Boron Analysis in Boron Ores by Inductively Coupled Plasma-Optical Emission Spectrometry with Sealed Acid Digestion at High Pressure

WANG Lei; YU Tingting; SUN Hongbin; ZHANG Baoke

doi:10.15898/j.ykcs.202308070131

Rock and Mineral Analysis > 2024 > 43(3): 468-475. > DOI: 10.15898/j.ykcs.202308070131

WANG Lei，YU Tingting，SUN Hongbin，et al. Boron Analysis in Boron Ores by Inductively Coupled Plasma-Optical Emission Spectrometry with Sealed Acid Digestion at High Pressure[J]. Rock and Mineral Analysis，2024，43（3）：468−475. DOI: 10.15898/j.ykcs.202308070131

Citation:

PDF (493 KB)

Boron Analysis in Boron Ores by Inductively Coupled Plasma-Optical Emission Spectrometry with Sealed Acid Digestion at High Pressure

National Research Center for Geoanalysis, Beijing 100037, China

More Information

Received Date: August 06, 2023
Revised Date: March 07, 2024
Accepted Date: March 19, 2024
Available Online: June 20, 2024

Abstract

HIGHLIGHTS
(1) There is no need to expel acid after sealed acid digestion of boron ore at high pressure, which effectively improves the analytical efficiency.

(2) The problem of BF₃ or BCl₃, which is easily volatilized when boric acid is heated and evaporated in concentrated acid solution, is solved by using a hydrofluoric acid-resistant sampling system.

(3) The method is suitable for the samples of boromagnesite, chambersite, salt lake type solid boron ore and ludwigite, and the content of boron in boron ores below 10% can be determined.

ABSTRACT

The literature provides reference for the accurate determination of boron by inductively coupled plasma-optical emission spectrometry (ICP-OES), but most of the studies are conducted on the standard substances of soil and stream sediment. In addition, the range of boron content is low, and the methods for the determination of high boron content in boron ores are few. A method of ICP-OES with sealed acid digestion at high pressure was developed for the determination of boron content in boron ores. Using nitric acid and hydrofluoric acid as reagents, the samples of boron ores were dissolved at high temperature and high pressure without acid drive, and ICP-OES equipped with a hydrofluoric acid-resistant sampling system was used to determine boron. The samples of boromagnesite, ludwigite, chambersite and salt lake type solid boron ore were taken as the research objects. The relative standard deviation (RSD, n=11) was 0.39%−2.66%, the detection limit of the method was 1.76g/g, and the determination range was 5.87g/g−10.8%. The measured values were consistent with the certified values after the verification of the reference materials. Compared with volumetric method and microwave digestion method, the results were in good agreement. This method does not require evaporating the sample solution, which solves the boron volatile loss problem. The BRIEF REPORT is available for this paper at http://www.ykcs.ac.cn/en/article/doi/10.15898/j.ykcs.202308070131.
BRIEF REPORT
Significance：The exploitation and utilization of boron resources play an important role in the development of modern industry. The accurate determination of boron content in boron ores provides powerful technical support for the utilization and the smelting technology study of boron ore deposit. Inductively coupled plasma-optical emission spectrometry (ICP-OES) has been widely used in the determination of boron content in samples due to its advantages of high accuracy and sensitivity, wide linear range, low detection limit and good precision. At present, most of the studies focus on the boron determination of the standard substances in soil and stream sediment with a narrow determination range; the methods for the determination of high boron content in boron ores are few. In the research, a method of ICP-OES was developed for the determination of boron content in boron ores with sealed acid solution digestion at high pressure and a hydrofluoric acid-resistant sampling system. The method satisfies the determination requirements, with advantages of using less reagent and avoiding boron loss.

