Determination of total rare earths in light rare earth concentrate by X-ray fluorescence spectrometry with fusion sample preparation
JIANG Tian-yi1,2,3, WU Wen-qi1,2,3, ZHANG Shu-jie1,2,3, REN Xu-dong1,2,3, DU Mei1,2,3
1. National Engineering Research Center of Rare Earth Metallurgy and Functional Materials, Baotou 014030, China 2. Baotou Research Institute of Rare Earth, Baotou 014030, China 3. State Key Laboratory of Bayunobo Rare EarthResource Researches and Comprehensive Utilization, Baotou 014030, China
Abstract：The rare earth concentrate is the raw material for rare earth industry. The methods for determination of total rare earths in rare earth concentrate usually have complicated steps and long procedures. The total content of rare earths in light rare earth concentrate was determined by X-ray fluorescence spectrometry (XRF) with fusion sample preparation. The conditions for sample preparation and determination were explored. 6.0000g of anhydrous lithium tetraborate-lithium metaborate mixed flux (mass ratio of 2∶1) was accurately weighed and transferred into platinum-gold crucible. 0.5000g of lithium nitrate was used as oxidizing agent to eliminate the erosion of platinum-gold crucible by the reducing substances in sample. 0.6000g of rare earth concentrate sample was weighed. Then 0.5000g of boron oxide was uniformly covered on sample surface to prevent sample from spattering. 0.5mL of 20mg/mL ammonium bromide solution was dropwise added as the releasing agent. The crucible was placed into sample fusion machine which had been preheated to 1050℃. The sample was melted for 19min to prepare the wafer.Thus the mineral effect, ranularity effect and surface effect could be eliminated. The spectral lines of rare earth elements were properly selected to reduce the spectral interference. The spectral interference and matrix effect were corrected with empirical coefficient method. The calibration curves of rare earth elements were established using the certified reference materials of rare earth concentrate. The correlation coefficients of calibration curves were between 0.991 and 0.999 for all components. The relative standard deviation (RSD) was less than 0.5%. The determination results of total rare earths were consistent with those obtained by gravimetric method. The precision and accuracy of method could meet the production requirements.
许涛,王东杰,郝茜,等.钐钴合金中稀土总量的测定[J].稀土,2014,35(3):72-76.XU Tao,WANG Dong-jie,HAO Qian,et al.Determination of total rare contents in samarium-cobalt alloys[J].Chinese Rare Earths,2014,35(3):72-76.
[2]
于亚辉,许涛,刘晓杰,等.酸溶法测定稀土抛光粉废粉中的稀土总量[J].稀土,2015,36(2):82-85.YU Ya-hui,XU Tao,LIU Xiao-jie,et al.Determination of total rare earth contents in waste rare earth polishing powder by acid digestion method[J].Chinese Rare Earths,2015,36(2):82-85.
[3]
刘丽静,刘晓杰,高励珍.焙烧矿中稀土总量的测定——草酸盐重量法[J].稀土,2009,30(2):78-80.LIU Li-jing,LIU Xiao-jie,GAO Li-zhen.Determination of total rare earth ore roasting-oxalate gravimetric method[J].Chinese Rare Earths,2009,30(2):78-80.
[4]
张文娟,谢玲君,刘鸿.ICP-AES法测定氟碳铈矿中低含量稀土总量[J].有色金属科学与工程,2016,7(3):1-8.ZHANG Wen-juan,XIE Ling-jun,LIU Hong.Determination of low content total rare earth in bastnasite by ICP-AES[J].Nonferrous Metals Science and Engineering,2016,7(3):1-8.
[5]
杜梅,刘晓杰.电感耦合等离子体发射光谱法测定包头稀土矿中的稀土总量[J].岩矿测试,2014,33(2):218-223.DU Mei,LIU Xiao-jie.Determination of total rare earth contents in Baotou rare earth ores by inductively coupled plasma atomic emission spectrometry[J].Rock and Mineral Analysis,2014,33(2):218-223.
[6]
梁述廷.地质样品中稀土总量的X射线荧光分析法测定[J].矿物岩石,1997,17(1):117-120.LIANG Shu-ting.Determination of total rare earth in geological samples by X-ray fluorescence analysis[J].Journal of Mineralogy and Petrology,1997,17(1):117-120.
[7]
张仕定,梁述廷,聂全新,等. XRFA法快速测定地质样品中的稀土总量[J].地质实验室,1992,8(6):335-337.ZHANG Shi-ding,LIANG Shu-ting,NIE Quan-xin,et al.Rapid determination of total rare earths in geological samples by XRFA[J].Geology Laboratory,1992,8(6):335-337.
[8]
程泽,刘晓光,谭玉娟,等.X射线荧光光谱法测定矿物中轻重稀土[J].2005,24(1):79-80.CHENG Ze,LIU Xiao-guang,TAN Yu-juan,et al.Determination of light and heavy rare earths in minerals by X-ray fluorescence spectrometry[J].Rock and Mineral Analysis,2005,24(1):79-80.
[9]
郭成才,陈艳.稀土精矿中镧、铈、镨、钕、钐、钆、钇X荧光光谱的直接测定[J].稀土,1996,17(3):70-71.GUO Cheng-cai,CHEN Yan.Determination of lanthanum,cerium,praseodymium,neodymium,samarium, gadolinium,yttrium in rare earth concentrates by X-ray fluorescence spectroscopy[J].Chinese Rare Earths,1996,17(3):70-71.
[10]
逯义. X射线荧光光谱法测定稀土精矿中的稀土元素分量[J].岩矿测试,2012,31(2):277-281.LU Yi.Determination of rare earth elements in rare earth concentrate X-ray fluorescence spectrometry[J].Rock and Mineral Analysis,2012,31(2):277-281.
[11]
德喜,王世武.X射线荧光光谱法测定稀土精矿各组份[J].冶金分析,1999,19(1):26-28.DE Xi,WANG Shi-wu.Determination of the components in rare earth concentrates by X-ray fluorescence spectrometry[J].Metallurgical Analysis,1999,19(1):26-28.
