光谱学与光谱分析, 2017, 37 (7): 2216, 网络出版: 2017-08-30  

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

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
作者单位
1 国家地质实验测试中心, 北京 100037
2 中国地质大学(武汉)材料与化学学院, 湖北 武汉 430074
摘要
波长与能量色散(WD-ED)复合式X射线荧光(XRF)光谱仪是一型国际上新近研发的XRF光谱仪。 该研究比较了此型光谱仪的特性, 建立了联用分析方法, 并用不确定度对所建方法进行了评估, 证明WD-EDXRF复合型光谱仪及其所建分析方法可用于土壤样品中主、 次、 痕量元素定量测定, 并兼具了WD和ED各自的优点。 研究表明: (1)对土壤质量和生态环境评价中具有重要意义的Mg, Al, P和K等元素, 因WDXRF对轻元素具有更高灵敏度, 故采用该型光谱仪和所建方法, 可弥补单一采用ED方法的不足, 从而为土壤质量和生态环境评价提供了更为灵敏和准确可靠的分析技术手段; (2)在本方法实验条件下, 采用WDXRF测定, 主元素Na2O, MgO, Al2O3, P2O5, K2O的检出限优于EDXRF, 而SiO2, SO3, CaO, MnO, Fe2O3则是由EDXRF测定的检出限更优。 对于谱线重叠较严重的微量元素, 多数情况下WDXRF的检出限更低; (3)对主元素而言, 总体上K及其原子序数之前的轻元素WDXRF准确度更好, Ca及其之后的元素EDXRF准确度更好。 然而, 由WDXRF和EDXRF获得的准确度也与样品相关, 在某些情况下, EDXRF测定K的准确度会更好。 微量元素和重叠干扰比较大的元素, 采用分辨率好的WDXRF可获得更好的准确度; 对于受其他元素谱线重叠影响较小的元素, EDXRF给出的结果准确度更好; (4)选用添加石蜡粘结剂的粉末压片法, 利用该方法制成的地质样品粉末压片结实、 无脱落, 未观察到掉渣、 掉粉现象, 且分析准确度和精密度良好; (5)利用所建立的WD-EDXRF方法测定了采自集中开采矿区和附近河流及河漫滩沉积物, 揭示矿区表层土含有较高浓度的Cu, Pb和Zn, 可为找矿提供指示信息; (6)进行了矿区周边农田土壤分析, 获得了元素分布趋势图, 揭示矿集区附近农田土壤Pb和As等浓度较高, 需要采取必要的生态与环境保护措施, 以减小和避免对于人类健康的潜在影响。
Abstract
The combination of wavelength dispersive and energy dispersion X-ray fluorescence analysis would take both of advantage of wavelength dispersive and energy dispersive. Now, A combined wavelength dispersive and energy dispersion X-ray fluorescence spectrometer was used in analysis of major, minor and trace elements in the soil samples taken from the fields around a Pb-Zn mine. The WD-ED XRF analytical method performance was evaluated by their uncertainty. The results revealed that (1) WDXRF shows more sensitive to the light elements, such as Na, Mg, Al, Si. (2) The limits of detections (LOD) of Na2O, MgO, Al2O3, P2O5, K2O by WDXRF are lower than those by EDXRF. The LODs of of SiO2, SO3, CaO, MnO and Fe2O3 are lower than those by WDXRF. For the minor and trace elements which have heavy overlap of spectral lines, WDXRF gives lower LOD; (3) For major elements, the analytical accuracy of the elements before K by WDXRF are better than those by EDXRF. For the elements after Ca, the accuracy by EDXRF are better. For minor and trace elements, if there are heavy overlapped spectral lines, WDXRF give more accurate results. Without heavy overlapped spectral lines, the accuracy of EDXRF is better; (4) Powder pellets with wax as binder were used in WD-EDXRF analysis without any observed drop of sample powder. Soil samples were determined. Generally, no significant differences were observed between measured results and certified values. (5) The WD-EDXRF method was applied to the determination of major, minor and trace elements in the surface soils in the mining area, and high concentrations of Cu, Pb and Zn were detectable; (6) The distributions of heavy elements were obtained in soils from the agricultural fields, and the high concentrations of Pb observed, which implies that the agricultural soils may have been polluted by the mining activities. And health risks need to be evaluated further.

沈亚婷, 李迎春, 孙梦荷, 何玉君, 王艳飞, 蔺雅洁. 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. SHEN Ya-ting, LI Ying-chun, SUN Meng-he, HE Yu-jun, WANG Yan-fei, LIN Ya-jie. 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.

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