• Core Journal of China
  • DOAJ
  • Scopus
  • Chinese Scientific and Technical Papers and Citations (CSTPC)
  • Chinese Science Citation Database (CSCD)
Advanced Search
LI Ying-chun, ZHANG Lei, SHANG Wen-yu. Determination of Selenium, Major and Minor Elements in Selenium-rich Soil Samples by X-ray Fluorescence Spectrometry with Powder Pellet Preparation[J]. Rock and Mineral Analysis, 2022, 41(1): 145-152. DOI: 10.15898/j.cnki.11-2131/td.202007090102
Citation: LI Ying-chun, ZHANG Lei, SHANG Wen-yu. Determination of Selenium, Major and Minor Elements in Selenium-rich Soil Samples by X-ray Fluorescence Spectrometry with Powder Pellet Preparation[J]. Rock and Mineral Analysis, 2022, 41(1): 145-152. DOI: 10.15898/j.cnki.11-2131/td.202007090102
shu

Determination of Selenium, Major and Minor Elements in Selenium-rich Soil Samples by X-ray Fluorescence Spectrometry with Powder Pellet Preparation

  • National Research Center for Geoanalysis, Beijing 100037, China

More Information
  • Received Date: July 08, 2020
  • Revised Date: June 04, 2021
  • Accepted Date: August 11, 2021
  • Published Date: January 27, 2022
    Abstract
  • HIGHLIGHTS
    (1) A wavelength dispersive and energy dispersive X-ray fluorescence (WD-ED XRF) spectrometry method was established to determine the major and minor elements in selenium-rich soil.
    (2) The technical difficulties in the determination of Se by XRF were investigated, and the analytical conditions were optimized reasonably.
    (3) The method can be used to determine the high content of Se, and can also provide quantitative or approximate quantitative results of 16 major and minor elements.
    BACKGROUNDAt present, the content of Se in soil is mainly determined by atomic fluorescence spectrometry, which has disadvantages such as large usage of acid and relatively complex pretreatment. Determination of high content of Se requires high dilution, which expands the analysis error.
    OBJECTIVESTo establish a method for the determination of Se and other elements in Se-rich soil samples by wavelength dispersive and energy dispersive X-ray fluorescence (WD-ED XRF).
    METHODSWD-ED XRF was used to determine 17 major and minor elements such as Se in Hubei selenium-rich soil samples with powder pellet. While 10 elements were analyzed by WD-XRF, As, Cu, Rb, Sr, Zr, Ba, Ni were analyzed by ED-XRF, which significantly reduced the measurement time.
    RESULTSBy mixing different certified reference materials in proportion to configure mixed certified reference materials, the problem of insufficient content of the existing Se reference materials in the range of 5-72μg/g was solved. For the determination of high content Se, the relative standard deviation was less than 10%, and the RSD of high content Se sample was less than 0.70%, through the precision and accuracy assessment.
    CONCLUSIONSThe proposed method satisfies the quantitative analysis of soil samples with Se content greater than 3.00μg/g, and provides the quantitative or approximate quantitative analysis results of 16 major and minor elements.
    • FullText(HTML)
    • References (33)
  • Yu T, Yang Z F, Lv Y Y, et al. The origin and geochemical cycle of soil selenium in a Se-rich area of China[J]. Journal of Geochemical Exploration, 2014, 139: 97-108. doi: 10.1016/j.gexplo.2013.09.006
    杨忠芳, 余涛, 侯青叶, 等. 海南岛农田土壤Se的地球化学特征[J]. 现代地质, 2012, 26(5): 837-849. doi: 10.3969/j.issn.1000-8527.2012.05.001

    Yang Z F, Yu T, Hou Q Y, et al. Geochemical characteristics of soil selenium in farmland of Hainan Island[J]. Geoscience, 2012, 26(5): 837-849. doi: 10.3969/j.issn.1000-8527.2012.05.001
    李杰, 杨志强, 刘枝刚, 等. 南宁市土壤硒分布特征及其影响因素探讨[J]. 土壤学报, 2012, 49(5): 1012-1020. https://www.cnki.com.cn/Article/CJFDTOTAL-TRXB201205021.htm

