Determination of lead in palladium diaminodichloride and palladium diaminodinitrite by electrothermal atomisation atomic absorption spectrometry

Abstract

A method is described for the determination of lead in palladium diaminodichloride and palladium diaminodinitrite by electrothermal atomisation atomic absorption spectrometry (ETAAS). Examination of the behaviour of these Pd compounds by thermal derivative analysis in the range 20–1000 °C demonstrates that the decomposition process takes place at 356 °C for palladium diaminodichloride and at 222 °C for palladium diaminodinitrite. Identification by X-ray diffraction and infrared spectrometry confirms that the predominant component in the products, heated at these temperatures, is Pd. The results obtained suggest that satisfactory analytical performance can be achieved using ETAAS without the use of a reducing agent and calibration using the standard additions method. The accuracy of the method was confirmed by solvent extraction flame atomic absorption spectrometry with the use of ammonium pyrrolidinedithiocarbamate as the complexing agent and isobutyl methyl ketone as extractant.