Ba0.5Sr0.5Co0.6Fe0.4O3-delta(BSCF5564) was synthesized by nitric acid aided EDTA citric acid complexing sol-gel method (NECC). Both, the phase formation temperature and time of BSCF5564 synthesized NECC were found to be low i.e. single perovskite phase formation temperature is 200 degrees C less as compared to the conventional method of synthesis. The orthorhombic perovskite structure has been formed after calcination at 800 degrees C for 5 h. Scanning electron microscopy reveals the formation of porous material constituting nanosized and irregularly shaped rod-like structure with particle size approximately ranges from 90 to 160 nm. The total weight loss of the BSCF5564 sample comes out to be 6.6%, indicating that quadrivalence state Co4+ and Fe4+ in the sample have been completely reduced to the trivalent state Co3+ and Fe3+ due to thermal analysis. The value of E-a for BSCF5564 prepared by NECC was 0.2288 eV. The electrical conductivity of BSCF5564 synthesized by NECC is observed to be steady at high temperature (above 700 degrees C). Copyright (C) 2011, Hydrogen Energy Publications, LLC. Published by Elsevier Ltd. All rights reserved.