A radiochemical solvent extraction method has been developed for the simultaneous determination of submicrogram amounts of Cd and Hg using115mCd and203Hg tracers respectively and thionalide as a single complexing reagent. Hg was determined by 0.05% thionalide in ethyl methyl ketone (EMK) at pH 8.5, masking Cd with 0.1M KCN. From the aqueous phase Cd was demasked using formal-dehyde-acetic acid, pH adjusted to 9.5 and extracted into 0.05% thionalide in chloroform. The method is simple, fast and yields accurate results.