Ferroalloys refer to metallurgical products added to molten iron as deoxidizers,alloy additives, etc. during steelmaking. Their compositions directly affect the smelting quality and steel characteristics. The composition analysis methods of ferroalloys mainly include wet analysis and instrumental analysis.Currently used ferroalloy analysis methods have the shortcomings including complex operations, long analysis cycles, and the need for complete sample digestion. Some ferroalloys have incomplete digestion, which makes analysis difficult. We use the powder compression method to form smooth and flat compression samples, which can be directly detected by X-ray fluorescence instrument. The primary and secondary element contents of silicon iron,manganese iron, silicon manganese alloy, chromium iron, molybdenum iron, vanadium iron, and niobium iron powder after mixing are measured separately. Working curves are made compareing with the standard samples from different manufacturers, and the mineral effect is verified to be insignificant via caculating the linearity of the curves. Grind the initial sample and through the maximum apertures of 150, 104, 74, 53 μm, respectively.After mixing the powder sample with the adhesive, powder tablets are molded and then detected on the X-ray fluorescence instrument. It is determined that when the maximum particle size of the powder is less than 74 μm, the fluorescence intensity of the tablet samples tends to stabilize, and the effect of particle size on the analysis results can be basically eliminated. This research can meet the detection requirements for the content of primary and secondary elements in different types of ferroalloys.