Abstract：The calibration samples were artificially synthesized using the standard samples of silicon-manganese and manganese-iron in according to a certain proportion. The calibration curves were prepared, and the determination method of silicon, manganese and phosphorus in silicon-manganese alloy by X-ray fluorescence spectrometry (XRF) was established. The detection limit of silicon, manganese and phosphorus was 0.015 3%, 0.018 9% and 0.002 9%, respectively. In order to avoid the corrosion of silicon-manganese alloy sample to the platinum-gold crucible, the silicon-manganese alloy sample was oxidized successively with lithium carbonate and sodium peroxide. The selection of flux and oxidizing agent as well as the operation method of pre-oxidization were discussed. The results indicated that the sample could be uniformly dispersed in flux when the mass ratio between sample and lithium tetraborate was 1∶30 and five drops of 400 g/L ammonium bromide solution was used as releasing agent. Meanwhile, it was simultaneously applicable for the determination of high and low content components. The relative standard deviation (RSD, n=10) was 0.29%, 0.14% and 0.92% when the content of silicon, manganese and phosphorus was 24.58%, 65.20% and 0.190%, respectively. The proposed method was applied to the determination of silicon, manganese and phosphorus in silicon-manganese alloy, and the found results were consistent with those obtained by the wet method. It could meet the requirements of routine analysis.
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