Porous poly(methacrylic-co-triethyleneglycol dimethacrylate) (MAA-SG) was prepared by suspension polymerization using benzoyl peroxide as an initiator, poly(vinyl alcohol) as a protective colloid, and n-hexane as a porogenic agent. The prepared polymer was base hydrolysed using hydroxyl amine and sodium methoxide into the corresponding polyhydroxamic acid (HYOX). The metal binding behavior of polyhydroxamic acid with various metal ions, the effect of pH on the metal ion capturing, and the selectivity of the resin towards the different metal ions were also examined by means of atomic absorption spectrophotometer. The thermal stability of the prepared base-hydrolysed polymer and the metal polymer complex was examined by thermal gravimetric analysis (TGA) and differential scanning calorimeter (DSC). The prepared porous polymer methacrylic-co-triethyleneglycol dimethacrylate and its different modulated forms were characterized by means of FTIR specroscopy and scanning electron microscope. The hydroxamic acid content was also examined by elemental analysis.