Journal Name:
Fresenius' Journal of Analytical Chemistry
Volume:
348
Issue:
11
Pages From:
730
To:
735
Date:
Tuesday, November 1, 1994
Abstract:
An extremely sensitive stripping voltammetric procedure for low level measurements of platinum (II, IV) or ruthenium (III, IV) is reported. The method is based on the interfacial accumulation of the platinum (II) or ruthenium (III)-1-(2-pyridylazo)-2-naphthol complex on the surface of a hanging mercury drop electrode, followed by the reduction of the adsorbed complex during the cathodic scan. The peak potential was found to be −0.8 V vs. Ag/AgCl electrode and the reduction current of the adsorbed complex ions of platinum (II) or ruthenium (III) was measured by differential pulse cathodic stripping voltammetry. The optimum experimental conditions were: 1.5×10−7 mol/l of 1-(2-pyridylazo)-2-naphthol solution of pH 9.3, preconcentration potential of −0.2 V, accumulation time of 3 min and pulse amplitude of 50 mV with 4 mV s^−1 scan rate in the presence of ethanol-water (30% v/v) — sodium sulphate (0.5 mol/l). Linear response up to 6.4 × 10^−8 and 5.1 × 10^−8 mol/l and a relative standard deviation (at 1.2×10^−8 mol/l) of 2.4 and 1.6% (n=5) for platinum (II) and ruthenium (III) respectively were obtained. The detection limits of platinum and ruthenium were 3.2×10^−10 and 4.1×10^−10 mol/l, respectively. The electronic spectra of the Pt(II) — PAN and Ru(III) — PAN complexes were measured at pH 9.3 and the stoichiometric ratios of the complexes formed were obtained by the molar ratio method. The effects of some interfering ions on the proposed procedure were critically investigated. The method was found suitable for the sub-microdetermination of ruthenium (IV) and platinum (IV) after their reduction to ruthenium (III) and platinum (II) with sulphur dioxide in acid media. The applicability of the method for the analysis of binary mixtures of ruthenium (III) and (IV) or platinum (II) and (IV) has also been carried out successfully. The method is simple, rapid, precise, and promising for the determination of the tested metal ions at micro-molar concentration level.
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