Professional Committee of Rock and Mineral Testing Technology of the Geological Society of China, National Geological Experiment and Testing CenterHost
2019 Vol. 38, No. 6
Article Contents

Jin-min SHI, Ting-jian FENG, Peng-fei FU, Yong-wu TANG, Da-lin CHEN, Chun-xiang ZHANG, Na YAN. Determination of Dispersed Elements in Metal Sulfide Ores by Inductively Coupled Plasma-Mass Spectrometry Using Microwave Digestion[J]. Rock and Mineral Analysis, 2019, 38(6): 631-639. doi: 10.15898/j.cnki.11-2131/td.201805300066
Citation: Jin-min SHI, Ting-jian FENG, Peng-fei FU, Yong-wu TANG, Da-lin CHEN, Chun-xiang ZHANG, Na YAN. Determination of Dispersed Elements in Metal Sulfide Ores by Inductively Coupled Plasma-Mass Spectrometry Using Microwave Digestion[J]. Rock and Mineral Analysis, 2019, 38(6): 631-639. doi: 10.15898/j.cnki.11-2131/td.201805300066

Determination of Dispersed Elements in Metal Sulfide Ores by Inductively Coupled Plasma-Mass Spectrometry Using Microwave Digestion

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  • BACKGROUNDCopper nickel and zinc concentrates all belong to metal sulfide minerals and are import commodities. The rapid and accurate analysis of dispersed elements in these samples is beneficial to the comprehensive utilization of mineral. However, the content of rare elements in such minerals is extremely low, and the properties of each element are different. In particular, Ge and Se cannot be precisely determined due to volatilization loss in wet digestion, and it is difficult to simultaneously measure various elements. OBJECTIVESTo simultaneously determine the various elements in the sample. METHODSCopper, zinc and nickel concentrates were used as representative sulfide minerals. The sample was pre-sealed by microwave digestion, and the content of rare elements was determined by inductively coupled plasma-mass spectrometry (ICP-MS). Simultaneous determination of various elements was realized. The experimental conditions of total solid solution, internal standard, mass spectrum interference elimination and pretreatment acid selection were compared. RESULTSDuring determination of Ga, Ge, Se, Cd, In, Te, La and Tl by microwave digestion in ICP-MS analysis, total amount of solid solution, internal standard, and mass spectrum interference elimination conditions was consistent in three types of metal sulfide ores. Unfortunately, the acid types were not the same. HNO3-HCl-HF-H2O2 system was more suitable for measuring Ga, Ge, Se, Cd, In, Te, La and Tl in nickel and zinc concentrates, and Ga, Ge, Se, Cd, In, La and Tl in copper concentrate. The recoveries of these elements ranged from 85.5% to 116.6%. The HCl-HNO3 (3:1) system was more suitable for detecting Te in copper concentrate. CONCLUSIONSThe method is simple, and the simultaneous determination of multiple elements is realized. Other factors of the method are the same, the acid digestion system is the key to selection.
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  • [1] 程秀花, 唐南安, 张明祖, 等.稀有分散元素分析方法的研究进展[J].理化检验(化学分册), 2013, 49(6):757-764.

    Google Scholar

    Cheng X H, Tang N A, Zhang M Z, et al.Recent advances of researches on analytical methods for rare and dispersed elements[J].Physical Testing and Chemical Analysis (Part B:Chemical Analysis), 2013, 49(6):757-764.

    Google Scholar

    [2] 程秀花, 黎卫亮, 郑民奇, 等.自制氢化物发生装置与电感耦合等离子体质谱仪联用测定地质样品中的稀散元素锗和碲[J].岩矿测试, 2016, 35(3):265-270.

    Google Scholar

    Cheng X H, Li W L, Zheng M Q, et al.Determination of germanium and tellurium in geological samples by a self-developed hydride generation device paired with inductively coupled plasma-mass spectrometer[J].Rock and Mineral Analysis, 2016, 35(3):265-270.

