Abstract: SHIMADZU MXF 2400 Multi-channel X-ray fluorescence spectrometer was used in the determination of silicon and iron in zincaluminumsilicon alloy. The effect of determination conditions including the sample surface smoothness and sample detection time on the determination results was studied. Under the optimized determination condition, the proposed method has been applied to the determination of silicon and iron in zincaluminumsilicon alloy. The results are in agreement with those by other methods with precision (RSD, n=11) of 1.15% for silicon and 0.44% for iron. The method provides the advantages of simple sample pretreatment, high sensitivity and high sample throughput.