Abstract

A new method has been developed for the determination of platinum and palladium based on separation and preconcentration with a microcolumn packed with nanometric TiO2 immobilised on silica gel (immobilised nanometric TiO2) prior to their determination by inductively coupled plasma‐atomic emission spectrometry. The optimum experimental parameters for the preconcentration of Pt and Pd, such as the pH of the sample solution, its flow rate and volume, the type and concentration of eluent and interfering ions, have been investigated. Platinum and Pd could be quantitatively retained by immobilised nanometric TiO2 in the pH range 6–8, then eluted completely with 2.0 ml of 3% m/v thiourea in 1.0 mol l−1 HNO3. The detection limits of this method for Pt and Pd were 12 and 7. 6 ng l−1 with an enrichment factor of 100, and the relative standard deviations were 4.7% and 3.3% at the 10 ng ml−1 level. The method has been applied for the determination of Pt and Pd in geological samples with satisfactory results.

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