In this paper, for the first time, polypyrrole-coated electrospun nanofibre mats have been used as separation membranes to electrolessly recover An from aqueous [Au(III)Cl-4](-) solutions, based on a continuous-flow membrane separation process. With a [Au(III)Cl-4](-) solution passing through the nanofibre membrane, the Au(III) ions were converted into elemental An. The gold recovered was deposited on the nanofibre membranes in the form of An particles, as confirmed by EDX and XPS measurements. It has been found that the polypyrrole-coated electrospun nanofibres are good candidate membrane material for the recovery of An, and the recovery efficiency is affected by the membrane thickness, the permeate flux rate and the initial [Au(III)Cl-4](-) concentration. (c) 2007 Elsevier B.V. All rights reserved.