Determination of manganese, silicon, phosphorus and iron in medium-low carbon ferromanganese alloy by X-ray fluorescence spectrometry with fusion sample preparation
ZHANG Xiang, LU Xiao-ming, ZHANG Yi, HE Wei
Reasearch Institute of Baoshan Iron and Steel Co., Ltd., Shanghai 201900, China
Abstract：During the determination of major and minor components in ferromanganese alloy by X-ray fluorescence spectrometry (XRF) with fusion sample preparation, the etching of platinum-gold crucible by ferromanganese alloy in sample pretreatment is a difficulty which must be focused on and solved. The medium-low carbon ferromanganese alloy sample was oxidized stepwise at high temperature using lithium tetraborate as flux and lithium carbonate as oxidizer. The glass tablet of medium-low carbon ferromanganese alloy was successfully prepared. The determination method of manganese, silicon, phosphorus and iron in medium-low carbon ferromanganese alloy by XRF was established. The optimal sample preparation conditions were obtained in experiments: 8.0000g of lithium tetraborate was fused and built-up on wall of platinum-gold crucible for protection layer; 0.4000g of medium-low carbon ferromanganese alloy and 0.8000g of lithium carbonate were mixed; the crucible was transferred into melting furnace and kept at 650℃ for 20min, then at 700℃ for 20min, at 720℃ for 20min, at 750℃ for 40min, at 820℃ for 40min and finally at 1100℃. After taking out and cooling, about 0.6g of ammonium iodide was added. The crucible was then transferred into furnace; the sample was fused for 30min by swing to prepare uniform glass tablet. The experimental method was applied for the determination of manganese, silicon, phosphorus and iron in one actual sample of medium-low carbon ferromanganese alloy. The relative standard deviations (RSD, n=11) of determination results were between 0.24% and 1.0%. Two standard samples and three actual samples of medium-low carbon ferromanganese alloy were determined according to the experimental method, and the found results were consistent with the standard values or those obtained by wet chemical method. The proposed method could effectively solve the corrosion problem of platinum-gold crucible in fusion sample preparation of medium-low carbon ferromanganese alloy. The detection limit of phosphorus which was very concerned in medium-low carbon ferromanganese alloy was 0.0030% (mass fraction, similarly hereinafter), and the low limit of determination was 0.0090%. It could meet the testing requirements of medium-low carbon ferromanganese alloy. Moreover, the rapid and quantitative analysis of major and minor components was realized.
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