The effects of dissolution medium, liberation time, adsorption temperature and Fe³⁺ addition amount on the determination results were discussed in this paper. The best determination conditions were determined, and the role of Fe³⁺ in ore dissolution and adsorption was discussed in detail. A trace amount of valence gold was separated and adsorbed by polyurethane foam. Gold was directly determined by graphite furnace atomic absorption spectrometry with thiourea solution to remove gold. The method is suitable for the determination of trace valence gold in stream sediments, soil and rocks. The detection limit of the method is 0.01 ng/g, the determination range is 0.03~300 ng/g, the recovery rates of valence gold are Au³⁺97.3%, Au⁺95.8%, Au⁰ 98.9%, respectively, and the separation precision (RSD, n=12) of valence gold is 7.3%~18.8%. Determination of valence gold by graphite furnace atomic absorption spectrometry can not only effectively inhibit interference of coexisting elements, but also reduce detection limit and improve sensitivity and accuracy. Automatic sample introduction reduces labor intensity and improves analysis and testing efficiency, thus suitable for testing large quantities of samples.