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 fluo-rescence spectrometry with ultra-fine powder pressing
马景治 1肖伟 1向兆 1李策 1董学林 2张秦锋2
作者信息
- 1. 湖北省地质实验测试中心,武汉 430034;自然资源部稀土稀有稀散矿产重点实验室,武汉 430034
- 2. 湖北省地质实验测试中心,武汉 430034;自然资源部稀土稀有稀散矿产重点实验室,武汉 430034;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
- 折叠
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30 µm,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.
Abstract
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 30 μm 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 RhKa 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Key words
soil/sediment/ultra-fine grind/powder pressing/X-ray fluorescence spectrometry引用本文复制引用
出版年
2025
NETL
NSTL
万方数据