Abstract：As the determination of chromium, silicon and phosphorus in silicon-chromium alloy by traditional chemical wet analysis method was replaced by energy dispersive X-ray fluorescence spectrometry, the requirements of production could be met from the premise of reducing manpower and material resources as well as green environmental protection. The pressed powder pellet was selected for sample preparation. 40g of crushed sample was ground for 20s to prepare 120-mesh (124μm) sample for chemical analysis. Then 0.20g of stearic acid and 2.00g of microcrystalline cellulose were added into 25.00g of sample for chemical analysis. The mixture was ground for 90s to reduce the particle size not less than 200-mesh (74μm). The analysis surface of the prepared sample pellet was smooth and firm under the conditions above. According to the characteristics of chromium, silicon and phosphorus, the optimal working parameters of spectrometer were obtained. The contents of silicon and phosphorus were determined under vacuum condition using low power primary target without optical filter, while the content of chromium was determined using high power secondary target mode. Due to the lack of certified reference materials for silicochrome alloy, several silicochrome alloy in different production stages with certain content gradient (the contents were accurately determined by chemical wet method) were used as calibration samples to establish the calibration curve. The influence among elements, the matrix effect, the particle size effect and the spectral overlapping interference was corrected or reduced by the empirical coefficient method. The precision test indicated that the relative standard deviation (RSD, n=10) was 0.002%, 0.002% and 0.016% for chromium, silicon and phosphorus in silicochrome alloy, respectively. The trueness test for production sample of silicochrome alloy was also conducted. The results were consistent with those obtained by chemical wet method. The proposed method realized the simultaneous determination of chromium, silicon and phosphorus in silicochrome alloy by X-ray fluorescence spectrometer, which broadened the new application fields of instrument.
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