Abstract:The accurate determination of major and minor components in bauxite is of great significance for the assigning of bauxite grade as well as the selection of smelting and production parameters.The content range of more than ten major and minor components in bauxite is usually wide,and two or more analysis methods are commonly employed for the determination.In this study, the certified reference material of bauxite and three certified reference materials of clay having similar composition with bauxite were used to prepare the calibration curve.The matrix effect was corrected by the variation theoretical α coefficient.Spectra plus software was used for the correction of loss on ignition (LOI).The method for the determination of major and minor components in bauxite(Al2O3,CaO,MgO,P2O5,Fe2O3,TiO2,MnO,SiO2,K2O and Na2O) by X-ray fluorescence spectrometry(XRF) with fusion sample preparation was established.The results showed that the uniform and transparent beads could be prepared under the following experimental conditions:the mixed flux of lithium tetraborate-lithium metaborate(mass ratio of 67∶33) was used as the flux;the dilution ratio was controlled at 1∶23;1.0 g of lithium nitrate was added into the mixture of sample and flux;the sample was peroxidized at 600 ℃ for 5 min and then fused at 1 075 ℃ for 10 min;total 50 mg of ammonium iodide was added in three batches as the release agent.The influence of two correction methods of loss on ignition(i.e., Spectra plus software and sample calcination) on the determination results of major and minor components in bauxite was investigated.The results showed that the results of two methods were basically consistent.One bauxite sample was determined in parallel for 11 times within one day by one analyst under same environment.The relative standard deviations (RSD,n=11) of determination results were between 0.20% and 4.1%.It was also determined in parallel for 11 times within 15 days by different analysts under same environment.The RSDs of determination results were between 0.25% and 4.7%.The contents of major and minor components in two bauxite samples were determined according to the experimental method,and the results were basically consistent with those obtained by titration or inductively coupled plasma atomic emission spectrometry(ICP-AES).
佡云, 马晓卉. 熔融制样-X射线荧光光谱法测定矾土中主次成分[J]. 冶金分析, 2024, 44(4): 79-86.
XIAN Yun, MA Xiaohui. Determination of major and minor components in bauxite by X-ray fluorescence spectrometry with fusion sample preparation. , 2024, 44(4): 79-86.
[1] 张满强.氟化物置换EDTA滴定法测定铝土矿中的三氧化二铝[J].新疆有色金属(Xinjiang Youse Jinshu),2018,41(1):94-95. [2] 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 Yuyun,SHI Lei.Determination of sulfate in high sulfur bauxite by barium chronate spectrophotometry[J].Metallurgical Analysis,2018,38(12):59-63. [3] 白万里,马慧侠,刘静,等.X射线荧光光谱法测定高铁铝土矿中8种组分[J].理化检验(化学分册),2018,54(8):973-979. BAI Wanli,MA Huixia,LIU Jing,et al.XRFS determination of 8 components in high ferric bauxites[J].Physical Testing and Chemical Analysis(Part B:Chemical Analysis),2018,54(8):973-979. [4] 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 Anjun,SU Mengxiao.Determination of major and minor components in medium-low grade bauxite and high-sulfur bauxite by wavelength dispersive X-ray fluorescence spetrometry[J].Metallurgical Analysis,2019,39(4):53-59. [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 Xianhong,LI Desheng,ZHANG Jinghua,et al.Determination of micro gallium in bauxite by butyl acetate extraction and flame atomic absorption spectometry[J].Metallurgical Analysis,2004,24(6):63-65. [6] 贾林.