The new "upper-rim" functionalized 11,23-disemicarbazono-26,28-n-dipropoxy-25,27-dihydroxy calix[4]arene has been synthesized by condensing 11,23-diformyl-26,28-n-dipropoxy-25,27-dihydroxy calix[4]arene with semicarbazide hydrochloride. This calix[4]arene-semicarbazone derivative was then covalently linked with commercially available Merrifield's peptide resin at the "lower-rim" to obtain polymeric chelating resin and its analytical properties were investigated. The resin was then used successfully for the separation and preconcentration of lanthanum(III), cerium(III), thorium(IV) and uranium (VI) prior to their determination by spectrophotometry and inductively coupled plasma atomic emission spectroscopy. The resin exhibits good separating ability with maximum sorption between pH 2.5-4.5 for Th(IV) and between pH 5.5-7.0 for U(VI) whereas La(III) and Ce(III) were found to have maximum sorption between pH 6.5-8.5. The elution studies were carried out with 0.01 M HCl for La(III) and Ce(III), 2.0 M HCl for Th(IV) and 0.25 M HCl for U(VI). The preconcentration factors for La(III), Ce(III), Th(IV) and U(VI) were 125, 130, 102 and 108, respectively. The resin shows good stability along with faster rate of equilibrium for all the metal ions. The influence of several ions (cations and anions) on the resin performance is also discussed. The relative standard deviation was between 96 and 98% with good analytical reliability. The proposed method was applied for the determination of metal ions in monazite sand and some standard geological materials. (C) 2002 Elsevier Science B.V. All rights reserved.