The calcination products containing Mg(II), Al(III), and Fe(III) in the brucite-like layers with varying Mg/Al/Fe molar ratios at 550 degrees C were used as the adsorbent to remove perchlorate from aqueous solution, while the Mg/(Al-Fe) hydrotalcite compounds were synthesized by co-precipitation method at a constant pH value. The Mg/(Al-Fe) hydrotalcite compounds (HMAF) were characterized by XRD, FT-IR and TG-DTA. The characteristics showed that the layered double hydroxides structures in the HMAF were lost during calcination at 550 degrees C, but were reconstructed subsequent to adsorption of perchlorate, indicating that the 'memory effect' appeared to play an important role in perchlorate adsorption. Batch adsorption studies were conducted under various equilibration conditions, such as molar ratios of Mg/Al/Fe, calcined temperature, different initial solution pH, adsorbent dose, initial perchlorate concentration, and co-existing anions. It was found that the existence of ferric iron in calcined Mg/(Al-Fe) hydrotalcite compound (CHMAF) was favorable to removal of perchlorate from water, and the best ratio of Mg/Al/Fe is 3:0.8:0.2 (CHMAF5%). This study demonstrated that the calcination product of Mg/(Al-Fe) hydrotalcite-like compound was a promising adsorbent for control of the perchlorate pollution in water. (C) 2012 Elsevier B.V. All rights reserved.