This study successfully developed an ion chromatography method for the detection of fluoride ions, chloride ions, and thiocyanate ions in fertilizer-grade ammonium sulfate. Due to the interference caused by the high concentration of sulfate ions in the sample on the detection results, we used SPEIC-Ba ion columns to purify the sample. Subsequently, the SH-AP-1 (5.5 μm, 4.0×250mm) chromatographic column was used for separation, and the conductivity detector was used for detection, with external standard method for quantitative analysis. During the method development process, we focused on optimizing the selection of Ba columns, the selection of chromatographic columns, and sample pretreatment. By systematically evaluating key indicators such as the linear range, detection limit, quantitation limit, accuracy, and precision of the method, all indicators met the expected standards. The method established in this study provides reliable technical support for the monitoring of fluoride ions, chloride ions, and thiocyanate ions in fertilizer-grade ammonium sulfate, which is of great significance for ensuring the quality and safety of fertilizer products.