    Li J, Yang Z Q, Liu Z G, et al. Distribution of selenium in soils of Nanning City and its influencing factors[J]. Acta Pedologica Sinica, 2012, 49(5): 1012-1020. https://www.cnki.com.cn/Article/CJFDTOTAL-TRXB201205021.htm
    商靖敏, 罗维, 吴光红, 等. 洋河流域不同土地利用类型土壤硒(Se)分布及影响因素[J]. 环境科学, 2015, 36(1): 301-308. https://www.cnki.com.cn/Article/CJFDTOTAL-HJKZ201501046.htm

    Shang J M, Luo W, Wu G H, et al. Spatial distribution of Se in soils from different land use types and its influencing factors within the Yanghe Watershed, China[J]. Environmental Sciences, 2015, 36(1): 301-308. https://www.cnki.com.cn/Article/CJFDTOTAL-HJKZ201501046.htm
    李杰, 刘久臣, 汤奇峰, 等. 川西高原地区水体中硒含量及分布特征研究[J]. 岩矿测试, 2018, 37 (2): 183-192. doi: 10.15898/j.cnki.11-2131/td.201709250154

    Li J, Liu J C, Tang Q F, et al. Study of the content and distribution of selenium in water samples from the western Sichuan Plateau and the incidence of Kaschin Beck disease[J]. Rock and Mineral Analysis, 2018, 37(2): 183-192. doi: 10.15898/j.cnki.11-2131/td.201709250154
    谢邦廷, 贺灵, 江官军, 等. 中国南方典型富硒区土壤硒有效性调控与评价[J]. 岩矿测试, 2017, 36(3): 273-281. doi: 10.15898/j.cnki.11-2131/td.201610100152

    Xie B T, He L, Jiang G J, et al. Regulation and evaluation of selenium availability in Se-rich soils in southern China[J]. Rock and Mineral Analysis, 2017, 36(3): 273-281. doi: 10.15898/j.cnki.11-2131/td.201610100152
    杨良策, 李明龙, 陈林, 等. 恩施市高Se区农田土壤Se地球化学特征[J]. 资源环境与工程, 2017, 30(6): 852-855. https://www.cnki.com.cn/Article/CJFDTOTAL-HBDK201606011.htm

    Yang L C, Li M L, Chen L, et al. Geochemical characteristics of soil selenium in farmland of Enshi, western Hubei[J]. Resources Environment & Engineering, 2017, 30(6): 852-855. https://www.cnki.com.cn/Article/CJFDTOTAL-HBDK201606011.htm
    张亚峰, 苗国文, 马强, 等. 青海省海东市平安区土壤Se的地球化学特征[J]. 地球与环境, 2019, 47(1): 74-80. https://www.cnki.com.cn/Article/CJFDTOTAL-DZDQ201901010.htm

    Zhang Y F, Miao G W, Ma Q, et al. Geochemical characteristics of Se in soil of the Pingan District, Haidong City, Qinghai Province[J]. Earth and Environment, 2019, 47(1): 74-80. https://www.cnki.com.cn/Article/CJFDTOTAL-DZDQ201901010.htm
    石天平, 梁述廷. 富硒土壤中Se(Ⅳ)和Se(Ⅵ)测定[J]. 安徽地质, 2019, 29(1): 69-70. https://www.cnki.com.cn/Article/CJFDTOTAL-AHDZ201901013.htm

    Shi T P, Liang S T. Determinations of Se(Ⅳ) and Se(Ⅵ) in selenium-rich soil[J]. Geology of Anhui, 2019, 29(1): 69-70. https://www.cnki.com.cn/Article/CJFDTOTAL-AHDZ201901013.htm
    李植忠, 关雄俊, 吴健玲, 等. 工业硫磺中As、Se的测定[J]. 光谱学与光谱分析, 2002, 22(5): 868-870. doi: 10.3321/j.issn:1000-0593.2002.05.049

    Li Z T, Guan X J, Wu J L, et al. Determination of arsenic and selenium in the industrial sulphur[J]. Spectroscopy and Spectral Analysis, 2002, 22(5): 868-870. doi: 10.3321/j.issn:1000-0593.2002.05.049
    张俊峰, 栾海光, 李杨. 电感耦合等离子体原子发射光谱(ICP-AES)法测定粗锑中的As、Bi、Cd、Cu、Fe、Pb和Se[J]. 中国无机分析化学, 2018, 8(3): 36-39. https://www.cnki.com.cn/Article/CJFDTOTAL-WJFX201803011.htm

