Determination of 15 Rare Earth Elements in Phosphate Ores by Inductively Coupled Plasma-Mass Spectrometry with Atmospheric Pressure Closed Microwave Digestion

ZHANG Nan; ZHENG Zhikang; WANG Jiasong; ZENG Jiangping

doi:10.15898/j.ykcs.202301110004

2024 Vol. 43, No. 2

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Article navigation > Rock and Mineral Analysis > 2024 > 43(2): 366-374

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ZHANG Nan, ZHENG Zhikang, WANG Jiasong, ZENG Jiangping. Determination of 15 Rare Earth Elements in Phosphate Ores by Inductively Coupled Plasma-Mass Spectrometry with Atmospheric Pressure Closed Microwave Digestion[J]. Rock and Mineral Analysis, 2024, 43(2): 366-374. doi: 10.15898/j.ykcs.202301110004

Citation:

ZHANG Nan, ZHENG Zhikang, WANG Jiasong, ZENG Jiangping. Determination of 15 Rare Earth Elements in Phosphate Ores by Inductively Coupled Plasma-Mass Spectrometry with Atmospheric Pressure Closed Microwave Digestion[J]. Rock and Mineral Analysis, 2024, 43(2): 366-374. doi: 10.15898/j.ykcs.202301110004

Determination of 15 Rare Earth Elements in Phosphate Ores by Inductively Coupled Plasma-Mass Spectrometry with Atmospheric Pressure Closed Microwave Digestion

1.
Tianjin Center, China Geological Survey, Tianjin 300170, China
2.
North China Geological Science and Technology Innovation Center, Tianjin 300170, China
3.
Key Laboratory of Coast Geo-Environment, China Geological Survey, Tianjin 300170, China

More Information

Corresponding author: ZENG Jiangping, zengjiangping@163.com

Received Date: 11 January 2023

Revised Date: 06 April 2023

Accepted Date: 15 June 2023

Publish Date: 30 April 2024

Abstract

Abstract

It takes a long time to treat ore samples by traditional alkali fusion and acid dissolution, and it is easy to cause environmental pollution. Microwave digestion directly releases energy to the sample with high efficiency, and volatile elements are retained in the digestion solution to prevent volatilization from causing deviation of results and environmental pollution. In this experiment, 0.2g of phosphate rock sample was taken and placed in a microwave digestion tank. 3mL hydrochloric acid, 3mL nitric acid, and 2mL hydrofluoric acid were added and then dissolved in the microwave digestion instrument. Then, 2mL of saturated boric acid solution was added for a further microwave digestion. After cooling, the sample was diluted in a 100mL volumetric flask with deionized water. Online addition of rhodium and rhenium as dual internal standards for inductively coupled plasma-mass spectrometry (ICP-MS) determination of rare earth elements in phosphate rock was performed. The relative standard deviation (RSD) of 15 rare earth elements was between 0.68% and 4.52%, the recovery was between 93.1% and 106.6%, and detection limit was between 0.003-0.029μg/g. Two phosphate ore samples were selected and compared with the mixed acid dissolution method. The relative standard deviation was −5.82%-5.99%.
- phosphate ore /
- rare earth elements /
- microwave digestion /
- saturated boric acid /
- complexation /
- inductively coupled plasma-mass spectrometry

