Hydrous oxides of cerium, aluminum, nickel and copper were prepared by alkaline precipitation method. Langmuir adsorption isotherm was studied and specific surface area was measured by BET method through N2 adsorption-desorption process. IR characterization of hydrous metal oxides before and after fluoride adsorption was also studied. Results show that different hydrous metal oxides have different specific surface areas and their pore size distributions also are not all the same. Adsorption capacity is not directly dependent on the specific surface area. Isotherm study indicates that the adsorption follows Langmuir model and shows the feature of monolayer adsorption. IR study before and after fluoride adsorption shows that different hydrous metal oxides have similar adsorption sites in the same IR region as well as adsorption sites in the different IR region. The comprehensive interaction of these adsorption sites with fluoride ions results in the different adsorption capacity of different hydrous metal oxides.