    Google Scholar

    [3] 杨俊衡.微波消解试样-原子荧光光谱法测定土壤中硒碲[J].理化检验(化学分册), 2008, 44(3):240-242.

    Google Scholar

    Yang J H.Microwave-assisted sample digestion AFS determination of Se and Te in soil[J].Physical Testing and Chemical Analysis (Part B:Chemical Analysis), 2008, 44(3):240-242.

    Google Scholar

    [4] Thangavel S, Dash K, Dhavile S M, et al.Determination of traces of As, B, Bi, Ga, Ge, P, Pb, Sb, Se, Si and Te in high-purity nickel using inductively coupled plasma optical emission spectrometry (ICP-OES)[J].Talanta, 2015, 131:505-509. doi: 10.1016/j.talanta.2014.08.026

    CrossRef Google Scholar

    [5] 程秀花, 黎卫亮, 王海蓉, 等.封闭酸溶样ICP-MS法直接测定地质样品中镓、铟、铊、锗[J].分析试验室, 2015, 34(10):1204-1208.

    Google Scholar

    Cheng X H, Li W L, Wang H R, et al.Determination of gallium, thallium and germanium in geological samples after pressurized acid digestion by in inductively coupled plasma-mass spectrometry[J].Chinese Journal of Analysis Laboratory, 2015, 34(10):1204-1208.

    Google Scholar

    [6] 王佳翰, 汤凯, 向懋笔, 等.密闭消解-电感耦合等离子体质谱法测定铅矿石中痕量镓铟铊镉锗[J].冶金分析, 2018, 38(12):19-25.

    Google Scholar

    Wang J H, Tang K, Xiang M B, et al.Determination of tracegallium, indium, thallum, cadmium and germaniumin lead ore by inductively coupled plasma mass spectrometry with closed digestion[J].Metallurgical Analysis, 2018, 38(12):19-25.

    Google Scholar

    [7] 张洁, 阳国运.树脂交换分离-电感耦合等离子体质谱法测定铅锌矿中钨钼锡锗硒碲[J].岩矿测试, 2018, 37(6):657-663.

    Google Scholar

    Zhang J, Yang G Y.Determination of tungsten, molybdenum, tin, germanium, selenium and tellurium in lead-zinc ore by inductively coupled plasma-mass spectrometry with resin exchange separation[J].Rock and Mineral Analysis, 2018, 37(6):657-663.

    Google Scholar

    [8] 陈浩凤, 于亚辉, 刘军, 等.电感耦合等离子体质谱法测定多金属矿中铟和铊[J].理化检验(化学分册), 2018, 54(2):220-222.

    Google Scholar

    Chen H F, Yu Y H, Liu J, et al.Determination of indium and bismuth in polymetallic ore by inductively coupled plasma mass spectrometry[J].Physical Testing and Chemical Analysis (Part B:Chemical Analysis), 2018, 54(2):220-222.

    Google Scholar

    [9] Satyanarayanan M, Balaram V, Sawant S S, et al.Rapid determination of REEs, PGEs, and other trace elements in geological and environmental materials by high resolution inductively coupled plasma mass spectrometry[J].Atomic Spectroscopy, 2018, 39(1):1-15.

    Google Scholar

    [10] 李湘, 王雪枫, 王奎, 等.氢化物发生-原子荧光光谱法同时测定铜精矿中硒和碲的含量[J].理化检验(化学分册), 2017, 53(1):64-67.

    Google Scholar

    Li X, Wang X F, Wang K, et al.Simultaneous determination of Se and Te in copper concentrate by HG-AFS[J].Physical Testing and Chemical Analysis (Part B:Chemical Analysis), 2017, 53(1):64-67.

    Google Scholar

    [11] 黎香荣, 罗明贵, 韦新红.微波消解-电感耦合等离子体质谱法测定锌精矿中痕量铊[J].冶金分析, 2016, 36(7):74-78.

