Adsorption is a process that occurs when a gas or liquid solute accumulates on the surface of a solid or, more rarely, a liquid (adsorbent), forming a molecular or atomic film (the adsorbate). Exchange adsorption, Physical adsorption and chemical adsorption have been recognized as adsorption types. This study involves the separation of an azeotropic mixture (benzene-cyclohexane) by adsorption technique using Eu-GAC(Granular Activated Carbon) and Sand. The Eu-GAC was produced by thermal pyrolysis of Eucalyptus tree branches and leaves and the Sand was collected from El-Khums seaside. The influence of several parameters such as dose or mass of adsorbent, pH, mesh number and contact time were investigated. The optimum adsorption efficiency occurred at pH 3. The optimum contact time for both adsorbents was found to be 3 hours. The adsorption of azeotropic mixture (benzenecyclohexane) improved by increasing adsorbent dose and mesh number (Mesh No 100). This study has concluded that it is possible to use activated carbon produced from locally available Eucalyptus trees (Eu-GAC) or Sand collected from seaside to separate the azeotropic mixture (benzene-cyclohexane) for obtaining a purified cyclohexane.