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The sand, silt, shale and clay fractions soils derived from Maastrichtian sediments in the Afikpo Basin, southeastern Nigeria exhibit unusually high cation-exchange capacities. Smectite was identified by X-ray diffraction in all sample fractions and was selectively dissolved by treatment with 1HCl and 0.5 NaOH. Structural formulae, based on chemical analysis of the dissolved material, suggest that the smectite is intermediate in composition between a di- and a trioctahedral mineral and that the octahedral cation occupancy, together with the number of Mg and Fe atoms per unit cell, decreases with decrease in particle size of the soil fraction examined. The mean formula for the smectite in the clay separate is: [(M+= 0.40, Si = 3.33, Al = 0.67), (Al = 1.07, Fe2+= 0.09, Fe3+= 0.41, Mg = 0.82)] O10(OH)2. Similar analysis of smectite present in clay-size material separate from weathered granitic rock taken from the bases of the soilprofiles showed that it had close to the full trioctahedral inherited from the weathered granites.The clay mineralogy of the soils was affected by inherited smectite, probably of hydrothermal of deuteric origin. This mineral is unstable in the soil environment and, although its alteration products are fairly uniform in composition. Keywords: Dissolution, Granitic, Octahedral, Smectite, Soil