We report a simple and efficient approach for graphene production, by electrochemical exfoliation of graphite rods, in acidic solutions. The applied bias and electrolyte concentration were optimized. The X-ray powder diffraction (XRD) patterns of nanosheets reveal the decreasing, or even the disappearance, of the graphene oxide peak by reducing the electrochemical exfoliation bias from +6 to +2.5 V. Thus, graphene with different oxidation degrees can be obtained by controlling the applied bias. An optimal graphene sample was prepared in a mixture of H₂SO₄ : HNO₃ (3 : 1 ratio; 1 M each) at a bias of +3 V. The interlayer spacing, crystallite size and the average number of layers were determined by XRD. The structural and morphological characteristics of the prepared samples were also investigated by Raman Spectroscopy, FTIR Spectroscopy, X-ray Photoelectron Spectroscopy (XPS), Transmission Electron Microscopy (TEM), Scanning Electron Microscopy (SEM), and Atomic Force Microscopy (AFM).

Two graphene samples co-doped with nitrogen and sulfur were synthesized by the hydrothermal method using thiourea as doping and reducing agent for graphene oxide (GO). An appropriate amount of thiourea was added to the aqueous dispersion of GO, previously sonicated for 30 min. The mixture was poured into an autoclave and placed in the oven for 3 h, at 120 and 200 °C. The samples were denoted NSGr-120 and NSGr-200, respectively, in agreement with the reaction temperatures. They were next morphologically and structurally characterized by advanced techniques, such as SEM/TEM, XPS, XRD, and FTIR. According to XPS analysis, the NSGr-120 sample has higher amounts of heteroatoms in comparison with NSGr-200, indicating that the reaction temperature is a crucial factor that affects the doping degree. In order to reveal the influence of the doping degree on the electrochemical performances of graphene-modified electrodes, they were tested in solutions containing L-cysteine molecules. The electrode with the best electrocatalytic performances, GC/NSGr-120, was tested to detect L-cysteine in a pharmaceutical drug, proving its applicability in real sample analysis.