岩矿测试2025，Vol.44Issue(2)：305-315,11.DOI:10.15898/j.ykcs.202403040030
粉末压片-X射线荧光光谱法测定小样品量土壤和沉积物中主量元素
Determination of Major Elements in Small-Weight Soil and Sediment Samples by X-Ray Fluorescence Spectrometry with Pressed-Powder Pellets
摘要
Abstract
The analysis of small-weight samples utilizing X-ray fluorescence spectrometry(XRF)poses a pivotal technical challenge in determining the chemical composition of valuable and scarce materials.Furthermore,the application of XRF to verify the homogeneity of reference materials has sparked debates regarding the minimum sample weight.At present,most of the geological samples(including reference material)are at the particle size of 74μm(-200 mesh)and the conventional sample weight is approximately 4g for XRF analysis with pressed-powder pellets.Here,0.1g weight soil or sediment was used for pressed-powder pellet preparation.The diameter of the XRF spectrometry sample box mask was changed to 12mm,and the diameter of the field view light barrier was reduced to 10mm.Based on the previously optimized instrumental measurement conditions,we successfully established a 0.1g sample weight analytical method for the quantification of ten major elements(SiO2,Al2O3,TFe2O3,MgO,Cao,Na2O,K2O,Mn,Ti,and P)utilizing wavelength dispersive XRF,which significantly reduced the necessary sample weight.This method 1employed a diverse range of 32 geochemical reference materials,encompassing variou types and content gradients.The detection limit of the 0.1g sample weight analysis method was between 14μ/g and 0.35%,and the precisioniitalic>=12)was less than 3.9%.Through comparative analysis,the results of the erence materials were all within the standard value range,and the absolute value of relative error(|RE|)was between 0 and 15.7%.There was no significant difference with the 4g sample weight analysis results(|RE|ranged from 0.3%to 28.3%).The practical sample results determined by the method of 0.1g sample and the conventional method of 4g sample are consistent.The established XRF method for the 0.1g weight sample is reliable.关键词
X射线荧光光谱法/粉末压片/样品量/土壤/沉积物Key words
X-ray fluorescence spectrometry/pressed-powder pellets/sample weight/soil/sediment分类
化学化工引用本文复制引用
赵红坤,顾雪,陈宏强,刘亚轩,马生明,张艳飞,张鹏鹏,李强,李振清,陈其慎,李勇..粉末压片-X射线荧光光谱法测定小样品量土壤和沉积物中主量元素[J].岩矿测试,2025,44(2):305-315,11.基金项目
中国地质调查局地质调查项目(DD20230040,DD20242247) （DD20230040,DD20242247）
国家重点研发计划项目(2018YFE0208300,2021YFC2903001) （2018YFE0208300,2021YFC2903001）
河北省中央引导地方科技发展资金项目(246Z4205G) （246Z4205G）
