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La0.8Sr0.2Ga0.8Mg0.2-xCoxO3-δ (LSGMC) powders containing different amounts of Co (x = 0.05 and 0.085) were prepared by a citrate sol-gel method. Crystalline powders were obtained by firing at 1000°C (10 h) and dense high-purity pellets were prepared by pressing (300 MPa) and sintering in air at 1475°C (5, 10 and 20 h). The sintered pellets of LSGMC were characterized by X-Ray Diffraction (XRD) Scanning Electron Microscopy (SEM) and Energy Dispersive Spectroscopy (EDS). The conductivity of sintered LSGMC pellets containing different amounts of Co ions in the B sites of the perovskite lattice was assessed by electrochemical impedance spectroscopy (EIS) in the 250–750 °C temperature range. Conductivity values and apparent activation energies were in good agreement with previously published data referring to materials with same composition, but prepared by solid-state reaction.