    Google Scholar

    Li X R, Luo M G, Wei X H.Determination of trace thallium in zinc concentrate by microwave digestion-inductively coupled plasm mass spectrometry[J].Metallurgical Analysis, 2016, 36(7):74-78.

    Google Scholar

    [12] 李超, 刘英波, 刘维理.电感耦合等离子体质谱法测定铅精矿和锌精矿中铊的含量[J].云南冶金, 2016, 45(4):66-70. doi: 10.3969/j.issn.1006-0308.2016.04.015

    CrossRef Google Scholar

    Li C, Liu Y B, Liu W L.The determination on thallium content in lead and zinc concentrate by inductively coupled plasma mass spectrometry[J].Yunnan Metallurgy, 2016, 45(4):66-70. doi: 10.3969/j.issn.1006-0308.2016.04.015

    CrossRef Google Scholar

    [13] 王洪桂, 陶丽萍, 胡兰基.微波消解-电感耦合等离子体质谱法(ICP-MS)测定锌精矿中的铟和锗[J].中国无机分析化学, 2015, 5(1):38-40. doi: 10.3969/j.issn.2095-1035.2015.01.011

    CrossRef Google Scholar

    Wang H G, Tao L P, Hu L J.Determination of indium and germanium in zinc concentrate by microwave digestion-ICP-MS[J].Chinese Journal of Inorganic Analytical Chemistry, 2015, 5(1):38-40. doi: 10.3969/j.issn.2095-1035.2015.01.011

    CrossRef Google Scholar

    [14] 陈永欣, 黎香荣, 谢毓群, 等.微波消解-等离子体发射光谱法测定含铜物料中9种组分[J].岩矿测试, 2011, 30(2):200-204. doi: 10.3969/j.issn.0254-5357.2011.02.016

    CrossRef Google Scholar

    Chen Y X, Li X R, Xie Y Q, et al.Inductively coupled plasma-atomic emission spectrometric determination of 9 components in materials containing copper with microwave-assisted digestion[J].Rock and Mineral Analysis, 2011, 30(2):200-204. doi: 10.3969/j.issn.0254-5357.2011.02.016

    CrossRef Google Scholar

    [15] 杨丽飞, 苏明跃, 郭芬.铜精矿样品的高压密封微波消解方法研究[J].冶金分析, 2011, 31(11):58-62. doi: 10.3969/j.issn.1000-7571.2011.11.012

    CrossRef Google Scholar

    Yang L F, Su M Y, Guo F.Study on high pressure sealed microwave digestion method of copper concentrate samples[J]. Metallurgical Analysis, 2011, 31(11):58-62. doi: 10.3969/j.issn.1000-7571.2011.11.012

    CrossRef Google Scholar

    [16] 陈玉红, 王海舟, 张华, 等.微波消解电感耦合等离子体质谱法测定铝合金中多元素[J].冶金分析, 2008, 28(7):1-6. doi: 10.3969/j.issn.1000-7571.2008.07.001

    CrossRef Google Scholar

    Chen Y H, Wang H Z, Zhang H, et al.Determination of multi-elements in aluminum alloys by using microwave digestion inductively coupled plasma mass spectrometry[J].Metallurgical Analysis, 2008, 28(7):1-6. doi: 10.3969/j.issn.1000-7571.2008.07.001

    CrossRef Google Scholar

    [17] 陈波, 刘洪青, 邢应香.电感耦合等离子体质谱法同时测定地质样品中锗硒碲[J].岩矿测试, 2014, 33(2):192-196. doi: 10.3969/j.issn.0254-5357.2014.02.006

    CrossRef Google Scholar

    Chen B, Liu H Q, Xing Y X.Simultaneous determination of Ge, Se and Te in geological samples by inductively coupled plasma-mass spectrometry[J].Rock and Mineral Analysis, 2014, 33(2):192-196. doi: 10.3969/j.issn.0254-5357.2014.02.006

    CrossRef Google Scholar

    [18] 任丽.密闭消解-ICP-MS法测定地质样品中稀有、稀土、稀散元素[J].新疆有色金属, 2018, 41(2):93-95.

