A new chelating ion exchanger, zirconium(IV) diethanolamine has been synthesized, characterized and studied for sorption of eight heavy metal ions at different pH (1-6). Sorption capacity of zirconium (IV)-diethanolamine sample (ZDEA(5)) for Cu(2+) and Hg(2+) was found to be 1.2 and 0.7 mmol g(-1), respectively. The effect of pH on sorption revealed that capacity generally decreases with decrease in pH and optimum pH for maximum sorption is 6. The distribution coefficients of metal ions on ZDEA(5) as a function of pH have been studied. Separations of Hg(2+) from its mixture with Zn(2+), Cd(2+), Ni(2+), Fe(3+) and Cu(2+) from its mixture with Fe(3+), Ni(2+) and Zn(2+) have been achieved quantitatively on a mini-column of ZDEA(5). On the basis of high selectivity and good sorption in acidic aqueous solutions a mini-column of ZDEA(5) has also been tested for recovery of Hg(2+) from dilute solutions.