Abstract：The components in environmental soil are complex. In order to simultaneously detect the contents of major and minor components in soil, a method for the determination of major and minor components in environmental soil by X-ray fluorescence spectrometry (XRF) with fusion sample preparation was established. In order to prevent corrosion of Pt-Au crucible,environmental soil sample was pre-oxidized by burning in muffle furnace at 800 ℃ for 2 h in experiments. Then the glass melt was prepared under the following conditions: the mixed reagent of lithium tetraborate and lithium metaborate [m(Li2B4O7)∶m(LiBO2)=67∶33] was used as flux; the dilution ratio was 10∶1; the lithium bromide was selected as the release agent; the fusion temperature and time was 1 050 ℃ and 10 min, respectively. A series of soil certified reference materials was selected to draw calibration curve.The classical coefficient method was used to correct the calibration curves. The calibration curves of 21 components in environmental soil, including SiO2, TiO2, Al2O3, Fe2O3, Mn3O4, MgO, CaO, Na2O, K2O, P2O5, SO3, V2O5, Cr2O3, SrO, ZrO2, BaO, NiO, CuO, ZnO, PbO and HfO2, were established. The linear correlation coefficients of calibration curves were 0.998 95-1.000 00. The limits of detection were 0.007%-0.023%. 21 major and minor components in environmental soil sample were determined according to the experimental method, and the relative standard deviations (RSD, n=7) of determination results were 0.055%-7.3%. Three certified reference materials of environmental soil were determined according to the experimental method, and the found results of each component were consistent with the certified values.
于磊, 张晓, 郭诗锦, 王存璐. 熔融制样-X射线荧光光谱法测定环境土壤中主次组分[J]. 冶金分析, 2023, 43(4): 77-83.
YU Lei, ZHANG Xiao, GUO Shijin, WANG Cunlu. Determination of major and minor components in environmental soil by X-ray fluorescence spectrometry with fusion sample preparation. , 2023, 43(4): 77-83.
[1] 杨立国,乔冬云,胡鹏宇,等.全自动消解-电感耦合等离子体质谱法测定环境土壤中13种元素[J].中国土壤与肥料,2019(1):190-195. YANG Liguo,QIAO Dongyun,HU Pengyu,et al.Determination of thirteen element in soil by inductively coupled plasma mass spectrometry with automatic digestion instrument[J].Soil and Fertilizer Sciences in China,2019(1):190-195. [2] 郎闻生.微波消解-电感耦合等离子体质谱法测定环境土壤中银的研究[J].黑龙江环境通报,2018,42(4):44-47. LANG Wensheng.Determination of Ag element in soil by inductively coupled plasma mass spectrometry with microwave digestion[J].Heilongjiang Environmental Journal,2018,42(4):44-47. [3] 寿受立,邵宏翔.土壤环境背景值11种金属元素的测定[J].中国环境监测,1990,6(1):63-67. SHOU Shouli,SHAO Hongxiang.Soil environmental background values-determination of 11 metallic elements[J]. Environmental Monitoring in China,1990,6(1):63-67. [4] 柯鹏振,马先锋,熊志涛,等.ICP-AES法多条谱线测定环境土壤中钒[J].中国环境监测,2013,9(1):116-119. KE Pengzhen,MA Xianfeng,XIONG Zhitao,et al.The research of measuring the vanadium(Ⅴ) content in soil by ICP-AES method for selecting several characteristic spectrum lines[J].Environmental Monitoring in China,2013,9(1):116-119. [5] 罗立强,詹秀春,李国会.X射线荧光光谱分析[M].北京:化学工业出版社,2015. [6] 王雅婷,贾长城,何芳,等.X 射线荧光光谱法测定土壤中34 种主、次痕量元素[J].城市地质,2018,3(1):100-107. WANG Yating,JIA Changcheng,HE Fang,et al.Determination of 34 major,minor and trace elements in soil samples by X-ray fluorescence spectrometry[J].Urban Geology,2018,3(1):100-107. [7] 张慧敏,高明.波长色散 X 射线荧光光谱法测定土壤中的总磷[J].江西化工,2019(6):185-186. ZHANG Huimin,GAO Ming.Determination of total phosphorus in soil by wavelength dispersive X-ray fluorescence spectrometry[J].Jiangxi Chemical,2019(6):185-186. [8] 李小平,黄春长.XRF光谱法研究城市工业区的土壤环境污染[J].土壤,2007,39(4):572-573. LI Xiaoping,HUANG Chunchang.Study on the soil environment pollution in city industry zone by XRF method[J].Soils,2007,39(4):572-573. [9] 柳金良,张鑫,宋茂生.熔融制样-X射线荧光光谱法同时测定石煤钒矿中12种主次成分[J].化学分析计量,2019,28(3):25-28. LIU Jinliang,ZHANG Xin,SONG Maosheng.Simultaneous determination of major and minor components in stone coal vanadium ore by X-ray fluorescence spectrometry with fusion sample preparation [J].Chemical Analysis and Meterage,2019,28(3):25-28. [10] 范佳慧,周莉莉,朱春要,等.熔融制样-X射线荧光光谱法测定除尘灰中10种组分[J].冶金分析,2019,39(10):61-66. FAN Jiahui,ZHOU Lili,ZHU Chunyao,et al.Determination of ten components in dust ash by X-ray fluorescence spectrometry with fusion sample preparation[J].Metallurgical Analysis,2019,39(10):61-66. [11] 邢文青,叶玉峰,吴超超,等.熔融法制样-X射线荧光光谱法测定煤灰中主次成分的含量[J].理化检验(化学分册),2018,59(9):1049-1053. XING Wenqing,YE Yufeng,WU Chaochao,et al.Determination of 5 elements in ferrotitanium by X-ray fluorescence spectrometry with melting method for sample preparation[J].Physical Testing and Chemical Analysis (Part B:Chemical Analysis),2018,59(9):1049-1053. [12] 黄康,李仲夏,朱静,等.熔融制样-X射线荧光光谱法测定金红石中主次组分[J].冶金分析,2020,40(3):68-72. HUANG Kang,LI Zhongxia,ZHU Jing,et al.Determination of major and minor components in rutile by X-ray fluorescence spectrometry with fusion sample preparation[J].Metallurgical Analysis,2020,40(3):68-72.
