Five new polymethacrylohydroxamic acids have been reported for complexation with divalent metal ions and their plausible separations. The metal ligand stability constants (log beta(2)) of divalent metal ions were determined in 70% dioxan-water media at 35 +/- 0.1 degrees C. The order of stability constant is discussed. Their physico-chemical properties have been determined. These acids are used as resins and parameters like rate of sorption, sodium ion uptake, total ion-exchange capacities, effect of pH on distribution coefficient, break through capacities etc. were determined. The chromatographic separations for binary, ternary, quaternary and quinary systems of metal ions (Cu, Zn, Ni, Co, Fe and Pb) have been described. The method is used for the determination of metal ions in synthetic and environmental samples.