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X射线荧光光谱分析方法是测量重金属的一种常用的分析方法，其操作简单、分析速度快，且可实现无损检测，但其应用多集中在岩土、合金等固态样品分析领域，如何将X射线荧光光谱分析方法扩展于液体样品领域，实现水体重金属快速、灵敏的检测具有重要的现实意义。选择一种具备高效富集的滤膜载体，是提升X射线荧光光谱测定水中重金属分析方法灵敏度和正确度以及应对复杂基底样品能力的核心，滤膜载体影响方法的工作曲线的相关系数、检出限、重复性。通过筛选不同材质的滤膜，将待测溶液滴加到滤膜进行烘干或自然晾干后，将富集了重金属的混合纤维滤膜（直径50 mm、孔径0.45μm）与X射线荧光光谱分析仪结合，发现Cr、Mn、Fe、Co、Ni、Cu、Zn、As、Cd、Pb等10种元素中除As之外其他元素工作曲线相关系数均大于0.99；除Cd之外其他元素的精密度均小于10%；发现各元素的回收率在70.0%～120%。方法具有较好的精密度和正确度，可以作为一种快速测定污水中重金属的分析方法。
Abstract：X-ray fluorescence analysis is a widely used method for measuring heavy metals,characterized by simple operation,rapid analysis,and non-destructive testing. However,its applications are mainly focused on the analysis of solid samples such as rocks,soils,and alloys. Extending the X-ray fluorescence analysis method to the field of liquid samples for the rapid and sensitive detection of heavy metals in water bodies is of great practical significance. Selecting a filter membrane carrier with high enrichment efficiency is crucial for improving the sensitivity,accuracy,and the ability to handle complex substrate samples in the X-ray fluorescence analysis of heavy metals in water. The filter membrane carrier influences the correlation coefficient of the method's working curve,detection limit,and repeatability. Through screening different types of filter membranes,adding the test solution onto the filter membrane,and drying it by baking or natural air-drying,and then combining the hybrid fiber filter membrane(diameter 50 mm,pore size 0. 45 μm) enriched with heavy metals with an X-ray fluorescence spectrometer,it was discovered that the correlation coefficients of the working curves for nine elements among Cr,Mn,Fe,Co,Ni,Cu,Zn,As,Cd,and Pb(excluding As) were all greater than 0. 99. The precision of all elements except Cd was less than 10%. The recoveries of each element were in the range of 70. 0%-120%. This method shows good precision and accuracy,and it represents a feasible analytical approach for the rapid determination of heavy metals in industrial wastewater.
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基本信息:
DOI：10.20236/j.CJIAC.2025.06.004
中图分类号:O657.34;X832
引用信息:
[1]申田田,陈阳,颜亮亮等.滤膜富集载体-X射线荧光光谱仪联用快速测定工业废水中重金属[J].中国无机分析化学,2025,15(06):776-783.DOI:10.20236/j.CJIAC.2025.06.004.
基金信息:
湖南省重点研发计划项目（2023SK2073）