Methods：A high pressure sealed acid digestion-ICP-OES method was developed for the determination of boron in boron ores, through systematic experimental research, reference material verification, and comparison of different methods. Using nitric acid and hydrofluoric acid as reagents, the sample of boron ore was dissolved at high temperature and high pressure without acid drive, and ICP-OES equipped with a hydrofluoric acid-resistant sampling system was used to determine boron. This method solved the problem of forming volatile BF₃ or BCl₃ when boric acid was heated and evaporated in concentrated acid solution, which caused loss.

Data and Results：The samples of boromagnesite, ludwigite, chambersite and salt lake solid boron ore were taken as the research objects, the measuring spectrum lines and the amount of reagents were studied. The results show that in boron ores, there was no interference of Si, Mg, Mn, Fe, Na or other elements on the three commonly used analytical spectral lines of boron in ICP-OES. The linear correlation coefficient (R²) of spectral lines was greater than 0.9995. The analytical spectral line of 249.677nm with moderate intensity was selected for boron. When the amount of hydrofluoric acid was greater than 1.0mL, the measured value was consistent with the certified value of the reference material. Considering the complexity of the geological sample, the experiment determined that the addition amount of hydrofluoric acid was 2.0mL. According to the experimental method, 5 actual samples with varying content of three types of boromagnesite, chambersite and salt lake solid boron ore were selected for determination. The relative standard deviation (RSD, n=11) was 0.39%−2.66%, the detection limit of the method was 1.76g/g, and the determination range was 5.87g/g−10.8%. The measured values were consistent with the certified values after the verification of the reference materials. Compared with volumetric method and microwave digestion method, the results were in good agreement. The repeatability and reproducibility of the method were verified by the precision collaborative experiments among the ten laboratories. The method only involves conventional reagents, vessels, high-pressure digestion tanks and ICP-OES instrument, which is suitable for popularization.

FullText(HTML)

References (31)

