In this paper we report on the electrosynthesis of polythiophene from aqueous media with sulphuric acid as the supporting electrolyte. The redox features of polythiophene on a bare carbon graphite working electrode and on a clay montmorillonite host matrix is also reported. Co-polymerisation of polythiophene and polyaniline from an electrolyte media containing both aniline and thiophene monomers reveal that, the redox centres of the two polymers are independent, hence suggesting the formation of a bilayer, even though no charge rectification is observed.The role of sodium thiosulphate as a novel electrocatalyst which has led to a I. Introduction: Polyaniline, polythiophene, and polypyrrole are amongst the most well researched of electronically conducting polymers. They have received much in research because of their known unique properties such as low density, well behaved electrochemistry,versatility in methods of production, high anisotropy of electrical conduction, and non-metallic temperature dependence of conductivity . Electrochemical methods have played a significant role in the characterization and synthesis of these materials. The major advantage of these electrochemical techniques lies in the fact that, they are especially well- suited to the controlled synthesis of these compounds and for the tuning of a well-defined oxidation state. Despite all the advances made in the study of these novel materials, the preparation, characterization and application of these electronically conducting polymeric systems are still largely un-understood, hence still a major focus of research activity in electrochemistry. The key areas where gaps still exist include understanding the behavior of these systems, in particular on the mechanism of charge transfer and on charge transport processes that occur during redox reactions of conducting polymeric materials. On the applications frontier, research continues on how to perfect their use/application in the fields of energy storage, electrocatalysis, organic electrochemistry, bio-electrochemistry, photo-electrochemistry, electro-analysis, sensors, electrochromic displays, microsystem technologies, electronic devices, microwave screening and corrosion protection etc . The intensity of research geared towards understanding the electrosynthesis, charge transfer mechanism and possible applications domain for these polymers is captured in the litany of references listed (1- 61) and the references therein. In this paper we report on the electrosynthesis of polythiophene from aqueous media with the mineral acids as supporting electrolyte. This is in contrast to the much used non-aqueous media with large organic salts as supporting electrolyte. We also report on the novel role of sodium thiosulphate as an electro-catalyst in the polythiophene redox process leading to tremendous improvement in the film electrode transfer kinetics/faradaic process. II. Experimental Section: Analytical grade acids were used as received without further purification. The thiophene and aniline monomers were triply distilled until a colorless liquid was obtained prior to use. The liquids were purged using an inert gas and stored under nitrogen. Triply distilled water or de-ionised water from a Millipore-purification system was used, in preparation of the electrolyte solutions. The cyclic voltammograms were generated from a potentiostat/galvanostat used in conjunction with a universal programmer which generated the cyclical potential waves. The signals were then fed into an x-y recorder. The modification of the carbon graphite working electrode was achieved by cycling the potential of the working electrode within a given potential window in an electrolyte solution containing thiophene or aniline monomer. The clay montmorillonite modification of the carbon graphite working electrode surface was achieved as discussed by Orata and Segor (62-63).