The physical and chemical properties of a hypercrosslinked Macronet polymer, MN-600, have been compared with a charcoal based activated carbon, A1100, to evaluate their performance as sorbents for trace toxic metal removal from water. The characterisation includes scanning electron micrographs (SEM), BET and Langmuir surface area measurements, Fourier transform infra red spectroscopy (FTIR) analysis, sodium capacity measurement, pH titration, direct titration and zeta potential measurements. Pore size distribution data were analysed using the density functional theory (DFT) model. These sorbents were used in mini-column experiments for the removal of copper, zinc and nickel from aqueous solutions. The sorbents were regenerated by eluting with 0.1 M hydrochloric acid solution. These studies were performed to elucidate the relationship between sorptive performance and the physical and chemical structure of these materials.