Determination of Nine Major and Minor Elements in Si-Ca-Ba Alloy by X-Ray Fluorescence Spectrometry with Two-Step Fusion Sample Preparation

A method for the determination of the contents of five major elements (Si, Ca, Ba, Al, Fe) and four minor elements (P, Mn, Cu, Cr) in Si-Ca-Ba alloy was established by X-ray fluorescence spectrometry (XRFS) with two-step fusion sample preparation. Li₂B₄O₇, Li₂CO₃ and samples with the mass ratio of 6:0.5:0.2 and ammonium nitrate (1.0-2.0 g) were wrapped in filter paper and put into a porcelain crucible with graphite powder as the bottom in advance. The first step of melting was made under the condition of programmed temperature. After cooling, the molten ball was transferred to a Pt-Au crucible, 0.5-1.0 g of NH₄I as release agent was added, and the second step of melting was made in a muffle furnace at 1 100 ℃ for 10-15 min. After cooling and forming, the glassy slice of sample obtained was used for XRFS analysis. Standard sample series for calibration were prepared by melting certified standard samples and internal control standard samples, and the matrix effect was corrected by the correction formula established by empirical α coefficient method. The results showed that correlation coefficients of the calibration curves were more than 0.950 0. The proposed method was used for the analysis of actual samples, RSDs (n=10) of the determined values of nine elements were less than 4.0%, and the determined values were consistent with those obtained by the methods described in literatures.