Determination of Niobium and Tantalum in Geochemical Exploration Samples by ICP-MS with Acid Solution at Normal Pressure

Chang-sheng DENG; Sheng-fu LI; Jian-mei ZHANG; Ming-li WANG; Fu-he LE; Fang-hong NIU

doi:10.15898/j.cnki.11-2131/td.201802060016

Rock and Mineral Analysis > 2018 > 37(4): 364-370. > DOI: 10.15898/j.cnki.11-2131/td.201802060016

Chang-sheng DENG, Sheng-fu LI, Jian-mei ZHANG, Ming-li WANG, Fu-he LE, Fang-hong NIU. Determination of Niobium and Tantalum in Geochemical Exploration Samples by ICP-MS with Acid Solution at Normal Pressure[J]. Rock and Mineral Analysis, 2018, 37(4): 364-370. DOI: 10.15898/j.cnki.11-2131/td.201802060016

Citation:

PDF (2626 KB)

Determination of Niobium and Tantalum in Geochemical Exploration Samples by ICP-MS with Acid Solution at Normal Pressure

1.
No. 216 Geology Party, China National Nuclear Corporation, Urumqi 830011, China
2.
Xinjiang Institute of Measurement & Testing Technology, Urumqi 830013, China

More Information

Received Date: February 05, 2018
Revised Date: March 17, 2018
Accepted Date: June 10, 2018
Published Date: June 30, 2018

Abstract

HIGHLIGHTS
(1) The key problems for accurate determination of niobium and tantalum in geochemical samples are to improve the dissolution rate and inhibit hydrolysis.

(2) The dissolution rate of niobium and tantalum can be improved by adding sulphuric acid into the acid solution system.

(3) The extracting agent of 5% hydrofluoric acid-5% sulphuric acid-5% hydrogen peroxide and the method of standard material curves can effectively inhibit the hydrolysis of niobium and tantalum.

(4) The method of standard material curves can effectively reduce the matrix effect (non-mass spectral interference).

ABSTRACT

BACKGROUNDDue to its high digestion efficiency, low equipment cost and low detection limit, atmospheric acid dissolution is widely used in the geological laboratory. However, the commonly used four acid methods (hydrofluoric acid-nitric acid-hydrochloric acid-perchloric acid) is insufficient to dissolve niobium and tantalum. At the same time, niobium and tantalum would be partially adsorbed or would settle on the vessel caused by hydrolysis and polymerization reactions leading to the test results are lower than the real values.
OBJECTIVESTo determine accurately the concentrations of Nb and Ta in geochemical samples, and to solve the two key problems of the dissolution rate and hydrolysis of Nb and Ta in the solution.
METHODSFor the insufficiency of dissolution, sulphuric acid was introduced into the acid solution system. The acid solution system of hydrofluoric acid-nitric acid-hydrochloric acid-perchloric acid-sulphuric acid is used to completely dissolve niobium-tantalum in the sample. In view of the hydrolysis, extracting agent of 5% hydrofluoric acid-5% sulphuric acid-5% hydrogen peroxide was used. At the same time, the standard material curves were made using the same analytical process as the sample. The combination of these two methods effectively inhibited the hydrolysis of niobium-tantalum in sample solution. The method of standard material curves reduced the error caused by the matrix inconsistency between the sample solution and the standard solution in ICP-MS analysis.
RESULTSThe relative deviation was less than ±7% and the relative standard deviation was 3.11%-6.27% (n=11). The detection limits of niobium and tantalum were 0.04 μg/g and 0.03 μg/g, respectively. Compared with the detection limit of 0.33 μg/g by alkali fusion method, it has obvious advantages.
CONCLUSIONSBy changing the acid solution system, the extracting agent, and the method of standard material curves, the proposed method can be applied to measure niobium and tantalum in geochemical exploration samples.

FullText(HTML)

References (19)

References

李冰, 杨红霞.电感耦合等离子体质谱原理和应用[M].北京:地质出版社, 2005:144-147.

Li B, Yang H X.Principle and Application of Inductively Coupled Plasma Mass Spectrometry[M].Beijing:Geological Publishing House, 2005:144-147.

李冰, 杨红霞.电感耦合等离子体质谱(ICP-MS)技术在地学研究中的应用[J].地学前缘, 2003, 10(2):367-377. doi: 10.3321/j.issn:1005-2321.2003.02.015

Li B, Yang H X.Applications of inductively coupled plasma mass spectrometry in earth science[J].Earth Science Frontiers, 2003, 10(2):367-377. doi: 10.3321/j.issn:1005-2321.2003.02.015

岩石矿物分析编委会.岩石矿物分析(第四版第三分册)[M].北京:地质出版社, 2011:381-396.

