Different sets of perovskite-type oxides of general formula Pr 0.8 Sr 0.2 Co 1-x Fe x O 3-δ (x=0.0, 0.2, 0.5, 0.8 and 1.0) were successfully prepared by low-cost single-step combustion synthesis at low temperatures based on the auto-ignition reaction of a nitrate solution in the presence of citric acid. Thermogravimetric and differential thermal analysis was carried out on nitrate-citrate precursors to determine the perovskite-phase formation process. The results revealed that the nitrate-citrate precursor exhibited self-propagating combustion behavior. Pr 0.8 Sr 0.2 Co 1-x Fe x O 3-δ powders showed an orthorhombic single-phase, with their unit cell volume increasing as a function of the Fe content (x). Scanning electron microscopy observations showed that the prepared powders were nanocrystalline. The Pr 0.8 Sr 0.2 Co 1-x Fe x O 3-δ powders were characterized as fuel cell electrodes on Ce 0.8 Sm 0.2 O 2-δ pellets in symmetrical cells, and the electrochemical properties of the electrode/electrolyte interfaces were investigated using electrochemical impedance spectroscopy (EIS) as a function of the temperature, Fe content (x) and oxygen partial pressure.