Simultaneous Determination of Palladium, Platinum and Rhodium by On-Line Column Enrichment and HPLC with 4-Hydroxy-1-Naphthalthiorhodanine as Pre-Column Derivatization Reagents

Abstract.

In this paper, 4-hydroxy-1-naphthalthiorhodanine (HNTR) was synthesized, and a new method for the simultaneous determination of palladium, platinum and rhodium ions as metal-HNTR chelates was developed using rapid column high-performance liquid chromatography combined with on-line enrichment. The palladium, platinum and rhodium ions were pre-column derivatized with HNTR to form colored chelates. The Pb-HNTR, Pt-HNTR and Rh-HNTR chelates could be absorbed onto the front of the enrichment column when they were injected into the injector and sent to the enrichment column [ZORBAX Stable Bound, 4.6 × 10 mm, 1.8 μm] with a buffer solution of 0.05 mol L⁻¹ sodium acetate-acetic acid (pH 4.0) as mobile phase. After enrichment, and by switching the six-ports switching valve, the retained chelates were back-flushed by mobile phase and traveling towards the analytical column. Separation of these chelates on the analytical column [ZORBAX Stable Bound, 4.6 × 50 mm, 1.8 μm] was satisfactory with 68% acetonitrile (containing 0.05 mol L⁻¹ of pH 4.0 sodium acetate-acetic acid buffer salt and 0.1% of tritonX-100) as mobile phase. Palladium, platinum and rhodium were separated completely within 2 min. The detection limits (S/N = 3) of palladium, platinum and rhodium are 1.2 ng L⁻¹, 1.5 ng L⁻¹ and 1.8 ng L⁻¹, respectively. This method was applied to the determination of palladium, platinum and rhodium in water, urine and soil samples with good results.