熔片制样-X射线荧光光谱法测定煤灰样品中主次量组分

Determination of Major and Minor Components in Coal Ash Samples by X-ray Fluorescence Spectrometry with Fused Bead Sample Preparation

采用混合熔剂熔融制备样片,用AxiosX射线荧光光谱仪测定煤灰样品中二氧化硅、氧化铝、氧化铁、氧化镁、氧化钙、氧化钠、氧化钾、二氧化钛、二氧化锰、五氧化二磷和三氧化硫等11种组分。重点研究了熔样比、熔样温度和标准样品的制备,解决了分析硫的难题。用基本参数法校正基体效应,分析方法的精密度(RSD,n=10)各组分均小于3%。用煤灰国家一级标准物质验证,结果与标准值相符。

A method for determination of SiO2, Al2O3, Fe2O3, MgO, CaO, Na2O, K2O, TiO2, MnO2, P2O5 and SO3 in coal ash samples by Axios X-ray fluorescence spectrometer with fused bead sample preparation was developed. The factors affecting analysis results including ratio of sample to flux, fusion temperature and preparation of standards were discussed. The matrix effect was corrected using fundamental parameter correction method. The method has been applied to the determination of these elements in National Standard Reference coal samples and the results are in agreement with certified values with precision （RSD, n = 10） of less than 3%.