超细粉末压片-X射线荧光光谱法测定土壤和沉积物中21种主微量元素  

Determination of 21 major and trace elements in soil and sediment by X-ray fluorescence spectrometry with ultra-fine powder pressing

作　　者：马景治 肖伟 向兆 李策 董学林 张秦锋 MA Jingzhil;XIAO Weil;XIANG Zhao;LI Ce;DONG Xuelin;ZHANG Qinfeng(Hubei Geological Research Laboratory,Wuhan 430034,China;Key Laboratory of Rare Mineral,Ministry of Natural Resources,Wuhan 430034,China;Hubei Key Laboratory of Resources and Eco-Environment Geology(Hubei Geological Bureau),Wuhan 430034,China)

机构地区：[1]湖北省地质实验测试中心,武汉430034 [2]自然资源部稀土稀有稀散矿产重点实验室,武汉430034 [3]资源与生态环境地质湖北省重点实验室(湖北省地质局),武汉430034

出　　处：《分析试验室》2025年第1期29-35,共7页Chinese Journal of Analysis Laboratory

基　　金：湖北省地质局项目(KJ2023-38);国家重点研发计划项目(2021YFC2903000)资助。

摘　　要：本研究建立了土壤和沉积物中21种主微量元素的超细粉末压片-X射线荧光光谱分析方法。通过超细粉碎,土壤和沉积物样品在5 min内被粉碎至颗粒累积分布为90%的粒径(D90)小于30μm,最大限度降低粒度效应的影响,且不改变土壤、沉积物样品的原始矿物组成。研究中选择待测元素含量适中的样品确定最佳测量条件;采用经验系数法和RhKa散射线内标法校正元素间的吸收-增强效应;使用烧失量对测试数据进行归一化计算。本方法检出限优于熔融法(尤其是对轻元素如钠、氯),准确度显著高于常规粉末压片法;除氯、溴外,其他元素的精密度均小于2%。该方法的建立为实现珍贵样品的小取样量分析及地质样品的快速绿色分析提供了一种有效的分析手段。A new method was established for the determination of 21 major trace elements in soil and sediment samples.The particle sizes of the soil and sediment samples were decreased to D90 lower than 30μm within 5 min by ultra-fine grind to minimize the particle size effects,and the mineral composition of soil and sediment samples was relatively consistent before and after ultra-fine grind.Samples with moderate contents of elements were selected to optimize the measurement conditions,the absorption-enhancement effect between elements was corrected by the empirical coefficient and the Rh Ka scattering line internal standard,and the loss-on-ignition was used to normalize the testing data.The detection limit of this method was better than the fusion method(especially for light elements such as sodium and chlorine),the accuracy was significantly improved compared with the conventional powder pressing tableting,and the precision was less than 2%for the elements except chlorine and bromine.The present method can provide a promising tool for small amount analysis of precious samples and rapid green analysis of geological samples.

关 键 词：土壤 沉积物 超细粉末 压片 X射线荧光光谱法 

分 类 号：O657.31[理学—分析化学] X832[理学—化学]