Coffee shell is an environmental concern to china along with steady growth of coffee production. This study attempt to characterize high specific surface area activated carbon (HSSA-AC). HSSA-AC was prepared from carbonized material which obtained from coffee shell by microwave irradiation. Textural properties and surface chemistry of HSSA-AC were found to be strongly depending on the activation time, KOH/C ratio and particle size. The textural properties of the samples were investigated by means of scanning electron microscope analyzer (SEM), cryogenic N2 adsorption, whereas, surface chemistry was probed through Fourier Transform Infrared (FTIR) spectrometer (Maldhure and Ekhe, 2011) and Hydrogen storage performance was tested by H2 adsorption. Maximum surface area of 3149 m2 g−1, Iodine adsorption value 2566 mg/g, Methylene Blue adsorption value 47.5 mL 0.1 g−1, the hydrogen adsorption value 0.91 wt% at 14 MPa and yield 39% was observed in case of microwave treated sample at activation time 9 min, KOH/C ratio 5 and particle size 0.25–0.71 mm. Results revealed usefulness of microwave treatment in influencing surface area of HSSA-AC which could be used in a hydrogen storage material research application.