Canakkale Onsekiz Mart University, Science and Arts Faculty, Department of Chemistry, 17100 Canakkale/Turkey E-mail: ydilgin@comu.edu.tr, ydilgin@yahoo.com Fax: 90-2862-180533 Department of Chemistry, Faculty of Arts and Sciences, Firat University, 23119 Elazig/Turkey Ege University, Science Faculty, Department of Chemistry, 35100 Bornova-lzmir/Turkey Manuscript received 15 January 2007, revised 12 July 2007, accepted 18 July 2007 The electrochemical study of a thiotriazole compound, S-benzyl-4-(4'-methylphenyl-4H-1,2,4-triazole-3-thiol (TTA) was made with cyclic voltammetry (CV) and differential pulse voltammetry (DPV) using glassy carbon electrode (GCE) as working electrode and an Ag/AgCI reference electrode in the Britton- Robinson buffer. The best results for electrooxidation of TTA were obtained in basic media (in 10% ethanol-0.2 M NaOH). This compound display one irreversible oxidation peak, which is attributed to a dimcrization process involving the formation of disulphide derivative (EC mechanism).