Determination of total amount of fifteen rare earth elements and its component in Bayan Obo ore by inductively coupled plasma mass spectrometry
ZHOU Kaihong1, ZHANG Lifeng1,2, LI Jia2
1. Baotou Research Institute of Rare Earths,State Key Laboratory of Baiyunobo Rare Earth Resource Researches and Comprehensive Utilization, Baotou 014030, China; 2. National Engineering Research Centre of Rare Earth Metallurgy and Funcional Materials, Baotou 014030, China
Abstract：Bayan Obo ores are typical lattice minerals, containing insoluble minerals such as niobium, zirconium, and titanium, which are difficult to be completely dissolved by conventional acid solution treatment. In experiments, Bayan Obo ore sample was melted and decomposed by sodium hydroxide and sodium peroxide. After leaching with hot water and alkali separation, the filter paper and the precipitate were destroyed and dissolved with hydrochloric acid and hydrogen peroxide. 1% hydrochloric acid was used as the measurement medium. The mass concentration of the matrix was controlled below 0.5 g/L. Cs was selected as internal standard to eliminate the matrix effect. Accordingly, the determination of total amount of fifteen rare earth elements (including lanthanum, cerium, praseodymium, neodymium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium, and yttrium) and its component in Bayan Obo ore by inductively coupled plasma mass spectrometry (ICP-MS) was established. The experiments showed that the mass concentration of each rare earth element in range of 5.00-100.0 ng/mL (in oxide, similarly hereinafter) had a good linear relationship with the intensity ratio between rare earth element and internal standard. The correlation coefficients were not less than 0.999 6. The limits of detection were in range of 0.010-0.034 ng/mL, and the limits of quantification were in range of 0.030-0.10 ng/mL. The total amount of fifteen rare earth elements and its component in Bayan Obo ore were determined according to the experimental method. The found results were basically consistent with those obtained by inductively coupled plasma atomic emission spectrometry or X-ray fluorescence spectrometry. The relative standard deviations (RSD, n=6) were between 1.0% and 4.9%. The spiked recoveries ranged from 95% to 105%. The proposed method was applied for the determination of total amount and its component of rare earth elements in certified reference materials. The measured results were basically consistent with the certified values.
周凯红, 张立锋, 李佳. 电感耦合等离子体质谱法测定白云鄂博矿石中15种稀土元素总量及其分量[J]. 冶金分析, 2022, 42(8): 87-95.
ZHOU Kaihong, ZHANG Lifeng, LI Jia. Determination of total amount of fifteen rare earth elements and its component in Bayan Obo ore by inductively coupled plasma mass spectrometry. , 2022, 42(8): 87-95.
[1] 秦玉芳,王其伟,金海龙,等.白云鄂博矿霓石型稀土矿石中铌的赋存状态与分布规律研究[J].矿产保护与利用,2021,41(3):144-149. QIN Yufang,WANG Qiwei,JIN Hailong,et al.Occurrence and distribution of niobium in aegirine-type rare earth ore in Bayan Obo mine[J].Conservation and Utilization of Mineral Resources,2021,41(3):144-149. [2] 柯昌辉,孙盛,赵永岗,等.内蒙古白云鄂博超大型稀土-铌-铁矿床控矿构造特征及深部找矿方向[J].地质通报,2021,40(1):95-109. KE Changhui,SUN Sheng,ZHAO Yonggang,et al.Ore-controlling structure and deep prospecting of the Bayan Obo large-sized REE-Nb-Fe ore deposit,Inner Mongolia[J].Geological Bulletin of China,2021,40(1):95-109. [3] 李潇雨,惠博,熊文良,等.白云鄂博稀土资源综合利用现状概述[J].矿产综合利用,2021(5):17-24. LI Xiaoyu,HUI Bo,XIONG Wenliang,et al.Multipurpose utilization of rare earth resources in Bayan Obo[J].Multipurpose Utilization of Mineral Resources,2021(5):17-24. [4] 谢玉玲,曲云伟,杨占峰,等.白云鄂博铁、铌、稀土矿床:研究进展、存在问题和新认识[J].矿床地质,2019,38(5):983-1003. XIE Yuling,QU Yunwei,YANG Zhanfeng,et al.Giant Bayan Obo Fe-Nb-REE deposit:Progresses,controversaries and new understandings[J].Mineral Deposits,2019,38(5):983-1003. [5] 吴石头,王亚平,孙德忠,等.电感耦合等离子体发射光谱法测定稀土矿石中15种稀土元素-四种前处理方法的比较[J].