Three kinds of redox fibers (fibers II, III, and IV) are prepared by amination of the reactive chloromethylated poly(vinyl acetate) grafting polystyrene-divinylbenzene fiber (fiber I) with diethanolamine, ethanolamine, or triethanolamine. The N-content of the fibers is 2.26, 2.71, and 1.86 mmol g(-1), respectively. Results of static adsorption experiments show that the adsorption amount of fibers II, III, and IV toward Au(III) reaches 550 mg g(-1), 620 mg g(-1), and 409 mg g(-1), respectively, between pH 2.0 and pH 3.0. Some adsorbed Au(III) can be reduced to Au(0). The reduction percentage of Au(III) adsorbed by fiber II increases with rising pH value of the solution and can be as high as 87% at pH 5.0. The amount of Au(IID adsorbed by fiber II increases with solution temperature, but decreases with ionic strength of the solution. The adsorption amount of fibers II and III toward Au(III) is less in ethanol or in acetacetate medium than in water. Kinetic adsorption data indicates that 50 min is needed for fiber II to adsorb half of its saturate adsorption amount of Au(III). It was proved by elemental analysis, infrared spectroscopy, nuclear magnetic resonance, and electron spectroscopy for chemical analysis determinations that the carbon atoms connecting with the hydroxy groups near the nitrogen atoms were easily oxidized into carbonyl ones during redox adsorption reaction of fibers II, III, and TV with Au(III). Some grains of gold adsorbed on fiber II were discovered under scanning electron microscopy.