熔融制片-X射线荧光光谱法测定磷矿石中主次量组分

Determination of Major and Minor Components in Phosphate Ores by X-ray Fluorescence Spectrometry with Fused Bead Sample Preparation

采用四硼酸锂-偏硼酸锂混合熔剂熔融制备样片,用Axios型X射线荧光光谱仪测定磷矿石样品中五氧化二磷、氟、二氧化硅、三氧化二铝、总三氧化二铁、氧化镁、氧化钙、氧化钠、氧化钾、二氧化钛、氧化锰、氧化锶和硫等13种组分。重点试验了熔样比、熔样温度和标样制备。用基本参数法校正基体效应,分析方法的精密度(RSD,n=10)除二氧化钛、氟和硫分别小于10.8%、6.0%及10.2%外,其余各组分均小于4.5%。用磷矿石国家一级标准物质验证,结果与标准值相符。

A method for determination of P2O5, F, SiO2, Al2O3, TFe2O3, MgO, CaO, Na2O, K2O, TiO2, MnO, SrO and S in phosphate ores by Axios X-ray fluorescence spectrometer using fusion bead sample preparation with Li2BaOT-LiBO2 mix flax was developed. The factors affecting the determination such as ratio of sample and flux, fusion temperature and preparation of calibration standards were studied in details. The matrix effect was corrected using fundamental coefficient method. The method has been applied to the determination of these elements in National Standard Reference phosphate ores and the results are in agreement with certified values with precision of less than 4.5% RSD （n = 10） with the exception of TiO2 （ 〈 10. 8% RSD）, F（ 〈 6.0% RSD） and S（ 〈 10. 2% RSD）.