We synthesized magnetic nickel ferrite nanoparticles by auto-combustion method using microwave radiation. Iron(III) nitrate nonahydrate, nickel nitrate pentahydrate and glycine as reactants were mixed. Then, this mixture was transferred into a domestic microwave oven with a power of 900 W for 30 min. The product was characterized by X-ray Diffraction (XRD), Fourier Transform Infrared spectroscopy (FT-IR) and Scanning Electron Microscopy (SEM). Also, application of synthesized nickel ferrite nanoparticles was studied for adsorption of Congo Red as an organic pollutant from aqueous solution.