The ability to control composition and size in the synthesis of bimetallic nanoparticles is important for the exploitation of the bimetallic catalytic properties. This paper reports recent findings of an investigation of the synthesis of gold-platinum (AuPt) bimetallic nanoparticles in aqueous solution via reduction of AuCl4
− and PtCl4
2− using a combination of reducing and capping agents. In addition to characterization of the morphological properties of the AuPt nanoparticles using TEM and XRD, the electrocatalytic activity of the carbon-supported AuPt nanoparticle catalysts was also examined for oxygen reduction reaction (ORR) using the rotating disk electrode (RDE) technique. The findings have implications to the design of bimetallic nanoparticle catalysts for fuel cell reactions.