Nanoparticles of polyaniline have attracted increasing attention for their smaller size and large surface area which may promote more effective doping, overcome the problem of process ability and lead to special electrical, optical, opto-electrical properties. In this work, polyaniline nanoparticles doped with beta-naphthalenesulfonic acid were prepared by a novel solid-state reaction synthesis method. Polyaniline was characterized by Fr-IR, XRD and cyclic voltammogrant on powder cavity microelectrode. The morphology of polyaniline particles was studied through SEM and TEM, and the electrical conductivity of pellets formed with polyaniline nanoparticles was measured by using a four-probe apparatus. Results showed that the average size of polyaniline particles doped with beta-naphthalenesulfonic acid obtained by this method was 30 similar to 50 nm run, and the polyaniline particles were spherical in shape. The measured electrical conductivity of pellets formed with polyaniline nanoparticles was 17 S/cm. XRD measurements indicated that the polyaniline nanoparticles were crystalline. The cyclic voltammogram of polyaniline naoparticles on powder microelectrode showed good electrochemical properties.