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References

[1]	韩兴国, 李凌浩, 黄建辉. 生物地球化学概论[M]. 北京: 高等教育出版社, 1999: 245-253. Google Scholar Han X G, Li L H, Huang J H. Introduction to biogeochemistry[M]. Beijing: Higher Education Press, 1999: 245-253. Google Scholar
[2]	郭江峰,姚多喜,陈健,等. 重庆龙潭组煤中稀土元素地球化学及地质成因分析[J]. 地学前缘, 2016, 23(3): 51. Google Scholar Guo J F,Yao D X,Chen J,et al. Geochemistry of the rare earth elements of coals from the Longtan Formation in Chongqing and its geological implication[J]. Earth Science Frontiers, 2016, 23(3): 51. Google Scholar
[3]	尹明, 李家熙. 岩石矿物分析（第四版: 第二分册）[M]. 北京: 地质出版社, 2011: 105-115. Google Scholar Yin M, Li J X. Rock and Mineral Analysis （The fourth edition: Volume Ⅱ） [M]. Beijing: Geological Publishing House , 2011: 105-115. Google Scholar
[4]	李冰,周建雄,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. Modern instrumental analysis of inorganic multi-elements[J]. Acta Geologica Sinica, 2011, 85(11): 1878−1916. Google Scholar
[5]	周凯红,张立峰,李佳. 电感耦合等离子体质谱法测定白云鄂博矿石中15种稀土元素总量及其分量[J]. 冶金分析, 2022, 42(8): 87−95. doi: 10.13228/j.boyuan.issn1000-7571.011751 CrossRef Google Scholar Zhou K H,Zhang L F,Li J. Determination of total amount of fifteen rare earth elements and its component in Bayan Obo ore by inductively coupled plasma mass spectrometry[J]. Metallurgical Analysis, 2022, 42(8): 87−95. doi: 10.13228/j.boyuan.issn1000-7571.011751 CrossRef Google Scholar
[6]	杨惠玲,杜天军,王书勤,等. 电感耦合等离子体质谱法测定金属矿中稀土和稀散元素[J]. 冶金分析, 2022, 42(5): 8−14. doi: 10.13228/j.boyuan.issn1000-7571.011704 CrossRef Google Scholar Yang H L,Du T J,Wang S Q,et al. Determination of rare earth and scattered elements in metallic ores by inductively coupled plasma mass spectrometry[J]. Metallurgical Analysis, 2022, 42(5): 8−14. doi: 10.13228/j.boyuan.issn1000-7571.011704 CrossRef Google Scholar
[7]	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. doi: 10.13228/j.boyuan.issn1000-7571.009739 CrossRef 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. doi: 10.13228/j.boyuan.issn1000-7571.009739 CrossRef Google Scholar
[8]	孙朝阳,杨凯,代小吕,等. 电感耦合等离子体质谱(ICP-MS)法测定岩石中的稀土元素[J]. 中国无机分析化学, 2015, 5(4): 48−52. doi: 10.3969/j.issn.2095-1035.2015.04.011 CrossRef Google Scholar Sun C Y,Yang K,Dai X L,et al. Determination of rare earth elements in rock by inductively coupled plasma mass spectrometry[J]. Chinese Journal of Inorganic Analytical Chemistry, 2015, 5(4): 48−52. doi: 10.3969/j.issn.2095-1035.2015.04.011 CrossRef Google Scholar
[9]	王家松,王力强,王娜,等. 偏硼酸锂熔融分解锆英砂的实验条件优化研究[J]. 华北地质, 2022, 45(4): 48−52. Google Scholar Wang J S,Wang L Q,Wang N,et al. Optimization of experimental conditions for melting decomposition of zircon sands by lithium metaborate[J]. North China Geology, 2022, 45(4): 48−52. Google Scholar
[10]	辛文彩,朱志刚,宋晓云,等. 应用电感耦合等离子体质谱测定深海富稀土沉积物中稀土元素方法研究[J]. 海洋地质前沿, 2022, 38(9): 92−96. Google Scholar Xin W C,Zhu Z G,Song X Y,et al. On pretreatment method for the determination of rare earth elements in deep sea REY-rich sediments by inductively coupled plasma-mass spectrometry[J]. Marine Geology Frontiers, 2022, 38(9): 92−96. Google Scholar
[11]	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. doi: 10.13228/j.boyuan.issn1000-7571.009753 CrossRef 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. doi: 10.13228/j.boyuan.issn1000-7571.009753 CrossRef Google Scholar
[12]	李正鹤,黄金松,王佳翰. 工作碱熔-电感耦合等离子体质谱法测定海洋沉积物中的稀土元素[J]. 化学世界, 2021, 11(4): 660−666. doi: 10.19500/j.cnki.0367-6358.20200701 CrossRef Google Scholar Li Z H,Huang J S,Wang J H. Determination of rare earth elements in marine sediments by alkali fusion inductively coupled plasma mass spectrometry[J]. Chemical World, 2021, 11(4): 660−666. doi: 10.19500/j.cnki.0367-6358.20200701 CrossRef Google Scholar
