Poly(o-anisidine) has been prepared using quinolinium fluorochromate C9H7NH[CrO3F] (QFC) as an oxidizing agent and the polymer was obtained in good yield. The detailed electrochemical studies have been performed in the presence of QFC in aqueous and non-aqueous media. TG analysis exhibited that the synthesized polymers have relatively high thermal stability. Conductivity of the polymers was found in the range of 10(-9) to 10(-3) Scm(-1) and the magnetic susceptibility measurement show the paramagnetic behaviour. The study also include the structural elucidation and external morphological properties of the synthesized polymers.