Electrochemical oxidation of methoxy substituted aniline (toluidine) has been done on both gold and platinum electrode cyclic voltametrically. The results were compared in different supporting electrolytes such as KCl, KNO3, H2SO4, HCl, etc. Effect of pH was observed on electrochemical oxidation of o- , m- & p- toluidine at gold and platinum electrode. During various scan single oxidation peak during first forward scan with no corresponding cathodic peak obtained while a new anodic cathodic couple peak appears in subsequent scan obtained. Kinetic parameters like heterogeneous rate constant, transfer co-efficient and diffusion co-efficient were also calculated. Micro quantities of toluidine by linear sweep voltammetry and hydrodynamic voltammetry were also determined.