[13]	曾江萍,王家松,王娜,等. 敞开酸溶-电感耦合等离子体质谱法测定锑矿石中的稀土元素[J]. 华北地质, 2021, 44(4): 80−84. Google Scholar Zeng J P,Wang J S,Wang N,et al. Determination of rare earth elements in antimony ore by open acid dissolution-inductively coupled plasma mass spectrometry[J]. North China Geology, 2021, 44(4): 80−84. Google Scholar
[14]	龚仓,丁洋,陆海川,等. 五酸溶样-电感耦合等离子体质谱法同时测定地质样品中的稀土等28种金属元素[J]. 岩矿测试, 2021, 40(3): 340−348. doi: 10.15898/j.cnki.11-2131/td.202011030136 CrossRef Google Scholar Gong C,Ding Y,Lu H C,et al. Simultaneous determination of 28 elements including rare earth elements by ICP-MS with five-acid dissolution[J]. Rock and Mineral Analysis, 2021, 40(3): 340−348. doi: 10.15898/j.cnki.11-2131/td.202011030136 CrossRef Google Scholar
[15]	Zhao W,Zong K Q,Liu Y S,et al. An effective oxide interference correction on Sc and REE for routine analyses of geological samples by inductively coupled plasma-mass spectrometry[J]. Journal of Earth Science, 2019, 30(6): 1302−1310. doi: 10.1007/s12583-019-0898-5 CrossRef Google Scholar
[16]	苏春风. 电感耦合等离子体质谱(ICP-MS)法测定稀土矿中16种稀土元素含量[J]. 中国无机分析化学, 2020, 10(6): 28−32. doi: 10.3969/j.issn.2095-1035.2020.06.007 CrossRef Google Scholar Su C F. Determination of 16 rare earth elements in rare earth ores by inductively coupled plasma mass spectrometry[J]. Chinese Journal of Inorganic Analytical Chemistry, 2020, 10(6): 28−32. doi: 10.3969/j.issn.2095-1035.2020.06.007 CrossRef Google Scholar
[17]	戴雪峰,蒋宗明,杨利华. 电感耦合等离子体质谱(ICP-MS)法测定铜铅锌矿中稀土元素[J]. 中国无机分析化学, 2016, 6(1): 26−29. doi: 10.3969/j.issn.2095-1035.2016.01.007 CrossRef Google Scholar Dai X F,Jiang Z M,Yang L H. Determination rare earth elements in copper,lead and zinc ores by inductively coupled plasma mass spectrometry[J]. Chinese Journal of Inorganic Analytical Chemistry, 2016, 6(1): 26−29. doi: 10.3969/j.issn.2095-1035.2016.01.007 CrossRef Google Scholar
[18]	张亚峰,冯俊,唐杰,等. 基于五酸溶样体系-ICP-MS同时测定地质样品中稀土等46种元素[J]. 质谱学报, 2016, 37(2): 186−192. doi: 10.7538/zpxb.2016.37.02.0186 CrossRef Google Scholar Zhang Y F,Feng J,Tang J,et al. Simultaneous determination of species of micro,trace and tare earth elements by ICP-MS based on the system of five-acids dissolution of sample[J]. Journal of Chinese Mass Spectrometry Society, 2016, 37(2): 186−192. doi: 10.7538/zpxb.2016.37.02.0186 CrossRef Google Scholar
[19]	程祎,李志伟,于亚辉,等. 高压密闭消解-电感耦合等离子体质谱法测定地质样品中铌、钽、锆、铪和16种稀土元素[J]. 理化检验(化学分册), 2020, 56(7): 782−787. Google Scholar Cheng Y,Li Z W,Yu Y H,et al. ICP-MS determination of Nb,Ta,Zr,Hf and 16 rare earth elements in geological samples with high pressure closed digestion[J]. Physical Testing and Chemical Analysis (Part B:Chemical Analysis), 2020, 56(7): 782−787. Google Scholar
[20]	曾江萍,王家松,朱悦,等. 敞开酸溶-电感耦合等离子体质谱法测定铀矿石中15种稀土元素[J]. 岩矿测试, 2022, 41(5): 789−797. doi: 10.15898/j.cnki.11-2131/td.202112070197 CrossRef Google Scholar Zeng J P,Wang J S,Zhu Y,et al. Determination of 15 rare earth elements in uranium ore by open acid dissolution-inductively coupled plasma-mass spectrometry[J]. Rock and Mineral Analysis, 2022, 41(5): 789−797. doi: 10.15898/j.cnki.11-2131/td.202112070197 CrossRef Google Scholar
[21]	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 Q. 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
[22]	王贵超,刘荣丽,王志坚,等. 微波消解-电感耦合等离子体质谱法测定深海沉积物中稀土总量[J]. 理化检验(化学分册), 2021, 57(7): 627−632. Google Scholar Wang G C,Liu R L,Wang Z J,et al. Determination of total content of rare earths in deep-sea sediments by inductively coupled plasma mass spectrometry after microwave digestion[J]. Physical Testing and Chemical Analysis (Part B:Chemical Analysis), 2021, 57(7): 627−632. Google Scholar
