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The synthesized ultra-microporous zirconium–magnesium bimetal oxide was adroitly synthesized via the use of sol-gel technique. The synthesized composite was applied in the adsorption of copper, nickel and zinc cations from aqueous solutions. The composite properties were characterized by X-ray diffraction (XRD), Surface area (BET) by nitrogen adsorption–desorption, Thermo-gravimetric measurement (TG/DTG) and Fourier transformed infra-red (FTIR). The surface morphology of the synthesized composite was studied via the use of scanning electron microscopy (SEM) and fractal dimension concept. The influence of initial pH on sorption of copper, nickel and zinc cations in terms of removal efficiency was studied and deduced that the removal increases significantly with increasing the pH from 3 to 11. The intra-particle kinetic diffusion model confirmed that the adsorption mechanism controlled by multi-diffusion steps, comprising both film and intra-particle diffusion. The Toth isotherm model was elected to represent equilibrium of the concerned cations adsorption onto the composite. The thermodynamic parameters were calculated via the use of Flory-Huggins model.