The Editorial Committee of Rock and Mineral Analysis.Rock and Mineral Analysis (Fourth Edition:Volume Ⅲ)[M].Beijing:Geological Publishing House, 2011:381-396.

叶家瑜, 江宝林.区域地球化学勘查样品分析方法[M].北京:地质出版社, 2004:252.

Ye J Y, Jiang B L.Analysis Methods of Regional Geochemical Exploration Samples[M].Beijing:Geological Publishing House, 2004:252.

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. doi: 10.15898/j.cnki.11-2131/td.201512030223

Li G, Yao Y L, Li J Y, et al.Progress of niobium and tantalum analytical technology[J].Rock and Mineral Analysis, 2018, 37(1):1-14. doi: 10.15898/j.cnki.11-2131/td.201512030223

何红蓼, 李冰, 韩丽荣, 等.封闭压力酸溶-ICP-MS法分析地质样品中47个元素的评价[J].分析试验室, 2002, 21(5):8-12. doi: 10.3969/j.issn.1000-0720.2002.05.004

He H L, Li B, Han L R, et al.Evaluation of determining 47 elements in geological samples by pressurized acid digestion-ICP-MS[J].Chinese Journal of Analysis Laboratory, 2002, 21(5):8-12. doi: 10.3969/j.issn.1000-0720.2002.05.004

时晓露, 刘洪青, 孙月婷, 等.电感耦合等离子体质谱法测定岩石样品中的锆铌铪钽两种预处理方法的比较[J].岩矿测试, 2009, 28(5):427-430. doi: 10.3969/j.issn.0254-5357.2009.05.006

Shi X L, Liu H Q, Sun Y T, et al.Comparison of two different sample pretreatment methods in determination of Zr, Nb, Hf, Ta in rocks by inductively coupled plasma-mass spectrometry[J].Rock and Mineral Analysis, 2009, 28(5):427-430. doi: 10.3969/j.issn.0254-5357.2009.05.006

戴雪峰, 董利明, 代小吕.电感耦合等离子体质谱法测定地质样品中锆、铪、铌、钽、锡[J].广州化工, 2016, 44(14):117-120. doi: 10.3969/j.issn.1001-9677.2016.14.043

Dai X F, Dong L M, Dai X L.Determination of Zr, Hf, Nb, Ta and Sn in geological samples by inductively coupled plasma-mass spectrometry[J].Guangzhou Chemical Industry, 2016, 44(14):117-120. doi: 10.3969/j.issn.1001-9677.2016.14.043

马生凤, 温宏利, 巩爱华, 等.偏硼酸锂碱熔-电感耦合等离子体发射光谱法测定硫化物矿中硅酸盐相的主成分[J].岩矿测试, 2009, 28(6):535-540. doi: 10.3969/j.issn.0254-5357.2009.06.007

Ma S F, Wen H L, Gong A H, et al.Determination of major components in silicate phase of sulphide ores by ICP-AES with lithium metaborate fusion sample pretreatment[J].Rock and Mineral Analysis, 2009, 28(6):535-540. doi: 10.3969/j.issn.0254-5357.2009.06.007

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. doi: 10.3321/j.issn:0379-1726.2009.01.005

Tong C L, Liu Y S, Hu S H, 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. doi: 10.3321/j.issn:0379-1726.2009.01.005

闫红玲, 来新泽, 王琳, 等.常压混合酸溶矿-电感耦合等离子体发射光谱法测定铌钽[J].世界地质, 2011, 30(3):493-496. doi: 10.3969/j.issn.1004-5589.2011.03.027

Yan H L, Lai X Z, Wang L, et al.Dissolution with mixed acids under normal pressure-determination of niobium and tantalum by inductively coupled plasma atomic emission spectrometry[J].Global Geology, 2011, 30(3):493-496. doi: 10.3969/j.issn.1004-5589.2011.03.027

王小如.电感耦合等离子体质谱应用实例[M].北京:化学工业出版社, 2005:66-78.

Wang X R.Application Examples of Inductively Coupled Plasma Mass Spectrometry[M].Beijing:Chemical Industry Press, 2005:66-78.