[23]	张宏丽,高小飞,姚明星,等. 微波消解-电感耦合等离子体质谱法测定赤泥中稀土总量及分量[J]. 稀土, 2019, 7(3): 96−101. doi: 10.16533/j.cnki.15-1099/tf.20190002 CrossRef Google Scholar Zhang H L,Gao X F,Yao M X,et al. Microwave dissolving-inductively coupled plasma mass spectrometric determination of total and individual REE in red mud[J]. Chinese Rare Earths, 2019, 7(3): 96−101. doi: 10.16533/j.cnki.15-1099/tf.20190002 CrossRef Google Scholar
[24]	黄金松,李正鹤,王佳翰. 微波消解-ICP-MS测定海洋沉积物中的稀土元素[J]. 化学试剂, 2021, 43(4): 515−519. doi: 10.13822/j.cnki.hxsj.2021007883 CrossRef Google Scholar Huang J S,Li Z H,Wang J H. Determination of rare earth elements in marine sediments by microwave digestion ICP-MS[J]. Chemical Reagents, 2021, 43(4): 515−519. doi: 10.13822/j.cnki.hxsj.2021007883 CrossRef Google Scholar
[25]	李银花,赵雨薇,刘曙,等. 微波消解-高分辨电感耦合等离子体质谱(HR-ICP-MS)法测定原油中22种微量元素[J]. 中国无机分析化学, 2022, 12(6): 94−102. doi: 10.3969/j.issn.2095-1035.2022.06.015 CrossRef Google Scholar Li Y H,Zhao Y W,Liu S,et al. Determination of 22 trace elements in crude oil by high resolution inductively coupled plasma mass spectrometry with microwave digestion[J]. Chinese Journal of Inorganic Analytical Chemistry, 2022, 12(6): 94−102. doi: 10.3969/j.issn.2095-1035.2022.06.015 CrossRef Google Scholar
[26]	沈健,赵雨薇,王兵. 微波消解-高分辨电感耦合等离子体质谱(HR-ICP-MS)法测定煤炭中35种痕量金属元素[J]. 中国无机分析化学, 2022, 12(2): 26−34. doi: 10.3969/j.issn.2095-1035.2022.02.004 CrossRef Google Scholar Shen J,Zhao Y W,Wang B. Determination of 35 trace metal elements in coal by high resolution inductively coupled plasma mass spectrometry with microwave digestion[J]. Chinese Journal of Inorganic Analytical Chemistry, 2022, 12(2): 26−34. doi: 10.3969/j.issn.2095-1035.2022.02.004 CrossRef Google Scholar
[27]	张楠,徐铁民,吴良英,等. 微波消解-电感耦合等离子体质谱法测定海泡石中的稀土元素[J]. 岩矿测试, 2018, 37(6): 644−649. Google Scholar Zhang N,Xu T M,Wu L Y,et al. Determination of rare earth elements in sepiolite by ICP-MS using microwave digestion[J]. Rock and Mineral Analysis, 2018, 37(6): 644−649. Google Scholar
[28]	郭振华,何汉江,田凤英. 混合酸分解-电感耦合等离子体质谱法测定磷矿石中15种稀土元素[J]. 岩矿测试, 2014, 33(1): 25−28. doi: 10.3969/j.issn.0254-5357.2014.01.005 CrossRef Google Scholar Guo Z H,He H J,Tian F Y. Determination of rare earth elements in phosphate ores by inductively coupled plasma-mass spectrometry with mixed acid dissolution[J]. Rock and Mineral Analysis, 2014, 33(1): 25−28. doi: 10.3969/j.issn.0254-5357.2014.01.005 CrossRef Google Scholar
[29]	倪文山,刘长森,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 S,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
[30]	李明来,王良士,彭新林,等. 电感耦合等离子体原子发射光谱法测定磷矿石中微量稀土元素[J]. 冶金分析, 2011, 30(1): 47−50. Google Scholar Li M L,Wang L S,Peng X L,et al. Determination of trace rare earth elements in phosphate ore by inductively coupled plasma atomic emission spectrometry[J]. Metallurgical Analysis, 2011, 30(1): 47−50. Google Scholar
[31]	李海,杨朝帅,余亚美,等. 微波消解-磺基水杨酸光度法测定磷矿石中铁[J]. 冶金分析, 2017, 37(1): 61−65. doi: 10.13228/j.boyuan.issn1000-7571.009930 CrossRef Google Scholar Li H,Yang C S,Yu Y M,et al. Determination of iron in phosphate ore by sulfosalicylic acid spectrophotometry with microwave digestion[J]. Metallurgical Analysis, 2017, 37(1): 61−65. doi: 10.13228/j.boyuan.issn1000-7571.009930 CrossRef Google Scholar
[32]	彭桦,张屹璇,余慧茹,等. 微波碱熔消解快速测定磷矿石和磷精矿中二氧化硅[J]. 云南化工, 2022, 49(9): 37−39. Google Scholar Peng H,Zhang Q X,Yu H R,et al. Rapid determination of silica in phosphate rock and phosphate concentrate by microwave alkaline melting and digestion[J]. Yunnan Chemical Technology, 2022, 49(9): 37−39. Google Scholar