On-line preconcentration, ion chromatographic separation and spectrophotometric determination of palladium at trace level

A new method for the determination of Pd by ion chromatography and spectrophotometric detection has been developed. The technique is based on the separation of palladium as PdCl42- by anion exchange and on the detection, at a wavelength of 407 nm. of metal as PdI42- after a post-column reaction with KI. The column used was an IonPac AS4 with HCl and HClO4 eluents. The eluent concentration and composition of post-column reagent were optimised in order to obtain the best separation and sensitivity for Pd. In order to reduce the detection limit, an on-line preconcentration step, has been optimised. The method, as developed, was suitable for palladium determination within a 300 ng/1 D.L. value. The method applied to a BCR reference material (CRM 277, estuarine sediment) gave satisfactory results in agreement with the certified value within a D.L. value of 1.3 mug/1 for the real sample. (C) 2003 Elsevier B.V. All rights reserved.