The cobalt ferrite spinel oxide series, Co,Fe,_,O, (0 < x < 3), has been prepared by coprecipitation. The adsorption-desorption isotherms of all the compositions calcined between 200 and 600°C have been measured using nitrogen gas at -196°C. The structural and the phase changes were characterized by TGA and XRD techniques. The results obtained revealed that the transformation of y-to a-Fe,03 was accompanied by a sharp decrease in the S,,, values. The addition of Co2+ ions into Fe,O, up to x = 0.6 led to an observable increase in the SBET value. This behaviour was attributed to the incorporation of Co2+ ions into the Fe,03 lattice and the retardation of the phase transition of y-to a-Fe,O,. The minimum S,,, values obtained at a lattice composition of x = 1.0 corresponded to the formation of a cobalt ferrite normal spinel which is associated with the existence of narrow pores. The increase in S,,, values in the cobalt-rich region, with a maximum at x = 2.6 is explained on the basis of the cationic replacement of Fe3+ ions in the Co,O, lattice. Finally, calculation of pore volume distribution was carried out, in addition to E-t plots, in order to study the nature of the surface porosity, which was found to be mesoporous.