Determination of twelve rare earth elements in rock containing refractory metals by inductively coupled plasma atomic emission spectrometry with coprecipitation separation
LI Qiu-ying1, GAN Jian-zhuang1, WANG Ying-jin2, FANG Hai-yan1, HE Jiao1, SUN Qi1
1. Guiyan Detection Technology (yunnan) Co., Ltd., Kunming 650106, China; 2. State Key Laboratory of Advanced Technologies for Comprehensive Utilization of Platinum Metals, Sino-Platinum Metals Co., Ltd., Kunming 650106, China
Abstract：The accurate determination of rare earth elements was of great significance for the mining of rare earth elements in mine of rock containing refectory metals. The sample was fused with sodium peroxide in muffle furnace at 750℃. After cooling, the melt was transferred into a beaker with hydrochloric acid (1+4) followed by adding ammonia water into solution. The sample was used as carrier to remove sodium salts and metal ions which could react with ammonia to form ammonia complexation ions by coprecipitation separation. The precipitates were washed with diluted ammonia water and then dissolved with hot diluted hydrochloric acid. La, Ce, Sm, Eu, Gd, Tb, Ho, Er, Dy, Tm, Yb and Y in the test solution were determined by inductively coupled plasma atomic emission spectrometry (ICP-AES). Consequently,a determination method of the above twelve rare earth elements in rock containing refectory metals was established. The linear ranges of calibration curves of these elements were between 0.10μg/mL and 25μg/mL. The detection limits of method were between 0.20μg/g and 1.0μg/g. The contents of twelve rare earth elements (including La, Ce, Sm, Eu, Gd, Tb, Ho, Er, Dy, Tm, Yb and Y) in rock samples containing refectory metals were determined according to the experimental method. The relative standard deviations (RSD, n=9) of determination results were between 3.2% and 6.2%, and the recoveries were between 90% and 110%. The proposed method was applicable for the determination of rare earth elements (the mass fractions were in range of 0.001%-0.50%) in rock containing refectory metals.
李秋莹, 甘建壮, 王应进, 方海燕, 何姣, 孙祺. 共沉淀分离-电感耦合等离子体原子发射光谱法测定含难熔金属岩石中12种稀土元素[J]. 冶金分析, 2019, 39(12): 25-30.
LI Qiu-ying, GAN Jian-zhuang, WANG Ying-jin, FANG Hai-yan, HE Jiao, SUN Qi. Determination of twelve rare earth elements in rock containing refractory metals by inductively coupled plasma atomic emission spectrometry with coprecipitation separation. , 2019, 39(12): 25-30.
席永清,邱海鸥,李金莲,等.电感耦合等离子体原子发射光谱法同时测定地质样品中的Zr、Hf、Sc、Th[J].分析试验室,2005,24(9):40-43.XI Yong-qing,QIU Hai-ou,LI Jin-lian,et al.Simultaneous determination of Zr,Hf,Sc,Th in geological samples by inductively coupled plasma atomic emission spectrometry[J].Chinese Journal of Analysis Laboratory,2005,24(9):40-43.
[5]
高会艳.ICP-MS和ICP-AES测定地球化学勘查样品及稀土矿石中铌钽方法体系的建立[J].岩矿测试,2014,33(3):312-320.GAO Hui-yan.Determination of niobium and tantalum system in earth exploration samples and rare earth ores by ICP-MS and ICP-AES[J].Rock and Mineral Analysis,2014,33(3):312-320.
[6]
倪文山,张萍,姚明星,等.微波消解-电感耦合等离子体原子发射光谱法测定矿石样品中铌钽[J].冶金分析,2010,30(8):50-53.NI Wen-shan,ZHANG Ping,YAO Ming-xing,et al.Inductively coupled plasma atomic emission spectrometric determination of niobium and tantalum in ore sample after microwave digestion[J].Metallurgical Analysis,2010,30(8):50-53.
[7]
何蔓,胡斌,江祖成,等.单一稀土元素检测方法的新近进展[J].分析科学学报,2005,21(5):569-576.HE Man,HU Bin,JIANG Zu-cheng,et al.Recent progress in the detection of single rare earth elements[J].Journal of Analytical Science,2005,21(5):569-576.
[8]
赵金伟,封亚辉,程薇,等.电感耦合等离子体法测定高纯氧化铕中14个稀土和20个非稀土杂质[J].光谱学与光谱分析,2003,23(5):972-975.ZHAO Jin-wei,FENG Ya-hui,CHENG Wei,et al.Determination of 14 rare earth elements and 20 non rare earth impurities in high purity europium oxide by ICP-AES[J].Spectroscopy and Spectral Analysis,2003,23(5):972-975.
[9]
陈世焱,和振云.ICP-AES和ICP-MS法测定光学玻璃中15种稀土元素[J].分析测试技术与仪器,2011,17(4):217-222.CHEN Shi-yan,HE Zhen-yun.Determination of 15 rare earth elements in optical glass by ICP-AES and ICP-MS[J].Analysis and Testing Technology and Instruments,2011,17(4):217-222.
