The heavy metals, such as Cr(VI), Pb(II) and Cd(II), in aqueous solutions are toxic even at trace levels and have caused adverse health impacts on human beings. Hence the removal of these heavy metals from the aqueous environment is important to protect biodiversity, hydrosphere ecosystems, and human beings. In this study, magnetic Nickel-Ferrite Nanoparticles (NFNs) were synthesized by co-precipitation method and characterized using X-Ray Diffraction (XRD), Energy Dispersive Spectroscopy (EDS) and Field Emission Scanning Electronic Microscopy (FE-SEM) techniques in order to confirm the crystalline structure, composition and morphology of the NFN’s, these were then used as adsorbent for the removal of Cr(VI), Pb(II) and Cd(II) from wastewater. The adsorption parameters under study were pH, dose and contact time. The values for optimum removal through batch-adsorption were investigated at different parameters (pH 3–7, dose: 10, 20, 30, 40 and 50 mg and contact time: 30, 60, 90, and 120 min). Removal efficiencies of Cr(VI), Pb(II) and Cd(II) were obtained 89%, 79% and 87% respectively under optimal conditions. It was found that the kinetics followed the pseudo second order model for the removal of heavy metals using Nickel ferrite nanoparticles.