    Google Scholar

    Ren L.Determination of rare, rare earth and rare elements in geological samples by closed digestion-ICP-MS[J].Xinjiang Nonferrous Metals, 2018, 41(2):93-95.

    Google Scholar

    [19] 雷超海.微波消解-ICP-MS法测定昆布中15种稀土元素[J].广州化工, 2017, 45(5):68-69. doi: 10.3969/j.issn.1001-9677.2017.05.025

    CrossRef Google Scholar

    Lei C H.Determination of 15 rare earth elements in Ecklonia Kurome determinated with microwave digestion-ICP-MS[J].Guangzhou Chemical Industry, 2017, 45(5):68-69. doi: 10.3969/j.issn.1001-9677.2017.05.025

    CrossRef Google Scholar

    [20] 叶青, 刘林海, 肖莉红.湿法消解和微波消解微量滴定法测定铜试样中铜的含量[J].岩矿测试, 2007, 26(6):493-494. doi: 10.3969/j.issn.0254-5357.2007.06.015

    CrossRef Google Scholar

    Ye Q, Liu L H, Xiao L H.Determination of copper-containing samples by micro-titrimetry with wet digestion and microwave digestion[J].Rock and Mineral Analysis, 2007, 26(6):493-494. doi: 10.3969/j.issn.0254-5357.2007.06.015

    CrossRef Google Scholar

    [21] 于亚辉, 李振, 陈浩凤, 等.电感耦合等离子体质谱法测定岩石中的稀散元素锗[J].当代化工, 2016, 45(2):432-434. doi: 10.3969/j.issn.1671-0460.2016.02.074

    CrossRef Google Scholar

    Yu Y H, Li Z, Chen H F, et al.Determination of dilute element Ge in rock by inductively coupled plasma-mass spectrometry[J].Contemporary Chemical Industry, 2016, 45(2):432-434. doi: 10.3969/j.issn.1671-0460.2016.02.074

    CrossRef Google Scholar

    [22] 李华玲, 郑荣华, 沈加林.高分辨电感耦合等离子体质谱法测定地质样品中的微量锗[J].理化检验(化学分册), 2014, 50(9):1101-1103.

    Google Scholar

    Li H L, Zheng R H, Shen J L.High resolution ICP-MS determination of trace amout of germanium in geological samples[J].Physical Testing and Chemical Analysis (Part B:Chemical Analysis), 2014, 50(9):1101-1103.

    Google Scholar

    [23] 王洪桂, 肖娟, 陶丽萍.微波消解ICP-MS测试铅精矿中的铟和锗[J].中国非金属矿工业导刊, 2015(1):22-23. doi: 10.3969/j.issn.1007-9386.2015.01.008

    CrossRef Google Scholar

    Wang H G, Xiao J, Tao L P.Microwave digestion ICP-MS test of indium and germanium in Pb concentrate[J].China Non-Metallic Mining Industry Guide, 2015(1):22-23. doi: 10.3969/j.issn.1007-9386.2015.01.008

    CrossRef Google Scholar

    [24] 蒋天成, 刘守廷, 梁利诚, 等.微波消解ICP-MS法测定广西北部湾海鸭蛋中硒和锗的含量[J].化学分析计量, 2012, 21(4):27-30. doi: 10.3969/j.issn.1008-6145.2012.04.008

    CrossRef Google Scholar

    Jiang T C, Liu S T, Liang L C, et al.Determination of selenium and germanium in sea duck eggs from Guangxi Beibu Gulf by microwave digestion-inductively coupled plasma mass spectrometry[J].Chemical Analysis and Meterage, 2012, 21(4):27-30. doi: 10.3969/j.issn.1008-6145.2012.04.008

    CrossRef Google Scholar

    [25] 赵小龙, 燕娜, 侍金敏, 等.微波消解-电感耦合等离子体质谱法测定镍精矿中Ga、Ge、Se、Cd、In、Te、La和Tl[J].理化检验(化学分册), 2017, 53(9):1031-1035.

