Sample Treatment Methods for Determination of Rare Earth Elements in Manganese Ore by High-pressure Closed Digestion-Inductively Coupled Plasma-Mass Spectrometry

Lei WU; Yi-bo LIU; Jia-song WANG; Liang-ying WU; Nan ZHANG; Na WANG

doi:10.15898/j.cnki.11-2131/td.201712060189

2018 Vol. 37, No. 6

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Lei WU, Yi-bo LIU, Jia-song WANG, Liang-ying WU, Nan ZHANG, Na WANG. Sample Treatment Methods for Determination of Rare Earth Elements in Manganese Ore by High-pressure Closed Digestion-Inductively Coupled Plasma-Mass Spectrometry[J]. Rock and Mineral Analysis, 2018, 37(6): 637-643. doi: 10.15898/j.cnki.11-2131/td.201712060189

Citation:

Lei WU, Yi-bo LIU, Jia-song WANG, Liang-ying WU, Nan ZHANG, Na WANG. Sample Treatment Methods for Determination of Rare Earth Elements in Manganese Ore by High-pressure Closed Digestion-Inductively Coupled Plasma-Mass Spectrometry[J]. Rock and Mineral Analysis, 2018, 37(6): 637-643. doi: 10.15898/j.cnki.11-2131/td.201712060189

Sample Treatment Methods for Determination of Rare Earth Elements in Manganese Ore by High-pressure Closed Digestion-Inductively Coupled Plasma-Mass Spectrometry

1.
Tianjin Center of Geological Survey, China Geological Survey, Tianjin 300170, China
2.
Key Laboratory of Muddy Coast Geo-Environment, China Geological Survey, Tianjin 300170, China

Received Date: 06 December 2017

Revised Date: 30 May 2018

Accepted Date: 11 June 2018

Abstract

Abstract

BACKGROUNDWith advantages of small sample quantity, less acid, and low blank, high-pressure closed digestion-Inductively Coupled Plasma-Mass Spectrometry became the main method in the determination of rare earth elements. However, the composition of manganese ore is complex with varying manganese contents and different valence states of Mn, often with accompanying (co)producing metals and other impurities. The ore is difficult to digest completely using conventional acid-soluble systems, resulting in inaccurate ICP-MS analytical results. OBJECTIVESTo optimize the acid-solution system condition of the high-pressure closed digestion method, in order to completely and effectively digest the manganese ore with complex components and improve the accuracy of the results. METHODSThree standards GBW07261, GBW07263, GBW07266 and an unknown sample of manganese ore were digested using three different acid-solution systems of high-pressure closed digestion:Hydrofluoric acid-nitric acid closed digestion, extracted with nitric acid (Method 1); Hydrofluoric acid-nitric acid-hydrogen peroxide closed digestion, redissolved with nitric acid-hydrogen peroxide, extracted with nitric acid (Method 2); Hydrofluoric acid-nitric acid closed digestion, redissolved with hydrochloric acid, extracted with nitric acid (Method 3). The contents of rare-earth elements were then determined by ICP-MS. RESULTSMethods 2 and Methods 3 can completely digest manganese ore samples. The results of rare-earth elements by ICP-MS were similar, and were consistent with the results of conventional sodium peroxide fusion. However, during the experimental process, for samples with high manganese content, Method 3 required repeated additions of hydrochloric acid before the samples were completely digested, whereas Method 2 need only one repeat. The precision of Method 2 was 0.96%-2.68%, and the recovery was 95.0%-107.0%. CONCLUSIONSFor different manganese ore samples, Method 2 can completely digest the samples. The determination of rare earth elements was reliable by ICP-MS. Method 2 was the most suitable sample digestion method for the determination of rare earth elements in manganese ores.
- manganese ore /
- rare earth elements /
- high-pressure closed digestion /
- hydrogen peroxide /
- Inductively Coupled Plasma-Mass Spectrometry