    Zhang J F, Luan H G, Li Y. Determination of As, Bi, Cd, Cu, Fe, Pb and Se in crude antimony by inductively coupled plasma atomic emission spectrometry (ICP-AES)[J]. Chinese Journal of Inorganic Analytical Chemistry, 2018, 8(3): 36-39. https://www.cnki.com.cn/Article/CJFDTOTAL-WJFX201803011.htm
    赵宗生, 赵小学, 姜晓旭, 等. 原子荧光光谱测定土壤和水系沉积物中硒的干扰来源及消除方法[J]. 岩矿测试, 2019, 38(3): 333-340. doi: 10.15898/j.cnki.11-2131/td.201809190106

    Zhao Z S, Zhao X X, Jiang X X, et al. Interference sources and elimination methods for the determination of selenium in soil and water sediment by atomic fluorescence spectrometry[J]. Rock and Mineral Analysis, 2019, 38(3): 333-340. doi: 10.15898/j.cnki.11-2131/td.201809190106
    张维宇, 张土秀, 倪天增. 程序控温石墨消解-原子荧光光谱法测定土壤中的硒[J]. 中国无机分析化学, 2011, 1(4): 36-39. https://www.cnki.com.cn/Article/CJFDTOTAL-WJFX201104010.htm

    Zhang W Y, Zhang S X, Ni T Z. Determination of total selenium in soil by atomic fluorescence spectrometry with program temperature-controlled graphite digestion[J]. Chinese Journal of Inorganic Analytical Chemistry, 2011, 1(4): 36-39. https://www.cnki.com.cn/Article/CJFDTOTAL-WJFX201104010.htm
    王晶, 肖娅萍, 梁晓庆, 等. 氢化物发生-原子荧光法测定不同产地绞股蓝及其根际土壤中As, Hg, Se[J]. 光谱学与光谱分析, 2012, 32(3): 813-816. https://www.cnki.com.cn/Article/CJFDTOTAL-GUAN201203053.htm

    Wang J, Xiao Y P, Liang X Q, et al. Determination of arsenic, mercury and selenium in gynostemma pentaphyllum and rhizospheric soil samples collected from different regions by hydride generation atomic fluorescence spectrometry[J]. Spectroscopy and Spectral Analysis, 2012, 32(3): 813-816. https://www.cnki.com.cn/Article/CJFDTOTAL-GUAN201203053.htm
    张勤, 李国会, 樊守忠, 等. X射线荧光光谱法测定土壤和水系沉积物等样品中碳、氮、氟、氯、硫、溴等42种主次和痕量元素[J]. 分析试验室, 2008, 27(11): 51-57. https://www.cnki.com.cn/Article/CJFDTOTAL-FXSY200811016.htm

    Zhang Q, Li G H, Fan S Z, et al. Study on determination of 42 major, minor and trace elements in soil and stream sediment samples[J]. Chinese Journal of Analysis Laboratory, 2008, 27(11): 51-57. https://www.cnki.com.cn/Article/CJFDTOTAL-FXSY200811016.htm
    刘玉纯, 林庆文, 马玲, 等. 粉末压片制样-X射线荧光光谱法分析地球化学调查样品测量条件的优化[J]. 岩矿测试, 2018, 37(6): 671-677. doi: 10.15898/j.cnki.11-2131/td.201801300014

    Lui Y C, Lin Q W, Ma L, et al. Optimization of measurement conditions for geochemical survey sample analysis by X-ray fluorescence spectrometry with pressed powder pellet sample preparation[J]. Rock and Mineral Analysis, 2018, 37(6): 671-677. doi: 10.15898/j.cnki.11-2131/td.201801300014
    阿丽莉, 贺攀红, 张盼盼. 粉末压片-X射线荧光光谱法测定地质样品中镧铈镨钕钐[J]. 冶金分析, 2019, 39(9): 39-45. A L L, https://www.cnki.com.cn/Article/CJFDTOTAL-YJFX201909007.htm

