1. Baowu Steel Group Shaoguan Iron and Steel Co., Ltd., Shaoguan 512123, China; 2. China MetallurgicalInformation and Standardization Institute, Beijing 100730, China; 3. Research Institute of Baoshan Iron andSteel Co., Ltd., Shanghai 201900, China
Abstract：During the determination of alloy samples by X-ray fluorescence spectrometry (XRF) with fusion sample preparation, the problem of platinum-gold crucible corrosion in alloy sample pretreatment should be emphatically solved. Anhydrous lithium tetraborate was selected as flux and barium dioxide-lithium carbonate was used as oxidizer. A determination method of manganese, silicon and phosphorus in ferromanganese and silicomanganese alloy by XRF with fusion sample preparation was established. The fusion sample preparation technique with low temperature preoxidation was adopted to solve the problem of platinum-gold crucible corrosion by ferromanganese and silicomanganese alloy. The influence of ignition loss or ignition increase of ferromanganese and silicomanganese alloy on determination results was eliminated with carbon ignition loss base and elimination term. The effect of experimental conditions (such as dilution ratio, addition amount of oxidizer, fusion temperature and fusion time) on determination of manganese, silicon and phosphorus in ferromanganese and silicomanganese alloy was further discussed. The following optimum conditions were obtained: the dilution ratio (mAnhydrous lithium tetraborate∶mSample) was 7∶0.25; 0.5000g of barium dioxide and 0.5000g of lithium carbonate were used as oxidizer; the fusion temperature was 1100℃; the static fusion time was 150s. The detection limit of manganese, silicon and phosphorus in method was 10μg/g, 25g/g and 18μg/g, respectively. The precision tests were conducted with national certified reference materials of ferromanganese (GSB03-1687-2004) and silicomanganese alloy (GSB03-1316-2000) under the optimal experimental conditions. The relative standard deviations (RSD) of determination results were 0.088% and 0.053% (Mn), 0.35% and 1.1% (Si), and 2.9% and 1.2% (P), respectively. The actual samples of ferromanganese and silicomanganese alloy were determined according to the experimental method, and the results were consistent with those obtained by the national standard method. The proposed method could meet the requirements of routine analysis.
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