The purpose of this work was to prepare graphite and lithium titanate (LTO) electrodes and test them for their use in Li-ion batteries. Electrodes were obtained by coating a paste consisting of active material, binder and a conductive additive on a current collector made of copper foil with a thin layer of conductive carbon. Li-ion cells were prepared as coin cells in a stainless steel case and in a commercial El-Cell. Electrochemical tests were performed in a two-electrode and three-electrode systems using cyclic voltammetry, constant current discharge/charge and electrochemical impedance spectroscopy. Dynamic light scattering was used to determine the particle size. The cyclic voltammogram for LTO shows current peaks without a diffusion tail, which means that the rate of intercalation of lithium ions is higher than the rate of charge transfer. For graphite, it can be seen that the intercalation process is gradual due to the structural reorganization of the active material. It also takes place at much lower potentials than that of LTO, which favours the SEI formation. The formations of SEI layer at graphite electrode is highly pronounced in the first charging/discharging cycle, leading to the deterioration of capacity. With LTO, the drop in capacity is much less pronounced. Stable discharge profiles were observed for LTO, while for graphite the voltages were continuously rising (charging) and falling (discharging). Coulombic efficiencies approached a value of 1 with every successive charging/discharging cycle. Electrochemical impedance spectroscopy spectra described the behavior of the electrode before and after cyclic voltammetry and proved an increase in polarization resistance and a decrease of diffusion rate of lithium cations in the case of the LTO electrode, while the resistance of the SEI and polarization resistance increased in the case of the graphite electrode. Three-electrode systems enabled simultaneous monitoring of the working electrode and the counter electrode (Li) with the help of a lithium reference electrode. The obtained results of voltage profiles and specific capacities did not show significant deviations in relation to two-electrode systems. Dynamic light scattering showed slightly higher uniformity and bigger particle size in LTO than graphite.