As part of contribution for developing a green recycling process of spent lead acid battery, a nanostructural lead oxide was prepared under the present investigation in low temperature calcination of lead citrate powder. The lead citrate, the precursor for preparation of this lead oxide, was synthesized through leaching of spent lead acid battery paste in citric acid solution. Both lead citrate and oxide products were characterized by means of thermogravimetric-differential thermal analysis (TG-DTA). X-ray diffraction (XRD), and scanning electron microscope (SEM). The results showed that the lead citrate was sheet-shape crystal of Pb(C6H6O7)center dot H2O. When the citrate was calcined in N-2 gas, beta-PbO in the orthorhombic phase was the main product containing small amount of Pb and C and it formed as spherical particles of 50-60 nm in diameter. On combusting the citrate in air at 370 degrees C (for 20 min), a mixture of orthorhombic beta-PbO, tetragonal alpha-PbO and Pb with the particle size of 100-200 nm was obtained, with beta-PbO as the major product. The property of the nanostructural lead oxide was investigated by electrochemical technique, such as cyclic voltammetry (CV). The CV measurements presented the electrochemical redox potentials, with reversibility and cycle stability over 15 cycles. Crown Copyright (C) 2011 Published by Elsevier B.V. All rights reserved.