The catalysts, sulphated zirconia and Fe(III) and Mn(II) ions containing sulphated zirconia were prepared by wet impregnation method. These catalysts were characterized for BET surface area, total surface acidity, elemental analysis and powder XRD. The catalytic activity of these catalysts was evaluated in vapour phase pinacol-pinacolone rearrangement of 2,3-dimenthyl-2.3-butanediol (pinacol). 2,3-dimethyl-2-butanone (pinacolone) and 2,3-dimethyl-1,4-butadiene were the two main products obtained. The effect of Fe(Ill), Mn(II) and their Mixture oil the physico-chemical characteristics and catalytic activity of sulphated zirconia was studied. The effect of nature of solvent oil the extent of conversion of pinacol and selectivity towards the products (ketone or diene) was also Studied. The activity of sulphated zirconia and its inodified forms was compared with the activity of pure ZrO2, Fe2O3 and MnO in the above mentioned reaction to evaluate the nature of effect Of support and metal ions.