Nanosized lead oxide particles were prepared by thermal decomposition of lead hydroxycarbonate synthesized under microwave irradiation. Urea and lead nitrate were used as the starting materials. Microstructure and morphology of the products were investigated by means of XRD, AFM, TEM, and IR absorption spectra. The results indicated that well crystallized, finely dispersed and spherical alpha-PbO naroparticles with a size of ca. 30 nm were obtained. Meanwhile, an orthogonal phase beta-PbO with a size of ca. 3 8 nm was also obtained when the calcinations temperature was up to 600 degreesC. In addition, a Pb(II)-selective electrode based on cellulose acetate was prepared using nanosized alpha-PbO powders synthesized. The electrode exhibited a Nernstian slope of 29 +/- 1 mV per decade in a linear range of 2.5 x 10(-5) mol L-1 to 1.0 x 10(-1) mol L-1 for Pb2+ ion. The detection limit of this electrode is down to 8.0 x 10(-6) moI L-1. This sensor has a short response time of about 10 s and could be used in a pH range of 2.0-8.0. High selectivity was obtained over a wide variety of metal ions. (C) 2004 Published by Elsevier B.V.