The electrochemical polymerizations and characterization studies were made for thernmonomers 3-hexylthiophene (3HT) and 3-methylthiophene (3MT) with respect to Pt, GC andrnAu electrodes. The electrochemical properties of the corresponding polymers poly(3-rnhexylthiophene) (P3HT) , poly(3-methylthiophene) (P3MT) were also studied in a monomerrnfree LiClO4 - acetonitrile solutions. Copolymers were shown to be electrochemicallyrnsynthesized from the monomers 3HT and 3MT and showed intermediate electrochemicalrnproperties between their corresponding homopolymers. The optimum copolymer ratio,rnpolymerization potential and deposition time that are required to obtain the bestrnelectrocatalytic effect was also demonstrated using various redox species. The electrocatalyticrneffect of this copolymer was studied on selected inorganic and organic samples. It was foundrnthat poly(3HT-co-3MT) modified platinum electrode is highly selective and sensitive towards these redox species. The detection limits for poly(3HT-co-3MT) modified Pt electrode were also shown for these redox species.rnKey words; poly(3-hexylthiophene), poly(3-methylthiophene), poly(3HT-co-3MT),rnElectrochemical Polymerization, Electrocatalysis.