Abstract
A rapid and sensitive method for the determination of trace amounts of nickel has been developed, in which a volatile nickel chelate is analysedby gas-liquid chromatography. The method involves extraction of the aqueous solution of nickel at pH 4.5–5.0 with a solution of monothiotrifluoroacetylacetone in n-hexane, the use of a single extraction giving recoveries in excess of 90%. The extract is washed with sodium hydroxide solution (0.01 M) to destroy residual chelating agent, and the bis(monothiotrifluoroacetylacetonato)nickel(II) is determined by gas chromatography on a 4-ft. teflon column packed with 5% silicone gum rubber (E350) on “Universal B” support. The extreme sensitivity of the electron capture detector enables 5·10 −11 g of nickel to be detected, while nickel concentrations down to 0.1 μg ml −1 have been determined in routine analyses. The effect of diverse metal ions is examined; the most significant interference, resulting from the presence of copper(II), is easily eliminated by preliminary treatment of the solution with hydrogen sulphide. The new method has been applied to the determination of nickel at the percentage level in an alloy, and at trace levels in tea and fat samples. The results show good agreement with independent analyses for the samples.
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