘洋,秦颖.铝土矿和赤泥的X射线荧光光谱测定[J].分析化学,1990(5):451-453.YUAN Han-zhang,LIU Yang,QIN Ying.Determination of bauxies and laterites by X-ray fluorescence spectrometry[J].Analytical Chemistry,1990(5):451-453.
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(1):71-73.ZHONG Dai-guo.X-ray fluorescence spectrometric analysis of major components in bauxite samples[J].Rock and Mineral Analysis,2008(1):71-73.
