By using acetate-buffer (sodium acetate and acetic acid)/NaCl mixed solutions, the deintercalation of carbonate ions (CO32-) was conducted on MgAl-LDHs at different Mg/Al ratios-LDH2 (LDH with Mg/Al approximate to 2) and LDH3 (LDH with Mg/Al approximate to 3). When only an acetate-buffer solution was used, decarbonation did not take place even if the buffer solution was made acidic enough to dissolve LDH itself; however, the addition of NaCl to the buffer solution caused deintercalation of the carbonate ions from the MgAl-LDHs and the reaction was conducted without any morphological and weight change at 25 degrees C. Under the optimum conditions, full decarbonation was attained for the two MgAl-LDHs in minutes, and the obtained LDHs contained Cl- in the interlayer space without incorporation of any acetate anions due to their extremely low anion selectivity of acetate ion. The allowable range for the concentration of the decarbonation solution is wide, and the change in pH due to the decarbonation reaction is slight because of the buffering effect. The decarbonation was affected by the Mg/Al ratio of the LDH; i.e., the present LDH2 was slightly more difficult to decarbonate than LDH3, probably due to the higher layer-charge density of LDH2. (c) 2008 Elsevier Inc. All rights reserved.