岩矿测试2025，Vol.44Issue(6)：1166-1175,10.DOI:10.15898/j.ykcs.202410080209
高压粉末制样-X射线荧光光谱法测定地质样品中铌锆和主量元素
Determination of Niobium,Zirconium and Major Elements in Geological Samples by X-ray Fluorescence Spectrometry with High-Pressure Powder Pelletization
摘要
Abstract
Powder pelletization is a green and pollution-free sample preparation technique;however,conventional pressing at 400kN suffers from pronounced particle-size and mineral effects that often lead to large errors,and some samples are difficult to compact.Increasing the pressing load reduces inter-particle voids and thus mitigates mineral effects.In this work,800kN high-pressure pelletization was used to produce smooth,dense pellets from a wide range of silicate samples.Calibration curves were established with national certified reference materials of silicate rocks,sediments and soils.Matrix effects and spectral overlaps were corrected by empirical coefficients and internal standard methods.Comparison of surface morphology,calibration slopes and reproducibility showed that high-pressure pellets consistently outperformed those prepared at normal pressure:detection limits were lower and precisions for most analytes were below 1.0%.The relative standard deviations(RSDs,n=4)of GBW07453 for Nb and Zr were 1.66%and 0.77%,respectively—substantially better than those obtained with conventional pressing(3.80%and 1.55%).The analysis of actual samples showed that the measured values of niobium and zirconium were consistent with the chemical values.High-pressure pelletization enables the simultaneous determination of Nb,Zr and major elements in geological samples by XRF,and the results meet the requirements of analysis.关键词
高压粉末制样/X射线荧光光谱法/硅酸盐岩石/沉积物/土壤/铌/锆/主量元素Key words
high pressure sample preparation/X-ray fluorescence spectrometry/silicate rock/sediment/soil/niobium/zirconium/major elements分类
化学化工引用本文复制引用
曾江萍,吴磊,王娜,刘义博,王力强..高压粉末制样-X射线荧光光谱法测定地质样品中铌锆和主量元素[J].岩矿测试,2025,44(6):1166-1175,10.基金项目
中国地质调查局地质调查项目(DD20230801202,DD20221727) （DD20230801202,DD20221727）
