This study aimed to fabricate, characterize and investigate the applicability of nickel ferrite (NiFe2O4 decorated exfoliated graphite for adsorptive removal of oils and organic compounds. The exfoliated graphite/NiFe2O4 was synthesized via a simple two-step process: (i) exfoliation of the lowcost natural graphite flakes using H2O2 as oxidizing agent and H2SO4 as intercalating agent, (ii) decoration of magnetic NiFe2O4 using the acid citric-based sol-gel process. The synthesized exfoliated graphite/NiFe2O4 hybrid was then applied for the sorption of diesel oil, vegetable oil, gasoline, petroleum ether and tetrahydrofuran. Moreover, the recyclability of the used materials was investigated using either chemical or physical extraction method. Properties of the exfoliated graphite/NiFe2O4 hybrid were analysed using relevant techniques such as Scanning Electron Microscopy (SEM), Transmission Electron Microscopy (TEM), X-ray diffraction (XRD), and Vibrating Sample Magnetometry (VSM) and N2 adsorption/desorption measurement.