岩矿测试,2014,33(1):12-19. WU Shitou,WANG Yaping,SUN Dezhong,et al.Determination of 15 rare earth elements in rare earth ores by inductively coupled plasma-atomic emission spectrometry: a comparison of four different pretreatment methods[J].Rock and Mineral Analysis,2014,33(1):12-19. [6] 杜芳艳.3-噻唑偶氮-5-氨基苯酚分光光度法测定铝矿石中稀土总量[J].冶金分析,2007,27(1):64-66. DU Fangyan.Spectrophotometric determination of total rare earths in aluminum ore with 3-thiazolylazo-5-amino phenol[J].Metallurgical Analysis,2007,27(1):64-66. [7] 文伟,张覃,解田,等.偶氮类显色剂用于含稀土磷矿石中稀土含量测定[J].稀土,2010,31(6):56-60. WEN Wei,ZHANG Qin,XIE Tian,et al.Determination of RE content in phosphate ores bearing rare earth with azo reagents[J].Chinese Rare Earths,2010,31(6):56-60. [8] 刘小林.电感耦合等离子体发射光谱法直接测定稀土矿石中15种稀土元素[J].化工设计通讯,2017,43(2):108-109. LIU Xiaolin.Direct determination of 15 rare earth elements in rare earth ore by inductively coupled plasma atomic emission spectrometry[J].Chemical Engineering Design Communications,2017,43(2):108-109. [9] 胡璇.电感耦合等离子体发射光谱法测定铝土矿中的稀土氧化物[J].岩矿测试,2020,39(6):954-960. HU Xuan.Determination of rare earth oxides in bauxite by inductively coupled plasma optical emission spectrometry[J].Rock and Mineral Analysis,2020,39(6):954-960. [10] 于丽丽.熔融制样-X射线荧光光谱法测定轻稀土矿石中8种主量稀土氧化物[J].冶金分析,2019,39(10):37-42. YU Lili.Determination of eight major rare earth oxides in light rare earth ore by X-ray fluorescence spectrometry with fusion sample preparation[J].Metallurgical Analysis,2019,39(10):37-42. [11] 肖志博.X荧光光谱法测定矿石中的稀土元素[J].世界有色金属,2019(12):130-131. XIAO Zhibo.Determination of rare earth elements by X-fluorescence spectrometry[J].World Nonferrous Metals,2019(12):130-131. [12] 梁亚丽,杨珍,阿丽莉,等.ICP-MS法测定钼矿石中伴生锂、镓和稀土元素[J].吉林大学学报(理学版),2021,59(2):427-434. LIANG Yali,YANG Zhen,A Lili,et al.Determination of associated lithium, gallium and rare earth elements in molybdenum ore by inductively coupled plasma mass spectrometry method[J].Journal of Jilin University(Science Edition),2021,59(2):427-434. [13] 康金春,李端婷.微波消解-ICP-MS测定岩土中稀土元素的试验研究[J].化学与粘合,2021,43(3):231-233. KANG Jinchun,LI Duanting.Determination of rare earth elements in rock and soil by microwave digestion ICP-MS method[J].Chemistry and Adhesion,2021,43(3):231-233. [14] 苏春风.电感耦合等离子体质谱(ICP-MS)法测定稀土矿中16种稀土元素含量[J].中国无机分析化学,2020,10(6):28-32. SU Chunfeng.Determination of 16 rare earth elements in rare earth ores by inductively coupled plasma mass spectrometry[J].Chinese Jorunal of Inorganic Analytical Chemistry,2020,10(6):28-32. [15] 张立锋,刘杰民,张翼明.电感耦合等离子体质谱法测定白云鄂博矿区土壤及植物中稀土总量[J].稀土,2016,37(4):106-112. ZHANG Lifeng,LIU Jiemin,ZHANG Yiming.Determination of total rare earth in soil and plants in Bayan Obo mining area by inductively coupled plasma mass spectrometry[J].Chinese Rare Earths,2016,37(4):106-112. [16] 张立锋,周凯红,张翼明,等.微波消解-电感耦合等离子体质谱法测定羊体各部位稀土总量[J].稀土,2019,40(6):96-104. ZHANG Lifeng,ZHOU Kaihong,ZHANG Yiming,et al.Determination of total content of rare earth in different parts of sheep by microwave digestion-inductively coupled plasma mass spectrometry[J].Chinese Rare Earths,2019,40(6):96-104. [17] 陈忠颖,刘巍,郭颖.电感耦合等离子体质谱法测定高纯铁中21种元素时的基体效应[J].理化检验(化学分册),2017,53(12):1416-1418. CHEN Zhongying,LIU Wei,GUO Ying.Matrix effect in the ICP-MS determination of 21 elements in high purity iron[J].Physical Testing and Chemical Analysis (Part B:Chemical Analysis),2017,53(12):1416-1418. [18] 刘曙,干兆祥,闵红.电感耦合等离子体质谱分析中金属元素的基体效应[J].冶金分析,2021,41(12):79-86. LIU Shu,GAN Zhaoxiang,MIN Hong.Matrix effect of metal elements in inductively coupled plasma mass spectrometry[J].Metallurgical Analysis,2021,41(12):79-86. [19] 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 Xiaojie.Determination of total rare earth contents of Baotou rare earth concentrates by inductively coupled plasma atomic emission spectrometry[J].Rock and Mineral Analysis,2014,33(2):218-223. [20] 周伟,曾梦,王健,等.熔融制样-X射线荧光光谱法测定稀土矿石中的主量元素和稀土元素[J].岩矿测试,2018,37(3):298-305. ZHOU Wei,ZENG Meng,WANG Jian,et al.Determination of major and rare earth elements in rare earth ores by X-ray fluorescence spectrometry with fusion sample preparation[J].Rock and Mineral Analysis,2018,37(3):298-305.
