Agricultural residues rich in lignocellulosic biomass are low-cost and sustainable adsorbents widely used in water treatment. In the present research, thermodynamics, kinetics, and equilibrium of nickel(II) and lead(II) ion biosorption were studied using a corncob (Zea mays). The experiments were performed in a batch system evaluating the effect of temperature and dose of adsorbent. Langmuir and Freundlich isotherms were used to study the equilibrium. Thermodynamic and kinetic parameters were determined using kinetic models (pseudo-first order, pseudo-second order, Elovich). Biosorbent characteristics were studied by Fourier-transform infrared spectroscopy, Scanning Electron Microscopy and Energy-dispersive X-ray spectroscopy. It was found that the hydroxyl, carboxyl, and phenolic groups are the major contributors to the removal process. Besides, Pb(II) ions form micro-complexes on the surface of the biomaterial while Ni(II) ions form bonds with active centers. It was found that the highest Ni(II) removal yields were achieved at 0.02 g of adsorbent and 70°C, while the highest Pb(II) removal yields were achieved at 0.003 g and 55°C. A maximum Ni(II) adsorption capacity of 3.52 mg∙g–1 (86%) and 13.32 mg∙g–1 (94.3%) for Pb(II) was obtained in 250 and 330 min, respectively. Pseudo-first order and pseudo-second order models best fit experimental data, and Langmuir and Freundlich models well describe the isotherm of the process. Thermodynamic parameters (ΔH0, ΔG0, ΔS0) suggest that the adsorption process of both cations is exothermic, irreversible, and not spontaneous.