Ammonium perchlorate is widely used as an oxidizer in the propellant formulation and pyrotechnics. According to military standard, having high purity and free of impurities, such as chlorate, is very important because it affects the performance of ammonium perchlorate. Thus, the removal of impurities in the production of ammonium perchlorate has been highly studied. Herein, the removal of chlorate was investigated via reductive process using metal nanoparticles. Firstly, stabilized Ni/Fe bimetallic nanoparticles (S-Ni/Fe NPs) were synthesized and the structure and size of the particles were determined by XRD, FE-SEM, and EDS. Nano particles were obtained with particle size of 20-50 nm. Prepared nanoparticles were used for the selective removal of chlorate in aqueous ammonium perchlorate. The main factors that affect the removal process such as pH, reaction temperature, reaction time and amount of nanoparticles were considered and the optimum values were determined. Under optimal conditions, chlorate in the presence of perchlorate, with 1.5 molar ratio, showed a removal of 100 percent, while the perchlorate had been removed to a very small amount. The proposed method for the removal of chlorate in a saturated solution of ammonium perchlorate, which is used in the production process, showed satisfactory results.