By carrying out decarbonation of CO32--type MgAl-LDH (layered double hydroxide) using an acetate-buffer/salt solution under N-2 flow, CO32-LDH was successfully converted into ClO4- and NO(3)(-)LDHs, which contain only a little residual CO32-, in one step under mild conditions. Due to the superior anion-exchangeability, they serve as suitable intermediates for the preparation of LDH hybrids.