偏硼酸锂熔融-电感耦合等离子体发射光谱法测定铝土矿中多种元素[J].世界有色金属,2018(3):239-240. JIA Lin.Determination of elements of bauxite with lithium metaborate fusion inductively coupled plasma atomic emission spectrometry[J].World Nonferrous Metals,2018(3):239-240. [7] 孙红宾,刘贵磊,赵怀颖,等.偏硼酸锂熔融-ICP-AES法测定含刚玉铝土矿中主成分[J].分析试验室,2017,36(12):1429-1434. SUN Hongbin,LIU Guilei,ZHAO Huaiying,et al.Determination of main components in corundum-bearing bauxite by ICP-AES with lithium metaborate fusion method[J].Chinese Journal of Analysis Laboratory,2017,36(12):1429-1434. [8] BORKHODOEV V Y.Accuracy of the fundamental parameter method for X-ray fluorescence analysis of rocks[J].X-ray Spectrometry,2010,31(3):209-218. [9] NAKAYAMA K,NAKAMURA T.Calibrating standards using chemical reagents for glass bead X-ray fluorescence analysis of geochemical samples[J].X-ray Spectrometry,2010,37(3):204-209. [10] 严方,谢永杰.催化裂化催化剂中镍钒锑的测定[J].中国测试,2010,36(1):46-48. YAN Fang,XIE Yongjie.Determination of Ni,V,Sb on FCC catalysts[J].China Measurement &Test,2010,36(1):46-48. [11] BECKHOFF B,KOLBE M,HAHN O,et al.Reference-free X-ray fluorescence analysis of an ancient Chinese ceramic[J].X-ray Spectrometry,2010,37(4):462-465. [12] 洪琛,叶正隆,沈华荣,等.景德镇玲珑釉的测试与分析[J].中国测试,2014,40(2):56-60. HONG Chen,YE Zhenglong,SHEN Huarong,et al.Testing and analysis of rice-pattern glaze produced in Jingdezhen[J].China Measurement & Test,2014,40(2):56-60. [13] 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 Zhijun,CHEN Jing,CHEN Haofeng,et al.Simultaneous determination of major and minor components in sillicate and bauxite by X-ray fluorescence spectrometry with fusion sample preparation[J].Metallurgical Analysis,2015,35(7):73-78. [14] 张珂,吴园园,董登超,等.镁碳砖显微结构与成分分析方法的综合研究[J].中国测试,2016,42(2):51-55. ZHANG Ke,WU Yuanyuan,DONG Dengchao,et al.Comprehensive study on microstructure and composition analysis methods of magnesiacarbon brick[J].China Measurement &Test,2016,42(2):51-55. [15] 常利民,刘峰,王晓霞,等.基于熔融制样测量钛铁中5种成分的研究[J].中国测试,2017,43(S1):68-71. CHANG Limin,LIU Feng,WANG Xiaoxia,et al.Analyze the content of 5 elements in Ti-Fe based on melting method[J].China Measurement & Test,2017,43(S1):68-71. [16] 夏传波,赵伟,郑建业,等.熔融制样-X射线荧光光谱法测定硅藻土中6种主次组分[J].冶金分析,2019,39(2):40-45. XIA Chuanbo,ZHAO Wei,ZHENG Jianye,et al.Determination of six major and minor components in diatomite by X-ray fluorescence spectrometry with fusion sample preparation[J].Metallurgical Analysis,2019,39(2):40-45. [17] 李志明.熔融制样-X射线荧光光谱法同时测定铝土矿中18种主次量及痕量元素[J].中国金属通报(China Metal Bulletin),2020(4):185-186. [18] 孙家政,陆润洲,姜红,等.XRF结合化学计量学对牛皮纸物证的研究[J].中国测试,2022,48(5):77-82. SUN Jiazheng,LU Runzhou,JIANG Hong,et al.Study on kraft paper evidence by XRF combined with chemometrics[J].China Measurement & Test,2022,48(5):77-82. [19] 曲月华,王翠艳,王一凌,等.熔融制样-X射线荧光光谱法测定石灰石中5种组分[J].冶金分析,2013,33(12):29-33. QU Yuehua,WANG Cuiyan,WANG Yiling,et al.Determination of five components in limestone by X-ray fluorescence spectrometry with fusion sample preparation[J].Metallurgical Analysis,2013,33(12):29-33. [20] 杜登福,肖洪训,刘青桥.生石灰的X荧光光谱分析[J].冶金分析,2002,22(3):64-66. DU Dengfu,XIAO Hongxun,LIU Qingqiao.Determination of calces by XRF spectrometry[J].Metallurgical Analysis,2002,22(3):64-66.