Abstract:The contents of major, minor and micro components in aluminum ores have important influence on the production process and product quality. However, traditional analysis method cannot satisfy the detection requirements due to the tedious operation and long determination period. The sample was prepared by the fusion method. The samples were pre-oxidized by lithium nitrate for sample preparation under the following conditions: Li2B4O7-LiBO2 mixture [m(Li2B4O7)∶m(LiBO2)=12∶22] was selected as flux; the ratio between flux and sample was 10∶1; NH4I was employed as the releasing agent; the sample was fused at 1050℃ for 10min. The certified reference materials and their mixture with high purity aluminum oxide was used as calibrations sample. The spectral overlapping was investigated. The absorption enhancement effect among elements was corrected by variable theoretical α influence coefficient method. The simultaneous determination method of fifteen elements in aluminum ores (including Al2O3, SiO2, Fe2O3, CaO, MgO, P2O5, Na2O, K2O, TiO2, MnO, Ga2O3, ZrO2, V2O5, Cr2O3 and S) by X-ray fluorescence spectrometry (XRF) was developed. The precision test showed that relative standard deviations (RSD, n=9) were between 0.18% and 12%. The accuracy test was conducted using standard samples, and the found results were consistent with the certified values. The proposed method could simultaneously meet the determination requirements of various aluminum ores such as bauxite, pyrophyllite, mullite, aluminite and kaolin.
孟亚东,孙洛新,傅晓强,等.氟盐取代-EDTA滴定法测定铝土矿中铝量[J].岩矿测试,2008,27(6):475-476.MENG Ya-dong,SUN Luo-xin,FU Xiao-qiang,et al.Determination of aluminum in bauxites by fluorate replacement-EDTA titrimetry[J].Rock and Mineral Analysis,2008,27(6):475-476.
王志远.刚玉粉、高岭土、莫来石中铝、硅的测定[J].中国无机分析化学,2011,1(3):35-38.WANG Zhi-yuan.Quantitative determination of alumium and silicon elements in corundum,Kaolin clay and Mullite[J].Chinese Journal of Inorganic Analytical Chemistry,2011,1(3):35-38.
[4]
洪达峰.硅钼蓝分光光度法测定高岭土中二氧化硅[J].冶金分析,2017,37(10):59-64.HONG Da-feng.Determination of silicon dioxide in kaolin by silicon molybdenum blue spectrophotometry[J].Metallurgical Analysis,2017,37(10):59-64.
[5]
朱鲜红,李德生,张晶华,等.乙酸丁酯萃取火焰原子吸收光谱法测定铝土矿中微量镓[J].冶金分析,2004,24(6):63-65.ZHU Xian-hong,LI De-sheng,ZHANG Jing-hua,et al.Determination of micro gallium in bauxite by butyl acetate extraction and flame atomic absorption spectrometry[J].Metallurgical Analysis,2004,24(6):63-65.
[6]
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.
[7]
甘婷婷,赵南京,殷高方,等.水体中铬、镉和铅的X射线荧光光谱同时快速分析方法研究[J].光谱学与光谱分析,2017,37(6):1912-1918.GAN Ting-ting,ZHAO Nan-jing,YIN Gao-fang,et al.Study on simultaneous and rapid analysis method of X-ray fluorescence spectrum for determination of chromium,cadmium and lead in water[J].Spectroscopy and Spectral Analysis,2017,37(6):1912-1918.
[8]
仵利萍,曾英,刘卫,等.熔融制样-X射线荧光光谱法测定高钛渣主次量元素[J].矿产综合利用,2017(1):81-84.WU Li-ping,ZENG Ying,LIU Wei,et al.Determination of major and minor elements in high titanium slag by X-ray fluorescence spectrometry with samples of smelting process[J].Multipurpose Utilization of Mineral Resources,2017(1):81-84.
[9]
朱俐,王瑾,尹利辉.X射线荧光光谱法快速检测化妆品中的15种重金属[J].分析试验室,2017,36(9):1084-1087.ZHU Li,WANG Jin,YIN Li-hui.Rapid screening of 15 heavy metals in cosmetics by X-ray fluorescence spectrometry[J].Chinese Journal of Analysis Laboratory,2017,36(9):1084-1087.
[10]
Krishna A K,Khanna T C,Mohan K R.Rapid quantitative determination of major and trace elements in silicate rocks and soils employing fused glass discs using wavelength dispersive X-ray fluorescence spectrometry[J].Spectrochimica Acta Part B:Atomic Spectroscopy,2016,122:165-171.
[11]
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.
乌静,戴学谦,刘伟,等.X射线荧光光谱法测定铁矾土中二氧化硅、氧化铝和氧化铁[J].冶金分析,2009,29(7):44-48.WU Jing,DAI Xue-qian,LIU Wei,et al.Determination of silicon dioxide,aluminum oxide and ferric oxide in laterite by X-ray fluorescence spectrometry[J].Metallurgical Analysis,2009,29(7):44-48.
[14]
郭寿兴,吴玉庆.X射线荧光光谱法测定叶腊石中的铝铁钾钠[J].岩矿测试,1993,12(4):290-292.GUO Shou-xing,WU Yu-qing.Determination of Al, Fe, K and Na in pyrophyllite by XRF[J].Rock and Mineral Analysis,1993,12(4):290-292.
[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 Guo-hui,LI Xiao-li.Systematic study on the fusion sample preparation in X-ray fluorescence spectrometric analysis[J].Metallurgical Analysis,2015,35(7):1-9.
[16]
Fernand C,Jimmy S B.硼酸盐熔融的物理与化学[M].卓尚军,译.上海:华东理工大学出版社,2006:23.