Professional Committee of Rock and Mineral Testing Technology of the Geological Society of China, National Geological Experiment and Testing CenterHost
2022 Vol. 41, No. 1
Article Contents

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

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

  • BACKGROUND

    At 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.

    OBJECTIVES

    To 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).

    METHODS

    WD-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.

    RESULTS

    By 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.

    CONCLUSIONS

    The 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.

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  • [1] 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

    CrossRef Google Scholar

    [2] 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

    CrossRef Google Scholar

    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

    CrossRef Google Scholar

    [3] 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.

    Google Scholar

    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.

    Google Scholar

    [4] 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.

    Google Scholar

    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.

    Google Scholar

    [5] 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.

    Google Scholar

    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.

    Google Scholar

    [6] 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.

    Google Scholar

    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.

    Google Scholar

    [7] 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.

    Google Scholar

    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.

    Google Scholar

    [8] 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.

    Google Scholar

    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.

    Google Scholar

    [9] 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.

    Google Scholar

    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.

    Google Scholar

    [10] 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

    CrossRef Google Scholar

    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

    CrossRef Google Scholar

    [11] 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.

    Google Scholar

    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.

    Google Scholar

    [12] 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.

    Google Scholar

    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.

    Google Scholar

    [13] 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.

    Google Scholar

    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.

    Google Scholar

    [14] 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.

    Google Scholar

    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.

    Google Scholar

    [15] 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.

    Google Scholar

    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.

    Google Scholar

    [16] 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.

    Google Scholar

    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.

    Google Scholar

    [17] 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,

    Google Scholar

    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.

    Google Scholar

    [18] 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.

    Google Scholar

    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.

    Google Scholar

    [19] 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.

    Google Scholar

    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.

    Google Scholar

    [20] 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.

    Google Scholar

    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.

    Google Scholar

    [21] 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.

    Google Scholar

    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.

    Google Scholar

    [22] 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.

    Google Scholar

    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.

    Google Scholar

    [23] 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.

    Google Scholar

    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.

    Google Scholar

    [24] 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.

    Google Scholar

    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.

    Google Scholar

    [25] 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.

    Google Scholar

    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.

    Google Scholar

    [26] 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.

    Google Scholar

    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.

    Google Scholar

    [27] 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.

    Google Scholar

    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.

    Google Scholar

    [28] 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.

    Google Scholar

    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.

    Google Scholar

    [29] 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.

    Google Scholar

    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.

    Google Scholar

    [30] 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.

    Google Scholar

    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.

    Google Scholar

    [31] 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.

    Google Scholar

    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.

    Google Scholar

    [32] 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.

    Google Scholar

    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.

    Google Scholar

    [33] 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.

    Google Scholar

    Gong Q. Understanding of some issues about inductively coupled plasma optical emission spectrometry[J]. Metallurgical Analysis, 2018, 38(9): 26-30.

    Google Scholar

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