    He P H, Zhang P P. Determination of lanthanum, cerium, praseodymium, neodymium and samarium in geological sample by X-ray fluorescence spectrometry with pressed powder pellet[J]. Metallurgical Analysis, 2019, 39 (9): 39-45. https://www.cnki.com.cn/Article/CJFDTOTAL-YJFX201909007.htm
    田衎, 郭伟臣, 杨永, 等. 波长色散X射线荧光光谱法测定土壤和水系沉积物中13种重金属元素[J]. 冶金分析, 2019, 39(10): 30-36. https://www.cnki.com.cn/Article/CJFDTOTAL-YJFX201910006.htm

    Tian K, Guo W C, Yang Y, et al. Determination of thirteen heavy metals in soil and stream sediment by wavelength dispersive X-ray fluorescence spectrometry[J]. Metallurgical Analysis, 2019, 39(10): 30-36. https://www.cnki.com.cn/Article/CJFDTOTAL-YJFX201910006.htm
    邓述培, 范鹏飞, 唐玉霜, 等. X射线荧光光谱(XRF)法测定土壤污染样品中9种重金属元素[J]. 中国无机分析化学, 2019, 9(4): 12-15. https://www.cnki.com.cn/Article/CJFDTOTAL-WJFX201904003.htm

    Deng S P, Fan P F, Tang Y S, et al. Determination of 9 kinds of soil pollution of heavy metals elements in samples by X-ray fluorescence spectrometry[J]. Chinese Journal of Inorganic Analytical Chemistry, 2019, 9(4): 12-15. https://www.cnki.com.cn/Article/CJFDTOTAL-WJFX201904003.htm
    闵秀云, 王德荣, 高春亮, 等. 粉末压片-X射线荧光光谱法测定盐湖样品中的主次元素[J]. 盐湖研究, 2016, 24(2): 32-36. https://www.cnki.com.cn/Article/CJFDTOTAL-YHYJ201602007.htm

    Min X Y, Wang D R, Gao C L, et al. Major and minor elements from salt lake samples determined by pressed powder pellet method and X-ray fluorescence spectrometry[J]. Journal of Salt Lake Research, 2016, 24(2): 32-36. https://www.cnki.com.cn/Article/CJFDTOTAL-YHYJ201602007.htm
    王佳妮, 张晗, 洪子肖, 等. X射线荧光光谱法测定螺旋藻中23种微量元素[J]. 分析试验室, 2016, 35(2): 130-134. https://www.cnki.com.cn/Article/CJFDTOTAL-FXSY201602003.htm

    Wang J N, Zhang H, Hong Z X, et al. Determination of 23 trace elements in spirulina using X-ray fluorescence spectrometry[J]. Chinese Journal of Analysis Laboratory, 2016, 35(2): 130-134. https://www.cnki.com.cn/Article/CJFDTOTAL-FXSY201602003.htm
    李小莉, 安树清, 徐铁民, 等. 超细粉末压片制样X射线荧光光谱测定碳酸岩样品中多种元素及CO2[J]. 光谱学与光谱分析, 2015, 35(6): 1741-1745. https://www.cnki.com.cn/Article/CJFDTOTAL-GUAN201506062.htm

    Li X L, An S Q, Xu T M, et al. Ultra-fine pressed powder pellet sample preparation XRF determination of multi-elements and carbon dioxide in carbonate[J]. Spectroscopy and Spectral Analysis, 2015, 35(6): 1741-1745. https://www.cnki.com.cn/Article/CJFDTOTAL-GUAN201506062.htm
    刘菊琴, 李小莉. 波长与能量色散复合型X射线荧光光谱仪测定海洋沉积物, 水系沉积物, 岩石和土壤样品中15种稀土元素[J]. 冶金分析, 2018, 38(5): 7-12. https://www.cnki.com.cn/Article/CJFDTOTAL-YJFX201805002.htm

    Liu J Q, Li X L. Determination of fifteen rare earth elements in ocean sediment, stream sediment, rock and soil samples by wavelength dispersion energy dispersion combined type X-ray fluorescence spectrometer[J]. Metallurgical Analysis, 2018, 38(5): 7-12. https://www.cnki.com.cn/Article/CJFDTOTAL-YJFX201805002.htm
    张颖, 朱爱美, 张迎秋, 等. 波长与能量色散复合式X射线荧光光谱技术测定海洋沉积物元素[J]. 分析化学, 2019, 47(7): 1090-1097. https://www.cnki.com.cn/Article/CJFDTOTAL-FXHX201907019.htm

