A synthetic route for mass production of monodisperse gold nanoclusters and nanoparticles is presented. A nanometer-sized raspberry-like architecture, consisting of an aggregation of repeated sequences of a three dimensional gold nanoparticle (AuNP)-organic component-AuNP arrangement, has been prepared with a single-step procedure in a biphasic organic/water system. In the biphasic mixture, reduction of Au3+ by aniline monomers affords nanoclusters as well as a polyaniline colloid that controls the growth of the clusters into nanoparticles. The reaction parameters (ratio of reactants, time, and temperature) can be varied to control the size of the nanoclusters and nanoparticles from 0.73 nm to 5.5 nm in the polyaniline matrix. Finally, electrochemical degradation of the polyaniline matrix affords isolated monodisperse nanoclusters and nanoparticles. (C) 2012 The Electrochemical Society. [DOI: 10.1149/2.071207jes] All rights reserved.