This paper describes the determination of the individual platinum-group elements by X-ray fluorescence after nickel-sulphide fire-assay collection. The platinum-group sulphide residue obtained after the dissolution of the nickel is dissolved in acid, and reduced to the metal by use of sodium borohydride. The finely divided metals are then filtered onto a millipore filter, and measured by X-ray fluorescence spectroscopy. The procedure makes use of gold as an internal standard. Factors affecting the accuracy and precision are investigated.