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References

[1]	曹煊, 李景喜, 余晶晶, 等.电感耦合等离子体质谱法测定井间示踪剂中稀土元素[J].岩矿测试, 2009, 28(2):91-96. doi: 10.3969/j.issn.0254-5357.2009.02.001 CrossRef Google Scholar Cao X, Li J X, Yu J J, et al.Determination of rare earth elements in inter-well tracers by inductively coupled plasma-mass spectrometry[J].Rock and Mineral Analysis, 2009, 28(2):91-96. doi: 10.3969/j.issn.0254-5357.2009.02.001 CrossRef Google Scholar
[2]	杨小丽, 崔森, 杨梅, 等.碱熔离子交换-电感耦合等离子体质谱法测定多金属矿中痕量稀土元素[J].冶金分析, 2011, 31(3):11-16. doi: 10.3969/j.issn.1000-7571.2011.03.003 CrossRef Google Scholar Yang X L, Cui S, Yang M, et al.Determination of rare earth elements in polymetallic ore by inductively coupled plasma-mass spectrometry after alkali fusion and ion exchange[J].Metallurgical Analysis, 2011, 31(3):11-16. doi: 10.3969/j.issn.1000-7571.2011.03.003 CrossRef Google Scholar
[3]	安正泽, 张仁彪, 陈甲才, 等.贵州省松桃县道坨超大型锰矿床的发现及其成因探讨[J].矿床地质, 2014, 33(4):870-884. doi: 10.3969/j.issn.0258-7106.2014.04.016 CrossRef Google Scholar An Z Z, Zhang R B, Chen J C, et al.Geological and geochemical characteristics of Daotuo superlarge manganese ore deposit in Songtao county of Guizhou Province:Constraint on formation mechanism of Mn-carbonate ores[J].Mineral Deposits, 2014, 33(4):870-884. doi: 10.3969/j.issn.0258-7106.2014.04.016 CrossRef Google Scholar
[4]	裴浩翔, 付勇, 徐志刚, 等.贵州道坨锰矿菱锰矿的稀土元素特征[J].沉积与特提斯地质, 2015, 35(1):76-85. doi: 10.3969/j.issn.1009-3850.2015.01.010 CrossRef Google Scholar Pei H X, Fu Y, Xu Z G, et al.REE characteristics of rhodochrosite from the Daotuo manganese deposit in Guizhou[J].Sedimentary Geology and Tethyan Geology, 2015, 35(1):76-85. doi: 10.3969/j.issn.1009-3850.2015.01.010 CrossRef Google Scholar
[5]	Zarasvandi A, Rezaei M, Sadeghi M, et al.Rare-earth element distribution and genesis of manganese ores associated with Tethyan ophiolites, Iran:A review[J].Mineralogical Magazine, 2016, 80(1):127-142. doi: 10.1180/minmag.2016.080.054 CrossRef Google Scholar
[6]	徐静, 王志强, 李明来, 等.电感耦合等离子体发射光谱法测定镝铁电解粉中15种稀土元素[J].冶金分析, 2013, 33(7):25-29. doi: 10.3969/j.issn.1000-7571.2013.07.005 CrossRef Google Scholar Xu J, Wang Z Q, Li M L, et al.Determination of fifteen rare earth elements in Dy-Fe electrolysis dust by inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis, 2013, 33(7):25-29. doi: 10.3969/j.issn.1000-7571.2013.07.005 CrossRef Google Scholar
[7]	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, 35(6):99-103. Google Scholar Du M, Xu T, Wu W Q.Review of the analytical lines of rare earth elements in rare earth standard analysis methods[J].Chinese Rare Earths, 2014, 35(6):99-103. Google Scholar
[8]	刘晓杰, 郝茜, 金文莉, 等.ICP-AES法测定钕铁硼废料中稀土总量[J].稀土, 2014, 35(2):88-91. Google Scholar Liu X J, Hao Q, Jin W L, et al.Determination of tatal rare earth content in NdFeB waste by inductively coupled plasma-atomic emission spectrometry[J].Chinese Rare Earths, 2014, 35(2):88-91. Google Scholar
[9]	陈贺海, 荣德福, 付冉冉, 等.微波消解-电感耦合等离子体质谱法测定铁矿石中15个稀土元素[J].岩矿测试, 2013, 32(5):702-708. doi: 10.3969/j.issn.0254-5357.2013.05.005 CrossRef Google Scholar Chen H H, Rong D F, Fu R R, et al.Determination of fifteen rare-earth elements in iron ores using inductively coupled plasma mass spectrometry with microwave digestion[J].Rock and Mineral Analysis, 2013, 32(5):702-708. doi: 10.3969/j.issn.0254-5357.2013.05.005 CrossRef Google Scholar
[10]	吴磊, 曾江萍, 刘义博, 等.硼酸溶液敞口酸溶-电感耦合等离子体质谱法测定萤石中稀土元素[J].岩矿测试, 2014, 33(1):20-24. doi: 10.3969/j.issn.0254-5357.2014.01.004 CrossRef Google Scholar Wu L, Zeng J P, Liu Y B, et al.Determination of rare earth elements in fluorite samples by open boric acid dissolution and inductively coupled plasma-mass spectrometry[J].Rock and Mineral Analysis, 2014, 33(1):20-24. doi: 10.3969/j.issn.0254-5357.2014.01.004 CrossRef Google Scholar