References

[1]	《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: 376−396. The editorial committee of “Rock and Mineral Analysis”. Rock and Mineral Analysis (The 4th edition, Volume Ⅱ) [M]. Beijing: Geological Publishing House, 2011: 376−396.
[2]	于微. 分光光度法测定水系沉积物中硼[J]. 吉林地质, 2014, 33(4): 61−63. doi: 10.3969/j.issn.1001-2427.2014.04.014 Yu W. Determination of boron in stream sediments by spectrophotometric method[J]. Jilin Geology, 2014, 33(4): 61−63. doi: 10.3969/j.issn.1001-2427.2014.04.014
[3]	邢书才, 杨永, 岳亚萍. 姜黄素分光光度法测定水中硼的优化检测条件研究[J]. 中国测试, 2019, 45(6): 65−69. Xing S C, Yang Y, Yue Y P. Study on the optimizing conditions for determining boron in water by curcumin spectrophotometry[J]. China Measurement & Test, 2019, 45(6): 65−69.
[4]	赵志刚, 韦雪梅, 赵华丽. 高氯酸消解电位滴定法测定硼粉纯度[J]. 化学分析计量, 2022, 31(6): 46−49. doi: 10.3969/j.issn.1008-6145.2022.06.011 Zhao Z G, Wei X M, Zhao H L. Determination of the purity of boron powder by potentiometric titration after sample digested by perchloric[J]. Chemical Analysis and Meterage, 2022, 31(6): 46−49. doi: 10.3969/j.issn.1008-6145.2022.06.011
[5]	王顺祥, 龚仓, 吴少青, 等. 固体进样-CCD光电直读发射光谱法测定地球化学样品中微量银、硼和锡[J]. 中国无机分析化学, 2023, 13(8): 863−868. doi: 10.3969/j.issn.2095-1035.2023.08.012 Wang S X, Gong C, Wu S Q, et al. Determination of trace silver, boron and tin in geochemical samples by CCD optical direct-reading emission spectrometer with solid injection[J]. Chinese Journal of Inorganic Analytical Chemistry, 2023, 13(8): 863−868. doi: 10.3969/j.issn.2095-1035.2023.08.012
[6]	张元, 王文东, 卢兵, 等. 碱熔-阳离子交换树脂分离ICP-MS法测定厚覆盖区地球化学调查样品中硼锗溴钼锡碘钨[J]. 岩矿测试, 2022, 41(1): 99−108. Zhang Y, Wang W D, Lu B, et al. Determination of boron, germanium, bromine, molybdenum, tin, iodine and tungsten in geochemical survey sample by ICP-MS with alkali fusion-cation exchange resin separation[J]. Rock and Mineral Analysis, 2022, 41(1): 99−108.
[7]	Manousi N, Kabir A, Furton K G, et al. Dual lab-in-syringe flow-batch platform for automatic fabric disk sorptive extraction/back-extraction as a front end to inductively coupled plasma atomic emission spectrometry[J]. Analytical Chemistry, 2022, 94(38): 12943−12947. doi: 10.1021/acs.analchem.2c02268
[8]	Vievard J, Amoikon T L, Coulibaly N A, et al. Extraction and quantification of pesticides and metals in palm wines by HS-SPME/GC–MS and ICP-AES/MS[J]. Food Chemistry, 2022, 393: 133352. doi: 10.1016/j.foodchem.2022.133352
[9]	Zeng Y, Yokoyama Y, Hirabayashi S, et al. A rapid and precise method of establishing age model for coral skeletal radiocarbon to study surface oceanography using coupled X-ray photos and ICP-AES measurement[J]. Nuclear Instruments and Methods in Physics Research Section B: Beam Interactions with Materials and Atoms, 2022, 533: 23−28.
[10]	Erickson B. Product review: ICP-AES remains competitive[J]. Analytical Chemistry, 1998, 70(5): 211A−215A. doi: 10.1021/ac9817725
