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%.