[11]	赵艳芳, 尚德荣, 翟毓秀, 等.应用ICP-MS法研究我国三种经济海藻中稀土元素含量[J].光谱学与光谱分析, 2015, 35(11):3196-3199. Google Scholar Zhao Y F, Shang D R, Zhai Y X, et al.Application of ICP-MS to detect rare earth elements in three economic macroalgaes in China[J].Spectroscopy and Spectral Analysis, 2015, 35(11):3196-3199. Google Scholar
[12]	倪文山, 刘长淼, 姚明星, 等.电感耦合等离子体质谱法测定磷灰石中稀土元素分量和总量[J].冶金分析, 2016, 36(7):69-73. Google Scholar Ni W S, Liu C M, Yao M X, et al.Determination of the total amount of rare earth elements and its component in apatite by inductively coupled plasma mass spectrometry[J].Metallurgical Analysis, 2016, 36(7):69-73. Google Scholar
[13]	李小莉, 张勤.粉末压片-X射线荧光光谱法测定土壤、水系沉积物和岩石样品中15种稀土元素[J].冶金分析, 2013, 33(7):35-40. doi: 10.3969/j.issn.1000-7571.2013.07.007 CrossRef Google Scholar Li X L, Zhang Q.Determination of fifteen rare earth elements in soil, stream sediment and rock samples by X-ray fluorescence spectrometry with pressed powder pellet[J].Metallurgical Analysis, 2013, 33(7):35-40. doi: 10.3969/j.issn.1000-7571.2013.07.007 CrossRef Google Scholar
[14]	杨小丽, 李小丹, 邹棣华.溶样方法对电感耦合等离子体质谱法测定铝土矿中稀土元素的影响[J].冶金分析, 2016, 36(7):56-62. Google Scholar Yang X L, Li X D, Zou D H.Influence of sample dissolution method on determination of rare earth elements in bauxite by inductively coupled plasma-mass spectrometry[J].Metallurgical Analysis, 2016, 36(7):56-62. Google Scholar
[15]	吴葆存, 于亚辉, 闫红岭, 等.碱熔-电感耦合等离子体质谱法测定钨矿石和钼矿石中稀土元素[J].冶金分析, 2016, 36(7):39-45. Google Scholar Wu B C, Yu Y H, Yan H L, et al.Determination of rare earth elements in tungsten ore and molybdenum ore by inductively coupled plasma mass spectrometry with alkali fusion[J].Metallurgical Analysis, 2016, 36(7):39-45. Google Scholar
[16]	陈小燕, 吕茜茜, 吴勇.电感耦合等离子体质谱法测定含铜物料中的16种稀土元素[J].理化检验(化学分册), 2016, 52(5):545-548. Google Scholar Chen X Y, Lü Q Q, Wu Y.ICP-MS determination of 16 kinds of rare earth elements in materials containing copper[J].Physical Testing and Chemistry Analysis Part B (Chemistry Analysis), 2016, 52(5):545-548. Google Scholar
[17]	王佩佩, 李霄, 宋伟娇.微波消解-电感耦合等离子体质谱法测定地质样品中稀土元素[J].分析测试学报, 2016, 35(2):235-240. doi: 10.3969/j.issn.1004-4957.2016.02.017 CrossRef Google Scholar Wang P P, Li X, Song W J.Determination of rare earth elements in geological samples by ICP-MS using microwave digestion[J].Journal of Instrumental Analysis, 2016, 35(2):235-240. doi: 10.3969/j.issn.1004-4957.2016.02.017 CrossRef Google Scholar
[18]	贾双琳, 赵平, 杨刚, 等.混合酸敞开或高压密闭溶样-ICPMS测定地质样品中稀土元素[J].岩矿测试, 2014, 33(2):186-191. doi: 10.3969/j.issn.0254-5357.2014.02.005 CrossRef Google Scholar Jia S L, Zhao P, Yang G, et al.Quick determination of rare earth elements in geological samples with open acid digestion or high-pressure closed digestion by inductively coupled plasma-mass spectrometry[J].Rock and Mineral Analysis, 2014, 33(2):186-191. doi: 10.3969/j.issn.0254-5357.2014.02.005 CrossRef Google Scholar
[19]	高晶晶, 刘季花, 张辉, 等.高压密闭消解-电感耦合等离子体质谱法测定海洋沉积物中稀土元素[J].岩矿测试, 2012, 31(3):425-429. doi: 10.3969/j.issn.0254-5357.2012.03.007 CrossRef Google Scholar Gao J J, Liu J H, Zhang H, et al.Determination of rare earth elements in the marine sediments by inductively coupled plasma-mass spectrometry with high-pressure closed digestion[J].Rock and Mineral Analysis, 2012, 31(3):425-429. doi: 10.3969/j.issn.0254-5357.2012.03.007 CrossRef Google Scholar
[20]	岩石矿物分析编委会.岩石矿物分析(第四版第二分册)[M].北京:地质出版社, 2011:115-118. Google Scholar The Editorial Committee of Rock and Mineral Analysis.Rock and Mineral Analysis (Fourth Edition:Volume Ⅱ)[M].Beijing:Geological Publishing House, 2011:115-118. Google Scholar