[11]	刘向磊, 孙文军, 任彧仲, 等. 微波消解混合模式电感耦合等离子体质谱法测定土壤或沉积物中银、锡、硼[J]. 质谱学报, 2022, 43(4): 522−532. doi: 10.7538/zpxb.2021.0205 Liu X L, Sun W J, Ren Y Z, et al. Determination of sliver, tin and boron in soil or sediment sample with microwave digestion by mixed mode inductive coupled plasma mass spectrometry[J]. Journal of Chinese Mass Spectrometry Society, 2022, 43(4): 522−532. doi: 10.7538/zpxb.2021.0205
[12]	刘跃, 王记鲁, 李静, 等. 高压密闭消解-电感耦合等离子体质谱(ICP-MS)法测定土壤背景点样品中的29种元素[J]. 中国无机分析化学, 2023, 13(2): 136−142. Liu Y, Wang J L, Li J, et al. Determination of 29 elements in soil background site samples by inductively coupled plasma mass spectrometry with high pressure closed digestion[J]. Chinese Journal of Inorganic Analytical Chemistry, 2023, 13(2): 136−142.
[13]	赵庆令, 李清彩, 蒲军, 等. 电感耦合等离子体发射光谱法同时测定土壤样品中砷硼铈碘铌硫钪锶钍锆等 31种元素[J]. 岩矿测试, 2010, 29(4): 455−457. Zhao Q L, Li Q C, Pu J, et al. Simultaneous determination of 31 elements in soil samples by inductively coupled plasma-atomic emission spectrometry[J]. Rock and Mineral Analysis, 2010, 29(4): 455−457.
[14]	杜宝华, 盛迪波, 王日中, 等. 电感耦合等离子体发射光谱(ICP-OES)法测定含硼聚乙烯核屏蔽材料中的硼[J]. 中国无机分析化学, 2023, 13(3): 274−277. doi: 10.3969/j.issn.2095-1035.2023.03.012 Du B H, Sheng D B, Wang R Z, et al. Determination of boron content in boron-containing polyethylene nuclear shielding materials by ICP-OES[J]. Chinese Journal of Inorganic Analytical Chemistry, 2023, 13(3): 274−277. doi: 10.3969/j.issn.2095-1035.2023.03.012
[15]	方宏树, 孔晓彦, 胡兰基. ICP-OES法测定盐湖土壤中锂和硼的方法研究[J]. 当代化工, 2023, 52(1): 248−252. Fang H S, Kong X Y, Hu L J. Study on the determination method of lithium and boron in salt lake soil by ICP-OES[J]. Contemporary Chemical Industry, 2023, 52(1): 248−252.
[16]	黄合生, 邢文青, 黄波, 等. ICP-AES法测定凝渣剂中铝和硼元素含量[J]. 南方金属, 2023, 250: 19−23. Huang H S, Xing W B, Huang B, et al. Determination of aluminum and boron in slag coagulant by inductively coupled plasma[J]. South Metals, 2023, 250: 19−23.
[17]	李冰, 马新荣, 杨红霞, 等. 封闭酸溶-电感耦合等离子体原子发射光谱法同时测定地质样品中硼砷硫[J]. 岩矿测试, 2003, 22(4): 241−247. doi: 10.3969/j.issn.0254-5357.2003.04.001 Li B, Ma X R, Yang H X, et al. Determination of boron, arsenic and sulfur in geological samples by inductively coupled plasma atomic emission spectrometry with sample treatment by pressurized decomposition[J]. Rock and Mineral Analysis, 2003, 22(4): 241−247. doi: 10.3969/j.issn.0254-5357.2003.04.001
[18]	Zarcinas B A, Cartwright B. Acid dissolution of soils and rocks for the determination of boron inductively coupled plasma atomic emission spectrometry[J]. Analyst, 1987, 112(8): 1107−1112. doi: 10.1039/an9871201107
[19]	方宏树, 何媛媛, 鲁海妍. 过氧化钠熔融ICP-OES法试测定地矿样品中的硼[J]. 化学工程师, 2023(1): 24−28. Fang H S, He Y Y, Lu H Y. Determination of boron in geological and mineral samples by sodium peroxide melting ICP-OES[J]. Chemical Engineer, 2023(1): 24−28.
[20]	易田芳, 向勇, 蒋建军, 等. 四酸微波消解-电感耦合等离子体发射光谱(ICP-OES)法测定土壤和沉积物中全硼含量[J]. 中国无机分析化学, 2023, 13(6): 576−581. doi: 10.3969/j.issn.2095-1035.2023.06.010 Yi T F, Xiang Y, Jiang J J, et al. Determination of total boron in soil and deposit by inductively coupled plasma optical emission spectroscopy with four acids-microwave digestion[J]. Chinese Journal of Inorganic Analytical Chemistry, 2023, 13(6): 576−581. doi: 10.3969/j.issn.2095-1035.2023.06.010
