Determination of niobium and tantalum in niobium-tantalum concentrate by inductively coupled plasma atomic emission spectrometry
ZHAN Da-chuan1,2, YANG Guo-yun*1,2, WU Ming-li1, NIE Xiao-yan1, PAN Qian-ni1,2
1. Key Laboratory of Radioactive and Rare Scattered Mineral Comprehensive Utilization, Ministry of Natural Resources, Mineral Application Institute of Guangdong Provincial, Shaoguan 512026, China; 2. Geology & Mineral Analysis & Test Research Center of Guangxi Zhuang Autonomous Region, Nanning 530023, China
Abstract：The accurate analysis of niobium and tantalum contents in niobium-tantalum concentrate is of great significance for the dressing and smelting as well as the development of new materials. The sample was digested by alkali fusion (fusion at 720℃ for 20min) in silver crucible using sodium hydroxide as the flux. After acid dissolution, the contents of niobium and tantalum in niobium-tantalum concentrate were determined by inductively coupled plasma atomic emission spectrometry (ICP-AES). The digestion methods of sample, the selection of internal standard elements and analytical line pairs, and the influence of coexisting elements were investigated. The results showed that cobalt and chromium was selected as the internal standard element for niobium and tantalum, respectively. The analytical line and internal standard line was Nb 309.4nm-Co 345.3nm and Ta 240.0nm-Cr 284.3nm, respectively. The coexisting elements such as aluminum, silicon, potassium, sodium, calcium, magnesium, copper, lead, zinc, sulfate, manganese, phosphorus, chromium, barium, cobalt, arsenic, nickel, strontium, beryllium, scandium and tin had no interference with the determination of niobium and tantalum. The limit of detection of niobium and tantalum was 0.007% and 0.011%, respectively. The contents of niobium and tantalum in four actual niobium-tantalum concentrate samples were determined according to the experimental method. Meanwhile, the average values of determination results in several laboratories were used as the recommended values for comparison. It indicated that the relative standard deviations (RSD, n=10) of determination results for niobium and tantalum were all less than 0.6%. The relative error was within ±5%.
殷学峰,崔军,董玉兰.纸上色层重量法测定铌矿和铌渣中五氧化二铌[J].冶金分析,2003,23(5):74-75.YIN Xue-feng,CUI Jun,DONG Yu-lan.Determination of niobium pentoxide in niobium residue by paper chromatographic analyses[J].Metallurgical Analysis,2003,23(5):74-75.
[2]
Nagiev K D.Spectrophotometric determination of simultaneously present niobium and tantalum[J].Journal of Analytical Chemistry,2004,59(10):930-934.
[3]
Motlalepula N,Walter P,Johann T N.Hydrometallurgical separation of niobium and tantalum: A fundamental approach[J].JOM,2016,68(2):556-566.
[4]
Cheng Y.Determination of alloy and impurity elements in the WC-Co based cemented carbide by microwave digestion-inductively coupled plasma atomic emission spectrometry[J].Applied Mechanics and Materials,2012,271-272:222-226.
[5]
姚玉玲,吴丽琨,刘卫,等.乙醇增敏-电感耦合等离子体发射光谱法测定矿石及选冶样品中的铌钽[J].岩矿测试,2015,34(2):224-228.YAO Yu-ling,WU Li-kun,LIU Wei,et al.Determination of Nb and Ta in ores and metallurgical samples by inductively coupled plasma-atomic emission spectrometry with ethanol as a sensitizer[J].Rock and Mineral Analysis,2015,34(2):224-228.
[6]
张军,陈慧连,曾宇斌.两种铌钽矿石消解方法的对比研究[J].广州化工,2014,42(10):120-122.ZHANG Jun,CHEN Hui-lian,ZENG Yu-bin.A comparative study of two kinds of niobium tantalum ore digestion method[J].Guangzhou Chemical Industry,2014,42(10):120-122.
[7]
李刚,姚玉玲,李婧祎,等.铌钽元素分析技术新进展[J].岩矿测试,2018,37(1):1-14.LI Gang,YAO Yu-ling,LI Jing-yi,et al.Progress of niobium and tantalum analytical technology[J].Rock and Mineral Analysis,2018,37(1):1-14.
[8]
童春临,刘勇胜,胡圣虹,等.ICP-MS分析用地质样品制备过程中Nb、Ta等元素的特殊化学行为[J].地球化学,2009,38(1):43-52.TONG Chun-lin,LIU Yong-sheng,HU Sheng-hong,et al.Specific chemical behavior of Nb and Ta in geological sample preparation with PTFE bomb for ICP-MS analysis[J].Geochimica,2009,38(1):43-52.
[9]
艾军,汤志勇.流动注射在线液-液萃取-ICP-AES测定土壤和化探样品中痕量铌和钽[J].光谱学与光谱分析,2001,21(5):658-660.AI Jun,TANG Zhi-yong.On-line determination of niobium and tantalum in soil and geochemical exploration samples by inductively coupled plasma atomic emission spectrometry with solvent extraction flow injection[J].Spectroscopy and Spectral Analysis,2001,21(5):658-660.
[10]
庄艾春,肖红新.碱熔-等离子体发射光谱法快速测定钽铌矿中钽和铌[J].广东化工,2018,45(9):222-223.ZHUANG Ai-chun,XIAO Hong-xin.Rapid determination of tantalum and niobium in tantalum niobium mine by alkali fusion plasma emission spectrometry[J].Guangdong Chemical Industry,2018,45(9):222-223.
[11]
王红丽,郑娟.焦硫酸钾熔融-电感耦合等离子体发射光谱法测定矿石中的铌、钽含量[J].低碳世界,2016,25:76-77.WANG Hong-li,ZHENG Juan.Determination of niobium and tantalum in ore by inductively coupled plasma emission spectrometry with alkali fusion with potassium pyrosulfate[J].Low Carbon World,2016,25:76-77.
[12]
刘环,康佳红,王玉学.碱熔-电感耦合等离子体质谱法测定地质样品中铍铯镓铊铌钽锆铪铀钍[J].冶金分析,2019,39(3):26-32.LIU Huan,KANG Jia-hong,WANG Yu-xue.Determination of beryllium,cesium,gallium,thallium,niobium,tantalum,zirconium,hafnium,uranium and thorium in geological sample by inductively coupled plasma mass spectrometry with alkali fusion[J].Metallurgical Analysis,2019,39(3):26-32.
