A novel phosphorus-containing carbonaceous sorbent has been prepared by pyrolysis of phosphorylated phenol-formaldehyde resin. The surface properties of the material have been characterised by nitrogen adsorption-desorption isotherms and MAS NMR-P-31 spectrometry. The ion-exchange properties of the carbon were assessed by pH-titration and electrophoretic mobility measurements. Sorption studies were performed in batch and mini-column experiments and indicated high affinity towards lead(II) over copper(II), nickel(II) and cadmium(II) for solutions containing these metals (in the mg/l and mu g/l range) although the rate of sorption was relatively slow. The sorption affinity series for metal ions studied coincides with the solubility products of the corresponding metal phosphates and stability constants of pyrophosphate complexes in aqueous solutions. Elution using conventional mineral acids yields good heavy metal recovery and effective adsorbent regeneration.