The solvent extraction and precipitation methods have been used to develop a process to separate platinum and rhodium from a synthetic chloride solutions containing other associated metals such as (mg/L): Pt-364, Rh-62, Al-13880, Mg-6980. Fe-1308 at <1 M HCl acidity. At pH 3.4, the quantitative precipitation of Al and Fe was achieved using 10 wt% Na3PO4.12H(2)O, with similar to 4% loss of Pt and Rh due to adsorption phenomenon. The selective separation of platinum was carried out with 0.01 M Aliquat 336 (a quaternary ammonium salt) at an aqueous to organic ratio (A/O) of 3.3 in two stages. Stripping of Pt from loaded organic (LO) at O/A ratio 6 with 0.5 M thiourea (tu) and HCl indicated that similar to 99.9% stripping efficiency. In stripping studies, needle like crystals of Pt were found and identified as tetrakis (thiourea) platinum (II) chloride ([Pt(tu)(4)]Cl-2). The selective precipitation of rhodium was performed with (NH4)(2)S from platinum free raffinate with a recovery of >99%. (C) 2012 Elsevier B.V. All rights reserved.