    Zhang Y, Zhu A M, Zhang Y Q, et al. Fast analysis of major and minor elements in marine sediments by wavelength and energy dispersive X-ray fluorescence spectrometer[J]. Chinese Journal of Analytical Chemistry, 2019, 47(7): 1090-1097. https://www.cnki.com.cn/Article/CJFDTOTAL-FXHX201907019.htm
    沈亚婷, 李迎春, 孙梦荷, 等. 波长与能量色散复合式X射线荧光光谱仪特性研究及矿区土壤分析[J]. 光谱学与光谱分析, 2017, 37(7): 2216-2224. https://www.cnki.com.cn/Article/CJFDTOTAL-GUAN201707044.htm

    Shen Y T, Li Y C, Sun M H, et al. Studies on characteristics on a combined wavelength and energy dispersion X-ray fluorescence spectrometer and determinations of major, minor and trace elements in soils around a mining area[J]. Spectroscopy and Spectral Analysis, 2017, 37(7): 2216-2224. https://www.cnki.com.cn/Article/CJFDTOTAL-GUAN201707044.htm
    李小莉, 薄玮, 徐进力, 等. 高压覆膜制样-X射线荧光光谱法测定多金属矿中的多种元素[J]. 中国无机分析化学, 2020, 10(2): 34-38. https://www.cnki.com.cn/Article/CJFDTOTAL-WJFX202002007.htm

    Li X L, Bo W, Xu J L, et al. Determination of multi elements in polymetallic ore by XRF with high pressure pressed pellet covered with polyester film[J]. Chinese Journal of Inorganic Analytical Chemistry, 2020, 10(2): 34-38. https://www.cnki.com.cn/Article/CJFDTOTAL-WJFX202002007.htm
    杨小丽, 刘星恒. XRF法测定以Cu、Pb、Zn为主的多金属矿中的主次元素[J]. 现代仪器, 2012, 18(4): 18-21. https://www.cnki.com.cn/Article/CJFDTOTAL-XDYI201204007.htm

    Yang X L, Lui X H. Determination of major and minor elements in Cu, Pb, Zn primarily polymetallic ore by X-ray fluorescence spectrometry[J]. Modern Instrumen, 2012, 18(4): 18-21. https://www.cnki.com.cn/Article/CJFDTOTAL-XDYI201204007.htm
    朱建明, 梁小兵, 李社红, 等. 湖北恩施渔塘坝自然硒的分布及其环境意义[J]. 地质论评, 2005, 51(4): 428-435. https://www.cnki.com.cn/Article/CJFDTOTAL-DZLP200504011.htm

    Zhu J M, Liang X B, Li S H, et al. The distribution of native selenium in Yutangba and its environmental significance[J]. Geological Review, 2005, 51(4): 428-435. https://www.cnki.com.cn/Article/CJFDTOTAL-DZLP200504011.htm
    李明龙, 徐辉, 许克元, 等. 恩施地区富硒地层分布规律及其控制因素探讨[J]. 资源环境与工程, 2018, 32(4): 557-562. https://www.cnki.com.cn/Article/CJFDTOTAL-HBDK201804009.htm

    Li M L, Xu H, Xu K Y, et al. Discussion on distribution regularity and controlling factors of selenium-rich strata in Enshi, Hubei Province[J]. Resources Environment & Engineering, 2018, 32(4): 557-562. https://www.cnki.com.cn/Article/CJFDTOTAL-HBDK201804009.htm
    余涛, 杨忠芳, 王锐, 等. 恩施典型富硒区土壤硒与其他元素组合特征及来源分析[J]. 土壤, 2018, 50(6): 1119-1125. https://www.cnki.com.cn/Article/CJFDTOTAL-TURA201806010.htm

