The chelating resins incorporating amide linkages were synthesized in open reaction vessels (OV) by polycondensing different proportions, viz., 1 : 1, 1 : 1.3, and 1.3 : 1 of polyethyleneimine (PEI) and diethylenetriaminepentaacetic acid (DTPA), respectively, at 145–155°C, and at varying curing times (15 h and 22 h). For the proportion 1 : 1, the synthesis was performed in a closed reaction vessel (CV) as well. The resins were characterized by FTIR, elemental, and thermogravimetric analysis, apart from sarptometric surface studies. The extent of crosslinking was evaluated by swelling measurements and the chemical stability was assessed by acid and alkali treatment. The effect of the mode of heating and curing times on the extent of crosslinking and pore structure modifications were evaluated. The influence of these factors on the capacities, the kinetics, and the break through curve trends of these resins were studied using zinc and cadmium metal ions as references. The reproducibility of the resins were ascertained by assessing the extent of change in the break through curve trends of their different batches, synthesized under identical conditions. © 1993 John Wiley & Sons, Inc.