Simultaneous Determination of Palladium and Platinum by On-line Enrichment and HPLC with 4-(2-Hydroxynaphthalene- 1-ylmethylene)-thiazolidine-2,5-Dithione as Pre-column Derivatization Reagent

Abstract

In this paper, a new reagent, 4-(2-hydroxy-naphthalene-1-ylmethylene)-thiazolidine-2,5-dithione (HNMTD) was synthesized. A new method for the simultaneous determination of palladium and platinum ions as metal-HNMTD chelates was developed using high performance liquid chromatography equipped with an on-line enrichment technique. Prior to chromatography the palladium and platinum ions were derivatized with HNMTD to coloured chelate complexes. The Pd-HNMTD and Pt-HNMTD complexes were then enriched on an enrichment column(ZORBAXReversed Phase StableBoundC₁₈, 4.6×10mm,1.8 μm) using a buffer solution of 0.05 mol L^–1 sodium acetate-acetic acid buffer (pH 3.8) as mobile phase.After the enrichment was completed, the retained chelates were back-flushed to the analytical column. The separation of chelates on the analytical column (ZORBAX Reversed Phase Stable Bound C₁₈, 4.6 × 50 mm, 1.8 μm) was satisfactory when 72% methanol (containing 0.05 mol L^–1 of pH 3.8 sodium acetate-acetic acid buffer salt and 0.1% of TritonX-100) was used as mobile phase. The Pt-HNMTD and Pd-HNMTD chelates were separated completely within 2 min. The detection limits (S/N = 3) for palladium and platinum were 1.2 ng L^–1 and 1.4 ng L^–1, respectively. The method was applied with good results to the determination of palladium and platinum in water and urine samples.

Keywords: Palladium, platinum, 4-(2-hydroxy-naphthalene-1-ylmethylene)-thiazolidine-2,5-dithione, high performance liquid chromatography, on-line enrichment.