[21]	《矿产资源工业要求手册》编委会. 矿产资源工业要求手册[M]. 北京: 地质出版社, 2012.
[22]	肖凡, 张宁, 姜云军, 等. 密闭酸溶-电感耦合等离子体原子发射光谱法测定地球化学调查样品中硼[J]. 冶金分析, 2018, 38(6): 50−54. Xiao F, Zhang N, Jiang Y J, et al. Determination of boron in geochemical survey sample by inductively coupled plasma atomic emission spectrometry after acid dissolution in closed system[J]. Metallurgical Analysis, 2018, 38(6): 50−54.
[23]	王蕾, 张保科, 马生凤, 等. 封闭压力酸溶-电感耦合等离子体光谱法测定钨矿石中的钨[J]. 岩矿测试, 2014, 33(5): 661−664. doi: 10.3969/j.issn.0254-5357.2014.05.008 Wang L, Zhang B K, Ma S F, et al. Determination of wolfram in tungsten ore by pressurized acid digestion-inductively coupled plasma-atomic emission spectrometry[J]. Rock and Mineral Analysis, 2014, 33(5): 661−664. doi: 10.3969/j.issn.0254-5357.2014.05.008
[24]	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: 226-227.
[25]	金佳旭, 郑旭, 付彦吉, 等. 不同酸液作用下牛蹄塘组页岩孔隙结构演化特征试验研究[J]. 工程地质学报, 2021, 29(3): 891−900. Jin J X, Zhen X, Fu Y J, et al. Experimental study of acidization impact to pore topological structure variation of Niutitang shale[J]. Journal of Engineering Geology, 2021, 29(3): 891−900.
[26]	印万忠. 氢氟酸在硅酸盐矿物浮选中的作用机制[J]. 黄金学报, 1999, 1(4): 271−274. Yin W Z. Effect mechanism of hydrofluoric acid in flotation of silicate minerals[J]. Gold Journal, 1999, 1(4): 271−274.
[27]	杨林, 邹国庆, 周武权, 等. 微波消解-电感耦合等离子体质谱(ICP-MS)法测定稀有多金属矿中锂铍铌钽铷铯[J]. 中国无机分析化学, 2023, 13(8): 825−830. doi: 10.3969/j.issn.2095-1035.2023.08.006 Yang L, Zou G Q, Zhou W Q, et al. Determination of Li, Be, Nb, Ta, Rb, Cs in rare polymetallic ores by inductively coupled plasma mass spectrometry (ICP-MS) with microwave digestion[J]. Chinese Journal of Inorganic Analytical Chemistry, 2023, 13(8): 825−830. doi: 10.3969/j.issn.2095-1035.2023.08.006
[28]	朱健, 马程程, 赵磊, 等. 高压密闭消解-电感耦合等离子体质谱法测定煤中17种金属元素[J]. 理化检验(化学分册), 2014, 50(8): 960−963. Zhu J, Ma C C, Zhao L, et al. ICP-MS determination of 17 metal elements in coal with high-pressure closed digestion[J]. Physical Testing and Chemical Analysis (Part B: Chemical Analysis), 2014, 50(8): 960−963.
[29]	马亮帮, 张大勇, 腾格尔, 等. 高压密闭消解-电感耦合等离子体质谱(ICP-MS)法测定煤中稀土元素[J]. 中国无机分析化学, 2019, 9(4): 27−30. Ma L B, Zhang D Y, Tenger, et al. Determination of rare earth elements in coal by inductively coupled plasma-mass spectrometry with high-pressure closed digestion[J]. Chinese Journal of Inorganic Analytical Chemistry, 2019, 9(4): 27−30.
[30]	李迎春, 周伟, 王健, 等. X射线荧光光谱法测定高锶高钡的硅酸盐样品中主量元素[J]. 岩矿测试, 2013, 32(2): 249−253. Li Y C, Zhou W, Wang J, et al. Determination of major elements in silicate samples with high content strontium and barium by X-ray fluorescence spectrometry[J]. Rock and Mineral Analysis, 2013, 32(2): 249−253.
[31]	李迎春, 张磊, 周伟, 等. 熔融制样-波长色散和能量色散X射线荧光光谱仪应用于硅酸盐类矿物及疑难样品分析[J]. 岩矿测试, 2020, 39(6): 828−838. Li Y C, Zhang L, Zhou W, et al. Determination of major and minor elements in rock, soils and sediments and complex samples by wavelength and energy dispersive X-ray fluorescence Spectrometry with fusion sampling[J]. Rock and Mineral Analysis, 2020, 39(6): 828−838.

