Determination of rare earth distribution and non-rare earth impurities in battery grade mischmetal by inductively coupled plasma atomic emission spectrometry
ZHANG Gui-mei1, WANG Yun-wei2, GAO Han-bing3, ZHOU Xiao-dong1
1.Smelting Branch of Northern China Rare Earth(Group) High-tech Co., Ltd., Baotou 014010, China; 2. College of Mathematics and Statistics of Northeastern University, Qinhuangdao 066000, China; 3. College of Mechanical Engineering of Hunan Institute of Technology, Hengyang 421000, China
Abstract：The sample was dissolved with hydrochloric acid. The mixed standard solution series were prepared with the rare earth distribution(lanthanum, cerium, praseodymium and neodymium) and non-rare earth impurities (iron, silicon, zinc and magnesium) to draw the calibration curves. The total content of rare earth elements in standard solution series was consistent with those in sample solution to eliminate the matrix effect. The rare earth distribution (lanthanum, cerium, praseodymium and neodymium) and non-rare earth impurities (iron, silicon, zinc and magnesium) in battery grade mischmetal were simultaneously determined by inductively coupled plasma atomic emission spectrometry (ICP-AES). The analytical lines for testing elements were selected. The interference of rare earth elements to the non-rare earth impurities as well as the mutual interference among non-rare earth impurities was investigated. The correlation coefficients (r) of linear regression equations of calibration curves were higher than 0.998 8. The rare earth distribution including lanthanum, cerium, praseodymium and neodymium in synthetic sample were determined according to the experimental method. The found results were consistent with the theoretical values, and the relative standard deviations (RSD, n=11) were not more than 3.0%. The detection limit of non-rare earth impurities including iron, silicon, zinc and magnesium was between 0.001 0% and 0.002 8% (mass fraction). The low limit of determination was between 0.005 0% and 0.014% (mass fraction). The non-rare earth impurities in low-zinc low-magnesium battery grade mischmetal sample were determined, and the found results were consistent with the reference values. The RSD (n=11) was between 1.3% and 9.0%. The rare earth distribution (lanthanum, cerium, praseodymium and neodymium) and non-rare earth impurities (iron, silicon, zinc and magnesium) in actual battery grade mischmetal samples and lanthanum-rich metal samples were determined according to the experimental method, and the found results were basically consistent with those obtained by other analysis methods.
姚强,王燕,朱宇宏,等.X射线荧光光谱法测定稀土镁合金中镧、铈和镨含量[J].理化检验:化学分册,2013,49(12):1515-1516. YAO Qiang,WANG Yan, ZHU Yu-hong,et al.Determination of lanthanum,cerium and praseodymium contents in rare earth magnesium alloys by X-ray fluorescence spectrometry[J].Physical Testing and Chemical Analysis Part B:Chemical Analysis,2013,49(12):1515-1516.
[2]
施意华,邱丽,唐碧玉,等.电感耦合等离子体质谱法测定离子型稀土矿中离子相稀土总量及分量[J].冶金分析,2014,34(9):14-15.SHI Yi-hua,QIU Li,TANG Bi-yu,et al.Determination of total ionic-phase rare earth and component inion-adsorption rare earth ore by inductively coupled plasma mass spectrometry[J].Metallurgical Analysis,2014,34(9):14-15.
[3]
梁远明,陈美斯,李柏开.P507萃淋树脂分离稀土元素的研究[J].华南师范大学学报:自然科学版, 1986(2):61-65.LIANG Yuan-ming,CHEN Mei-si,LI Bo-kai.Study of separation rare earth elements by P507 extraction resin [J].Journal of South China Normal University:Natural Science Edition,1986(2):61-65.
[4]
张玻,贾江涛,廖春生,等.分光光度法测定混合稀土中的钕[J].稀有金属,2008(4):540-542.ZHANG Bo,JIA Jiang-tao,LIAO Chun-sheng,et al.Determinaton of neodymium in the mixed rare earth by spectrophotometry[J].Rare Metals,2008(4):540-542.
[5]
石如祥,张红玲.偶氮胂Ⅲ光度法测定无铅锡基焊料中稀土总量[J].冶金分析,2014,34(5):72-75.SHI Ru-xiang,ZHANG Hong-ling.Determination of total rare earth in lead-free tin-based solder by spectrophotometry with arsenazoⅢ[J].Metallurgical Analysis,2014,34(5):72-75.
[6]
崔爱端,张秀燕.ICP-AES法测定镨钕氧化物及镨钕金属中的镧、铈、钐、钇、铝和硅量[J].稀土,2006(4):75-77. CUI Ai-duan,ZHANG Xiu-yan.Determination of lanthanum, cerium, samarium, yttrium, aluminium and silicon contents in praseodymium neodymium oxide and praseodymium neodymium metal by inductively coupled plasma atomic emission spectrometry[J].Rare Earth,2006(4):75-77.
[7]
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(3): 218-223. DU Mei,LIU Xiao-jie.Determination of the total amount of rare earth in baotou rare earth mine by inductively coupled plasma emission spectrometry[J].Rock and Mineral Analysis,2014,33(3):218-223.
[8]
张杰,于永丽,戚淑芳,等.电感耦合等离子体原子发射光谱法测定轻稀土元素[J].冶金分析,2009,29(4): 20-23. ZHANG Jie,YU Yong-li,QI Shu-fang,et al.Determination of light rare earth elements by inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2009,29(4):20-23.
[9]
杜梅,许涛,吴文琪.稀土标准分析方法中稀土元素分析谱线的述评[J].稀土,2014(6):99-105. DU Mei,XU Tao,WU Wen-qi.Analysis spectral line review of rare earth elements in rare earth standard analysis method [J].Rare Earth,2014(6):99-105.
[10]
钱振彭,王长庆,陈维华.稀土元素ICP-AES光谱图[M].北京:冶金工业出版社,1982.
[11]
吴波英,黄少文. ICP-AES在稀土元素分析中的抗干扰技术的应用及进展[J].稀土,2005(5):20-25,63. WU Bo-ying,HUANG Shao-wen.Application and development of the correction techniques of interferences in the analysis of rare earth elements by ICP- AES [J].Rare Earth,2005(5):20-25,63.
