Journal
TURKISH JOURNAL OF CHEMISTRY
Volume 37, Issue 5, Pages 746-755Publisher
Tubitak Scientific & Technological Research Council Turkey
DOI: 10.3906/kim-1212-23
Keywords
Acetylacetone; palladium; preconcentration/separation and determination; solidified floating organic drop microextraction; ultrasound-assisted emulsification; flow injection-flame atomic absorption spectrometry (FI-FAAS)
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The ultrasound-assisted emulsification-solidified floating organic drop microextraction (USAE-SFODME) methodology was combined with flow injection-lame atomic absorption spectrometry (FI-FAAS) for the separation/preconcentration and determination of palladium at ultratrace level. In this method, the palladium ion in the aqueous solution was complexed with acetylacetone (6 x 10(-3) mol L-1) in the pH range of 1-7 and was extracted into 40 mu L of 1-undecanol, which was sonically dispersed in the aqueous phase. The vial was then centrifuged and cooled in an ice bath for 5 min. The solidi fi ed extract was melted and diluted to 100 mu L with a solution of hydrochloric (1 mol L-1) acid in ethanol, and the concentration of palladium was determined by FI-FAAS. Under the optimum conditions, an enhancement factor of 55 and a good relative standard deviation of +/- 2.1% at 40 mu g L-1 were obtained (n = 7). The proposed method was successfully applied to the determination of palladium in different types of water samples. Accuracy was assessed through recovery experiments, independent analysis by furnace atomic absorption spectrometry, and analysis of a certified reference ore by the proposed method.
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