Solvent extraction separation of platinum (IV) and palladium (II) was carried out with 2-ethylhexyl phosphonic acid mono-2-ethylhexyl ester (PC-88A) in toluene in the presence of stannous chloride. Platinum was quantitatively extracted from 0.5-2.25 M HCl with 5 x 10(-3) M PC-88A in toluene while palladium was extracted from 0.75-2.0 M HCl-HClO4 acid mixture with 6x10(-4) MPC-88A in toluene. Platinum from the organic phase was stripped with 4 M HCl and determined colorimetrically by the stannous chloride method at 403 nm while palladium was determined by direct spectrophotometry in the organic phase at 586 nm. Platinum was quantitatively separated from palladium in the ratios of 1:1, 1:5 and 10:1. The proposed methods were successfully applied for the analysis of platinum and palladium in real samples.