Five alkyl phosphate triesters (APTEs), including trimethyl phosphate (TMP), triethyl phosphate (TEP), triisopropyl phosphate (TPP), tributyl phosphate (TBP) and trioctyl phosphate (TOP), were used as activating agents for preparing activated carbons (AC-APTEs) with high surface acidity and metal ion sorption capacity. N-2 adsorption/desorption isotherms, surface morphologies, elemental compositions, results of Boehm's titration and sorption capacities of heavy metal ions of the carbons were investigated. AC-APTEs contained much more acidic groups and exhibited much less surface area (<500 m(2)/g) in comparison with activated carbon (AC-PPA, 1145 m(2)/g) obtained from phosphoric acid activation. For the AC-APTEs, AC-TOP had the highest surface area (488 m(2)/g), AC-TMP showed the highest yield (41.1%), and AC-TBP possessed the highest acidic groups (2.695 mmol/g), oxygen content (47.0%) and metal ion sorption capacities (40.1 mg/g for Ni(II) and 53.5 mg/g for Cd(II)). For the carbons, AC-APTEs showed much larger Ni(II) and Cd(II) sorption capacities than AC-PPA, except AC-TPP. The differences of the carbons in the physicochemical and sorption properties suggested surface chemistry of the carbons was the main factor influencing their sorption capacities whereas the pore structure played a secondary role. (C) 2014 Elsevier B.V. All rights reserved.