The chemical oxidation of aniline and its ring-substituted derivatives can produce materials with highly regular and reproducible nanoscale morphology. Polyaniline nanofibers are known to be obtained across a wide range of reaction conditions. We have prepared poly(o-toluidine) as both nanofibers or porous microspheres, depending on reactant concentrations. These materials have also been synthesized in the presence of gold nanoparticles (NPs) that were prepared by the reduction of HAuCl₄. Characteristic UV-Vis and FTIR spectra indicate their successful formation. Electron microscopy shows that the NPs are completely incorporated into the polyaniline nanofibers. However, the morphology of poly(o-toluidine) is altered when polymerized in their presence. These nanocomposites may offer enhanced electrical conductivity and additional reactivity relative to the well-characterized conducting polymers alone. They are being explored for use as components in biosensors and other electronic devices.