Determination of palladium by atomic-absorption spectrophotometry after adsorption of its acenaphthenequinone dioxime complex on microcrystalline naphthalene

Abstract

A sensitive procedure for the determination of trace amounts of palladium by enrichment of its acenaphthenequinone dioxime complex on microcrystalline naphthalene is described. The complex adsorbs readily on the naphthalene surfae formed in situ in the pH range 1.5–5.1 after vigorous shaking for a few seconds. The naphthalene-sorbed palladium complex is separated by filtration and dissolved in butylamine-dimethylformamide solution. It is then quantified by flame atomic-absorption spectrophotometry using an air-acetylene flame at 247.6 nm. Beer's law is obeyed for 4–90 µg of palladium in the final 10 ml of butylamine-dimethylformamide solution. The sensitivity for 1% absorption is 0.16 µg ml^–1. For ten replicate determinations of 60 µg of palladium the relative standard deviation does not exceed 1.27%. The interferences due to diverse cations and anions have been determined and the use of the procedure has been demonstrated for the determination of palladium in some synthetic alloy samples.