Adsorptive preconcentration for voltammetric measurements of trace levels of zirconium.

This paper describes an electrochemical stripping procedure for ultratrace measurements of zirconium, in which preconcentration is achieved by the adsorption of a zirconium-Solochrome Violet RS complex onto a hanging mercury drop electrode. Cyclic voltammetry was used to characterize the interfacial and redox behaviour. For a 10-min preconcentration time, the detection limit found was 2.3 x 10(-10)M. Optimal experimental conditions were found to be use of a stirred acetate buffer (pH 4.6) solution with Solochrome Violet RS concentration 1.5 x 10(-6)M, a preconcentration potential of -0.3 V and linear scan mode. A 60-fold enhancement of the response is obtained following 5-min preconcentration. With preconcentration for 60 sec, calibration plots for zirconium are linear for the 1.1 x 10(-8)-1.1 x 10(-7)M range. The relative standard deviation at 5.5 x 10(-8)M is 1.7%. Possible interferences by surface-active organic materials and other trace metals have been investigated. Zirconium added to a sea-water sample at the 10 ng/ml level was readily determined.