Doping and functionalization could significantly assist in the improvement of the electrochemical properties of graphene derivatives. Herein, we report a one-pot synthesis of fluorinated graphene oxide (FGO) from graphite. The surface morphology, functionalities and composition of the resulting FGO have been studied using various surface characterization techniques, revealing that layer-structured nanosheets with ˜1.0 at. % F were formed. The carbon bound F exhibited semi-ionic bonding characteristic and significantly increased the capacitance of FGO compared to graphene oxide (GO). Further, the FGO has been employed for the simultaneous detection of heavy metal ions Cd2+, Pb2+, Cu2+ and Hg2+ using square wave anodic stripping voltammetry; and a substantial improvement in the electrochemical sensing performance is achieved in comparison with GO.