Determination of palladium in various samples by atomic absorption spectrometry after preconcentration with dimethylglyoxime on silica gel

A preconcentration method based on the adsorption of palladium-dimethylglyoxime (DMG) complex on silica gel for the determination of palladium at trace levels by atomic absorption spectrometry (AAS) has been developed. The retained palladium as Pd(DMG)(2) complex was eluted with 1 mol l(-1) HCl in acetone. The effect of some analytical parameters such as pH, amount of reagent and the sample volume on the recovery of palladium was examined in synthetic solutions containing street dust matrix. The influence of some matrix ions on the recovery of palladium was investigated by using the developed method when the elements were present both individually and together. The results showed that 2500 mug ml(-1) Na+, K+, Mg2+, Al3+ and Fe3+; 5000 mug ml(-1) Ca2+; 500 mug ml(-1) Pb2+; 125 mug ml(-1) Zn2+; 50 mug ml(-1) Cu2+ and 25 mug ml(-1) Ni2+ did not interfere with the palladium signal. At the optimum conditions determined experimentally, the recovery for palladium was found to be 95.3 +/- 1.2% at the 95% confidence level. The relative standard deviation and limit of detection (3s/b) of the method were found to be 1.7% and 1.2 mug l(-1), respectively. In order to determine the adsorption behaviour of silica gel, the adsorption isotherm of palladium was studied and the binding equilibrium constant and adsorption capacity were calculated to be 0.38 1 mg(-1) and 4.06 mg g(-1), respectively. The determination of palladium in various samples was performed by using both flame AAS and graphite furnace AAS. The proposed method was successfully applied for the determination of palladium in the street dust, anode slime, rock and catalytic converter samples. (C) 2004 Published by Elsevier B.V