This article describes the synthesis and extraction properties of new calix(aza)crown monomers and their polymer-bound analogues. These compounds have been synthesized by reacting calix-(aza)crowns (4a, 4b and 4c) with Merrifield's resin. Their cation phase-transfer studies were performed by using liquid-liquid extraction procedure. It has been inferred from the observations that monomer 4a shows a good extraction behavior toward selected alkali (Na+, K+, Cs+) and transition metal cations (Cu2+, Co2+, Cd2+, Ni2+, Hg2+, Pb2+), while 4b and 4c prefer Na+ and K+ among alkali metal cations, respectively. The polymer analogues 5a and 5b are efficient extractants for all the selected metal cations; whereas 5c is selective only for transition metal cations. (C) 2007 Elsevier Ltd. All rights reserved.