The guanidine ligand attached to vinylbenzyl chloride matrix as well as its sorption ability to tetrachloroaurate and dicyanoaurate ions were investigated upon using X-ray photoelectron spectroscopy. The form of metallic gold, Au(0), was not observed on gold loaded resin surface when solutions of tetrachloroaurate or potassium dicyanoaurate were used. Complete elution of gold was achieved for both regeneration media: thiourea solution and mixture of sodium hydroxide and benzoate. The results demonstrate that XPS can also be a powerful technique for the analysis of the oxidation state of sorbed metal and can be a suitable method for the confirmation of functional groups incorporated in the polymer. (C) 2003 Elsevier Ltd. All rights reserved.