Determination of silicon, calcium, barium, phosphorus, aluminum in silicon-calcium-barium alloy by X-ray fluorescence spectrometry with fusion sample preparation
WANG Juan
Manufacturing Department of Panzhihua Steel & Vanadium Co., Ltd., Panzhihua 617000, China
Abstract：In order to eliminate the corrosion problem of platinum-gold crucible during fusion sample preparation of silicon-calcium-barium alloy, the silicon-calcium-barium alloy sample was melted to molten ball at high temperature in porcelain crucible with graphite at the bottom using lithium tetraborate-lithium carbonate (m∶m=2∶1) as the pre-oxidation flux. Then the molten ball was transferred into platinum-gold crucible to prepare glass sheets using lithium tetraborate as the flux. In this way, the corrosion problem of the platinum-gold crucible in the process of fusion and sample preparation was effectively solved. The determination of silicon, calcium, barium, phosphorus and aluminum in silicon-calcium-barium alloy by X-ray fluorescence spectrometry (XRF) with fusion sample preparation was realized. The optimal sample preparation conditions were obtained in experiments: 0.2000g of silicon-calcium-barium alloy sample, 2.0000g of lithium tetraborate and 1.0000g of lithium carbonate were mixed in a porcelain crucible with graphite underlay; after complete ashing at 500℃ and fusion at 900℃ for 15min, the mixture was taken out for cooling and then transferred into platinum-gold crucible; 3.0000g of lithium tetraborate and 0.50mL of 300g/L potassium iodide as release agent were added; after fusion at 1150℃ for 15min, the mixture was taken out for shaking followed by fusion for another 15min; finally the mixture was taken out for shaking, cooling and preparation of uniform glass sheets. The certified reference materials and internal control sample of silicon-calcium-barium alloy with proper concentration gradient were employed to prepare the calibration curves. The correlation coefficients of calibration curves were all greater than or equal to 0.9997. The precision test results indicated that the relative standard deviations (RSD, n=10) of the measured results were between 0.11% and 5.9%. The accuracy test results showed that measured values of silicon-calcium-barium alloy standard sample were consistent with the standard values. The silicon-calcium-barium alloy samples were analyzed according to the experimental method, and the found results were in good agreement with those obtained by the industry standard. Moreover, the t-test of paired data was carried out. It indicated that there was no significant difference between proposed method and the industry standard analysis method. The proposed method could meet the requirements of daily production inspection.
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