[1]	LIU Ze, CHEN Zhenyu, CHEN Xiaodan, XU Wentan, LIU Chunhua, ZHU Zeying, NIU Zhijian, ZHAO Chenhui, ZHAO Yunbiao. Quantitative Analysis of Be in Herderite by Electron Probe Microanalysis[J]. Rock and Mineral Analysis, 2024, 43(5): 703-712. DOI: 10.15898/j.ykcs.202311010171
[2]	LIU Jin, WANG Jian, WANG Guijun, ZHANG Xiaogang, SHANG Ling. Analysis of Mineralogical Characteristics of Leucosphenite from the Fengcheng Formation in the Junggar Basin by Electron Probe Microanalyzer and X-ray Diffractometer[J]. Rock and Mineral Analysis, 2022, 41(5): 764-773. DOI: 10.15898/j.cnki.11-2131/td.202108190101
[3]	Mei-fang YE, San LIU, Gu-wei XIE, Hui-bo ZHAO, Ning-chao ZHOU, Xiao-yan WEI, Jian-guo YANG, Hong HOU, Lei WANG, Yi WANG. Characteristics of Micas from Sericitolite of the Gongpoquan and Baishantang Deposits, Beishan Area by Scanning Electron Microscope, X-ray Diffraction and Electron Microprobe Analyses[J]. Rock and Mineral Analysis, 2016, 35(2): 166-177. DOI: 10.15898/j.cnki.11-2131/td.2016.02.009
[4]	Han WANG, Zheng-yu ZHOU, Qian ZHONG, Rui-ting LIU, Qi LIU, Ying-bo LI. Study on Petrological and Mineralogical Characteristics of Laos Stone by EPMA-XRD-SEM[J]. Rock and Mineral Analysis, 2016, 35(1): 56-61. DOI: 10.15898/j.cnki.11-2131/td.2016.01.010
[5]	Yan LAN, Tai-jin LU, Wei-ming CHEN, Yang LIU, Rong LIANG, Ying MA, Xiao-hu ZHANG. A Non-destructive Measurement Method of Gem Jadeite Content in Jadeitite Based on Specific Gravity and X-ray Powder Diffraction[J]. Rock and Mineral Analysis, 2015, 34(2): 207-212. DOI: 10.15898/j.cnki.11-2131/td.2015.02.009
[6]	Nai-cen XU, Jia-lin SHEN, Jing ZHANG. Application of X-ray Diffraction, X-ray Fluorescence Spectrometry and Electron Microprobe in the Identification of Basalt[J]. Rock and Mineral Analysis, 2015, 34(1): 75-81. DOI: 10.15898/j.cnki.11-2131/td.2015.01.010
[7]	Yi WANG, Na CHANG, Ya-fei LIU, Hui-bo ZHAO, San LIU. Study on the Mineralogical Characteristics of Cinnabar Jade by X-ray Powder Diffraction-Laser Raman Spectroscopy-Electron Probe from Xunyang, Shan'xi Province[J]. Rock and Mineral Analysis, 2014, 33(6): 802-807. DOI: 10.15898/j.cnki.11-2131/td.2014.06.007
[8]	Wei REN, Lijin WANG, Jiaping LI. Detection of Emerald from Xinjiang by Electron Probe Microanalyzer and X-ray Diffractometer[J]. Rock and Mineral Analysis, 2010, 29(2): 179-181.
[9]	Progress in Background Subtraction and Spectral Interference Correction in Electron Probe Microanalysis[J]. Rock and Mineral Analysis, 2008, 27(1): 49-54.
[10]	Evaluation of the Methods for Quantitative Determination of FeO and Fe2O3 by Electron Probe Microanalysis[J]. Rock and Mineral Analysis, 2007, 26(3): 213-218.

Supplements (0)

Cited By

Get Citation

PDF

XML

Article views (179) PDF downloads (58)

Turn off MathJax

Article Contents

ABSTRACT

References

Boron Analysis in Boron Ores by Inductively Coupled Plasma-Optical Emission Spectrometry with Sealed Acid Digestion at High Pressure

ABSTRACT

References

Related Articles

Catalog

Boron Analysis in Boron Ores by Inductively Coupled Plasma-Optical Emission Spectrometry with Sealed Acid Digestion at High Pressure

ABSTRACT

References

Related Articles

Catalog

Export File

Citation

Format

Content