The heavy metals, such as Pb(II) and radioisotope Cr(III), 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 of the utmost importance to protect biodiversity, hydrosphere ecosystems, and human beings. In this study, the reduced graphene oxide based inverse spinel nickel ferrite (rGONF) nanocomposite has been prepared and was utilized for the removal of Pb(II) and Cr(III) from aqueous solutions. The prepared rGONF has been confirmed by X-ray photoelectron (XPS) and Raman spectroscopy. The surface characteristics of rGONF were measured by scanning electron microscopy (SEM), High-Resolution Transmission Electron Microscope (HR-TEM), and Brunauer-Emmett-Teller (BET) surface analysis. The average particle size of rGONF was found to be 32.0 ± 2.0 nm. The surface site density for the specific surface area (Ns) of rGONF was found to be 0.00238 mol·g⁻¹, which was higher than that of the graphene oxide (GO) and NiFe₂O₄, which was expected. The prepared rGONF has been successfully applied for the removal of Pb(II) and Cr(III) by batch mode. The batch adsorption studies concluded that the adsorption of Pb(II) and Cr(III) onto rGONF was rapid and the adsorption percentage was more than 99% for both metal ions. The adsorption isotherm results found that the adsorptive removal of both metal ions onto rGONF occurred through monolayer adsorption on a homogeneous surface of rGONF. The pH-edge adsorption results suggest the adsorption occurs through an inner-sphere surface complex, which is proved by 2-pKa-diffusion model fitting, where the pH-edge adsorption data was well fitted. The adsorption of metal ions increased with increasing temperature. The overall obtained results demonstrated that the rGONF was an effective adsorbent for Pb(II) and Cr(III) removal from wastewater.