This report presents the effect of synthesis conditions on the synthesis of graphene nanosheets via electrochemical exfoliation method for adsorbing methylene blue from aqueous solution. Oxygen-containing functional groups and defects in the material were characterized by Raman and X-ray photoelectron spectroscopy (XPS). As a result, by using voltage of 15 V, (NH4)2SO4 (5%, 250 mL) and KOH (7.5%, 250 mL), the obtained material showed the highest MB adsorption capacity due to the high densities of oxygen-containing groups and defects comparison to other conditions.