Microwave irradiated lamellar double hydroxides containing different divalent metals (Mn2+, Zn2+, or Mg2+) were prepared with Al3+ as the trivalent metal. Samples containing Mn2+ and Zn2+ were unstable at 400 degrees C, leading to formation of mixed oxides and spinel phases. Acid-base properties of the samples were characterized by nitromethane and CO2 adsorption followed by FTIR spectroscopy. Decomposition of adsorbed nitromethane leads to isocyanate species that acts as probe molecules of acid-base sites at the surface. These properties determine the ability of materials to retain CO2. Indeed, whereas Mn-O sites are able to interact directly with CO2 molecules, Mg-O and Zn-O are able to form carbonate species as a result of the CO2 sorption.