马生凤, 温宏利, 李冰, 等.微波消解-耐氢氟酸系统电感耦合等离子体发射光谱法测定铌钽矿中的铌和钽[J].岩矿测试, 2016, 35(3):271-275. doi: 10.15898/j.cnki.11-2131/td.2016.03.009

Ma S F, Wen H L, Li B, et al.Determination of Nb and Ta in Nb-Ta ore by inductively coupled plasma-optical emission spectrometry with a combined microwave digestion hydrofluoric acid-resistant system[J].Rock and Mineral Analysis, 2016, 35(3):271-275. doi: 10.15898/j.cnki.11-2131/td.2016.03.009

Awaji S, Nakamura K, Nozaki T, et al.A simple method for precise determination of 23 trace elements in granitic rocks by ICP-MS after lithium tetraborate fusion[J].Resource Geology, 2010, 56(4):471-478. http://www.wanfangdata.com.cn/details/detail.do?_type=perio&id=JJ025667420

Hall G E M, Pelchat J C.Analysis of standard reference materials for Zr, Nb, Hf and Ta by ICP-MS after lithium metaborate fusion and cupferron separation[J].Geostandards & Geoanalytical Research, 1990, 14(1):197-206. doi: 10.1111/j.1751-908X.1990.tb00072.x

Munker C.Nb/Ta fractionation in a Cambrian arc/back arc system, New Zealand:Source constraints and application of refined ICP-MS techniques[J].Chemical Geology, 1998, 144(1-2):23-45. doi: 10.1016/S0009-2541(97)00105-8

胡家祯, 于亚辉, 吴娣, 等.电感耦合等离子体质谱法(ICP-MS)测定水系沉积物中的铌钽锆铪[J].矿产与地质, 2016, 30(4):699-702. doi: 10.3969/j.issn.1001-5663.2016.04.030

Hu J Z, Yu Y H, Wu D, et al.Determination of Nb, Ta, Zr, and Hf in stream sediment by inductively coupled plasma mass spectrometry (ICP-MS)[J].Mineral Resources and Geology, 2016, 30(4):699-702. doi: 10.3969/j.issn.1001-5663.2016.04.030

刘卫, 栾亚兰, 仵丽萍.电感耦合等离子体光谱法测定锂辉石选矿产品中铌和钽[J].理化检验(化学分册), 2006, 42(9):715-716. http://d.old.wanfangdata.com.cn/Periodical/lhjy-hx200609007

Liu W, Luan Y L, Wu L P.ICP-AES determination of Nb and Ta in products of oredressing of spodumene[J].Physical Testing and Chemical Analysis(Part B:Chemical Analysis), 2006, 42(9):715-716. http://d.old.wanfangdata.com.cn/Periodical/lhjy-hx200609007

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):224-248. doi: 10.15898/j.cnki.11-2131/td.2015.02.012

Yao Y L, Wu L K, Liu W, 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):224-248. doi: 10.15898/j.cnki.11-2131/td.2015.02.012

Supplements (0)

Cited By

Cited by

Periodical cited type(5)

1.	蔡宁波，王琳霖，鲍一遥，李怡普，万泽鑫，康志梅，罗胜元. 中扬子地台宜昌地区寒武系水井沱组优质页岩储层发育特征及天然气富集机理研究. 中国地质. 2025(01): 111-130 .
2.	石阳志，季永承，何叶，周芸，陈美军，江铭. 太阳浅层页岩气田有机碳含量预测及其影响因素分析. 能源与环保. 2024(01): 183-192 .
3.	马超，黄晓依，高胜天，刘鑫，王诚. 核磁共振技术在致密岩心孔隙量化表征中的应用. 中国科技论文. 2024(05): 540-546+574 .
4.	赵肖飞，李王鹏，葛勋，李沛，葛小瞳，刘雅利，吴海光，吕修祥. 松辽盆地北部林甸地区青山口组一段页岩储层特征及主控因素. 东北石油大学学报. 2024(06): 31-48+143-144 .
5.	田冲，李怡，黎丁源，张伟，钟可塑，周尚文，罗超，江文滨，李度，何亮，杨雪. 页岩储层孔隙度测定方法优选与推荐. 天然气工业. 2023(06): 57-65 .

Other cited types(1)

Get Citation

PDF

XML

Article views (1447) PDF downloads (70) Cited by(6)

Turn off MathJax

Article Contents

ABSTRACT

References

Determination of Niobium and Tantalum in Geochemical Exploration Samples by ICP-MS with Acid Solution at Normal Pressure

ABSTRACT

References

Cited by

Periodical cited type(5)

Other cited types(1)

Catalog

Export File

Citation

Format

Content