Determination of silicon, phosphorus, manganese, aluminum, calcium and chromium in ferrosilicon by X-ray fluorescence spectrometry with fusion sample preparation
YANG Xin-neng, LI Xiao-qing, YANG Da-jun, TANG Ben-qin
Manufacturing Department of Panzhihua Steel & Vanadium Co., Ltd., Panzhihua 617000, China
Abstract：During the determination of ferrosilicon sample by X-ray fluorescence spectrometry (XRF) with fusion sample preparation, the corrosion of platinum-gold crucible by alloy sample in sample pretreatment should be solved. Ferrosilicon sample was pre-oxidized and fused at high temperature in porcelain crucible with graphite on the bottom using lithium tetraborate-lithium carbonate as the pre-oxidation reagent. Then the melt was transferred into platinum-gold crucible for sample preparation using lithium tetraborate as flux. The determination of silicon, phosphorus, manganese, aluminum, calcium and chromium in ferrosilicon by XRF with fusion sample preparation was realized. The flux system and oxidation method in pre-oxidation fusion as well as the dilution ratio between sample and flux were investigated in experiments. The results showed that the prepared sample was uniform and transparent without bubbles, which could meet the determination requirements, under the following conditions: the dilution ratio between sample and flux was 1∶35; the release agent was 10 drops of 300g/L potassium iodide solution; the sample was fused at 1100℃ for 30min. The certified reference materials of ferrosilicon with series of concentration gradient were employed to prepare the calibration curves. The linear correlation coefficients of calibration curves for testing elements were all higher than 0.9995. The proposed method was applied for the determination of silicon, phosphorus, manganese, aluminum, calcium and chromium in actual sample of ferrosilicon. The relative standard deviations (RSD, n=11) of determination results were between 0.1% and 5.8%. The accuracy test showed that the determination results of ferrosilicon standard sample were consistent with the certified values. The determination results of actual ferrosilicon samples were consistent with those obtained by national standard methods. The proposed method could meet the requirements of routine analysis.
杨新能, 李小青, 杨大军, 唐本芹. 熔融制样-X射线荧光光谱法测定硅铁中硅磷锰铝钙铬[J]. 冶金分析, 2019, 39(10): 43-48.
YANG Xin-neng, LI Xiao-qing, YANG Da-jun, TANG Ben-qin. Determination of silicon, phosphorus, manganese, aluminum, calcium and chromium in ferrosilicon by X-ray fluorescence spectrometry with fusion sample preparation. , 2019, 39(10): 43-48.
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