Dithizone, a selective and sensitive reagent for mercury, was anchored on cross-linked poly(vinyl pyridine) and was used for the preconcentration of nanogram levels of mercury. The polymeric support was characterised for the extent of coupled dithizone and thermal properties. The support was used in batch and column experiments for the preconcentration of mercury. Various conditions such as pH, temperature, flow rate and column parameters were optimised for the maximum extent of mercury loading. Figures exceeding 140 mg/g support were achieved at optimised conditions. Mixture of 0.2 M nitric acid and 2.0% ammonium nitrate in 1 : 1 proportion elutes mercury quantitatively. Separation of mercury from binary and ternary mixtures of mercury, palladium, zinc and cadmium was achieved without any cross-contamination.