Glutaraldehyde (GA)-crosslinked chitosan beads (GA-CS) are prepared with coagulating solution containing sodium tripolyphosphate and GA, and used for the adsorption of metals from binary-metal solution Au(III) and Pd(II). GA-CS exhibited selective sorption of Au(III) in the Au(III)-Pd(II) mixture. X-ray diffraction analyses showed that Au(III) was reduced to Au(0) following sorption, while Pd(II) was present as unreduced divalent form. Increased GA led to more selectivity toward Au(III), indicating that Au(III) selectivity is attributed to reduction-couple sorption of Au(III) with a reducing agent GA. Furthermore, a 2-step desorption process enabled selective recovery of Pd and Au using 5 M HCl and 0.5 M thiourea-1 M HCl, respectively, leading to pure Pd(II) and Au(III)-enriched solutions. This finding may open a new way to design reduction-coupled selectivity-tunable metal sorbents by combination of redox potentials of metal ions and reducing agents. (C) 2013 Elsevier B.V. All rights reserved.