Platinum group elements (PGEs) find extensive use in high technology applications due to their unique chemical and physical properties. Some of these are in vehicle exhaust catalysts, medicine, electronic and chemical industries, etc. The widespread use of PGEs for various applications, particularly in vehicle catalytic converters and tumor treatment, etc., is leading to the increased release of these elements into the environment. Studies have shown that, under suitable conditions, certain chemical forms of PGEs emitted from vehicles could become bioavailable.[1,2] Determination of these elements is important for understanding the chemical nature of PGEs in environmental samples and their impact on ecological and biological systems.[3–5] The metallic forms of PGEs are generally considered to be inert as regards biological reactions. On the other hand, certain PGE compounds are known to be cytotoxic and to have mutagenic and carcinogenic effects and they are among the most potent allergens and sensitizers.[3] Due to the increase in the use of Pd in place of Pt in catalytic convertors, a predominance of the former element in airborne particulate matter has been observed over the last decade.[6] This increase in the concentrations of Pd in environmental samples is of concern because, among the PGEs, Pd has the highest bio-accessibility and mobility in the environment.[7] The process of thermal neutron induced fission of fissile nuclides, e.g. 235U, 239Pu, leads to the production of a wide range of fission products in varying quantities. Palladium (Pd), rhodium (Rh) and ruthenium (Ru) are the only three PGEs formed to a significant extent during the nuclear fission process. The actual amounts of formation of these PGEs depend on the type of reactor system as well as on the burn-up of the nuclear fuel.[8,9] With the future development of a proper recovery and decontamination process, the availability of these metals is likely to increase and they can thus serve as an alternative resource to meet the increasing demand for noble metals.[10] A reliable analytical procedure for the quantification of the PGEs is, therefore, important at different stages of reprocessing. Analytical methods have been described for the determination of PGEs in synthetic and actual nuclear waste solutions.[11,12]