A method is described that is suitable for the determination of gold in ores, concentrates, residues and solutions obtained from pilot-plant metallurgical research on complex sulphides. Gold(III) is selectively absorbed from nitric acid solution on an anion-exchange resin. Gold is eluted from the column with dimethylformamide-nitric acid at 65 °C. The gold in the eluate is determined by differential-pulse anodic stripping voltammetry using a glassy carbon electrode. The samples analysed ranged in gold concentration from 0.5 to 35 µg g^–1. Results obtained for gold in two Canadian Certified Reference Material Project ores were in good agreement with the certified values. The relative standard deviations were 1–2%.