A procedure for platinum and gold determination utilizing, neutron activation combined with radiochemical separation, has been developed. The reaction198Pt (n,
is used for Pt determination. Four procedures for gold separation are examined: (1) adsorption on untreated polyurethane foam (UPF). (2) extraction with dibutyl sulphide. (3) reduction of gold to elementary state in conc. H2SO4, and extraction of gold as diethyldithiocarbamate complex. The extraction with Cu(DDC)2 is chosen as the most suitable process and applied to platinum and gold determinations in Bowen's Kale and mice organs, previously treated with Biocisplatinum® specimens.