    Google Scholar

    Zhao X L, Yan N, Shi J M, et al.Determination of Ga, Ge, Se, Cd, In, Te, La and Tl in nickel concentrates by ICP-MS combined with microwave digestion[J].Physical Testing and Chemical Analysis (Part B:Chemical Analysis), 2017, 53(9):1031-1035.

    Google Scholar

    [26] 燕娜, 赵生国, 赵伟, 等.微波消解-电感耦合等离子体质谱测定铜精矿中7种稀有金属元素[J].岩矿测试, 2014, 33(2):197-202. doi: 10.3969/j.issn.0254-5357.2014.02.007

    CrossRef Google Scholar

    Yan N, Zhao S G, Zhao W, et al.Determination of seven rare metal elements in copper concentrates by inductively coupled plasma-mass spectrometry combined with microwave digestion[J].Rock and Mineral Analysis, 2014, 33(2):197-202. doi: 10.3969/j.issn.0254-5357.2014.02.007

    CrossRef Google Scholar

    [27] 李冰, 周剑雄, 詹秀春.无机多元素现代仪器分析技术[J].地质学报, 2011, 85(11):1878-1916.

    Google Scholar

    Li B, Zhou J X, Zhan X C.Inorganic multi-element modern instrument analysis technology[J].Acta Geologica Sinica, 2011, 85(11):1878-1916.

    Google Scholar

    [28] 孙朝阳, 董利明, 贺颖婷, 等.电感耦合等离子体质谱法测定地质样品中钪镓锗铟镉铊时的干扰及其消除方法[J].理化检验(化学分册), 2016, 52(9):1026-1030.

    Google Scholar

    Sun C Y, Dong L M, He Y T, et al.Elimination of interferences in ICP-MS determination of Se, Ga, Ge, In, Cd and Tl in geological samples[J].Physical Testing and Chemical Analysis (Part B:Chemical Analysis), 2016, 52(9):1026-1030.

    Google Scholar

    [29] 熊英, 吴赫, 王龙山.电感耦合等离子体质谱法同时测定铜铅锌矿石中微量元素镓铟铊钨钼的干扰消除[J].岩矿测试, 2011, 30(1):7-11. doi: 10.3969/j.issn.0254-5357.2011.01.002

    CrossRef Google Scholar

    Xiong Y, Wu H, Wang L S.Elimination of interference in simultaneous determination of trace Ga, In, Ta, W and Mo in copper, lead and zinc ores by inductively coupled plasma-mass spectrometry[J].Rock and Mineral Analysis, 2011, 30(1):7-11. doi: 10.3969/j.issn.0254-5357.2011.01.002

    CrossRef Google Scholar

    [30] 赵小学, 张霖琳, 张建平, 等.ICP-MS在环境分析中的质谱干扰及其消除[J].中国环境监测, 2014, 30(3):101-106. doi: 10.3969/j.issn.1002-6002.2014.03.022

    CrossRef Google Scholar

    Zhao X X, Zhang L L, Zhang J P, et al.Spectral interference and elimination of environmental analysis with ICP-MS[J].Environmental Monitoring in China, 2014, 30(3):101-106. doi: 10.3969/j.issn.1002-6002.2014.03.022

    CrossRef Google Scholar

    [31] 李国榕, 王亚平, 孙元方, 等.电感耦合等离子体质谱法测定地质样品中稀散元素铬镓铟碲铊[J].岩矿测试, 2010, 29(3):255-258. doi: 10.3969/j.issn.0254-5357.2010.03.012

    CrossRef Google Scholar

    Li G R, Wang Y P, Sun Y F, et al.Determination of Cr, Ga, In, Te and Tl in geological samples by inductively coupled plasma-mass spectrometry[J].Rock and Mineral Analysis, 2010, 29(3):255-258. doi: 10.3969/j.issn.0254-5357.2010.03.012

    CrossRef Google Scholar

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