A selective solid-phase extraction procedure using chemically modified Amberlite XAD-4 with monoaza dibenzo 18-crown-6 ether was investigated for the preconcentration and separation of La(III), Nd(III) and Sm(III) in synthetic solution. Before loading samples on synthesized adsorbent adjust pH 4.5 by suitable buffer solution. The adsorbed rare earth elements were eluted by 2 M hydrochloric acid. Various parameters like preconcentration, breakthrough capacity, flow rate were investigated. The limits of detection (n = 5) and limits of quantification (n = 5) for La(III), Nd(III) and Sm(III) were founded 3.9, 4.2 and 7.4 mu g L(-1) and 13, 15 and 26 mu g L(-1), respectively. The eluted metal ions were determined by ICP-AES. (C) 2010 Elsevier Ltd. All rights reserved.