    Yu T, Yang Z F, Wang R, et al. Characteristics and sources of soil selenium and other elements in typical high selenium soil area of Enshi[J]. Soils, 2018, 50(6): 1119-1125. https://www.cnki.com.cn/Article/CJFDTOTAL-TURA201806010.htm
    邹辉, 王卉, 段碧辉, 等. 恩施州宣恩地区富硒土壤硒含量特征及影响因素研究[J]. 资源环境与工程, 2018, 32(4): 546-550. https://www.cnki.com.cn/Article/CJFDTOTAL-HBDK201804007.htm

    Zou H, Wang H, Duan B H, et al. Study on selenium contents characteristics of selenium-rich soil in Xuan'en area of Enshi and its influencing factors[J]. Resources Environment & Engineering, 2018, 32(4): 546-550. https://www.cnki.com.cn/Article/CJFDTOTAL-HBDK201804007.htm
    李清彩, 赵庆令. 粉末压片制样波长色散X射线荧光光谱法测定钼矿石中9种元素[J]. 岩矿测试, 2014, 33(6): 839-843. http://www.ykcs.ac.cn/article/id/29977e2b-27e8-4c8c-9ca8-a1fa8c863efd

    Li Q C, Zhao Q L. Determination of 9 elements in molybdenum ore by wavelength dispersive X-ray fluorescence spectrometry with powder pelleting preparation[J]. Rock and Mineral Analysis, 2014, 33(6): 839-843. http://www.ykcs.ac.cn/article/id/29977e2b-27e8-4c8c-9ca8-a1fa8c863efd
    龚琦. 对电感耦合等离子体发射光谱法中一些问题的认识[J]. 冶金分析, 2018, 38(9): 26-30. https://www.cnki.com.cn/Article/CJFDTOTAL-YJFX201809005.htm

    Gong Q. Understanding of some issues about inductively coupled plasma optical emission spectrometry[J]. Metallurgical Analysis, 2018, 38(9): 26-30. https://www.cnki.com.cn/Article/CJFDTOTAL-YJFX201809005.htm
    • Related Articles
  • Supplements (0)

  • Cited by

    Periodical cited type(7)

    1. 赵令浩，孙冬阳，胡明月，袁继海，范晨子，詹秀春. 激光剥蚀-扇形磁场电感耦合等离子体质谱法同时测定锆石U-Pb年龄和微量元素含量. 岩矿测试. 2024(01): 47-62 . 本站查看
    2. 王奇奇，孙贺，顾海欧，侯振辉，葛粲，汪方跃，周涛发. 磺酸型阳离子树脂的元素分配行为及高精度同位素分析应用. 岩矿测试. 2024(01): 63-75 . 本站查看
    3. 曹瑞芹，杨忠芳，余涛. 镉锌稳定同位素地球化学及其在土壤等地质体中的危害与治理研究进展. 中国地质. 2024(03): 833-864 .
    4. 程文瀚，吴萌，赵艳丽，赵俊哲. 锌同位素环境地球化学研究进展. 高校地质学报. 2024(03): 312-321 .
    5. 李卫娜，蔡虹明，袁玮，郑旺，陈玖斌. 土柱实验在土壤重金属污染研究中的应用进展与展望. 地球与环境. 2024(05): 652-661 .
    6. 帅旺财，刘文奇，马丽雅，蔡虹明，陈玖斌，袁玮. 典型有色金属冶炼场地重金属来源解析及生态健康风险评估. 地球与环境. 2024(06): 756-770 .
    7. 夏亚飞，刘宇晖，高庭，刘承帅. 基于金属稳定同位素的矿冶影响区土壤重金属污染源解析研究进展. 地球科学进展. 2023(04): 331-348 .

    Other cited types(1)

Catalog

    Get Citation
    PDF
    XML
    Article views (494) PDF downloads (58) Cited by(8)
    Turn off MathJax
    Article Contents
    ABSTRACT
    References

    Competent Authorities：China Association for Science and Technology

    Sponsored by：Geological Society of China; National Research Center for Geoanalysis

    Address：No. 26 Baiwanzhuang Road, Xicheng District, Beijing 100037, China Email：ykcs_zazhi@163.com Tel：010-68999562

    京公网安备 11010202008159号 京ICP备2022024991号

    Supported by: Beijing Renhe Information Technology Co., Ltd.  Baidu Analytics

    /

    DownLoad:  Full-Size Img  PowerPoint
    Return
    Return