Woven polyacryloamidoxime cloth was prepared from the polyacrylonitrile precursor via reaction in methanolic hydroxylamine. Preparation was controllable and reproducible and the reaction conditions were optimized with respect to the time of conversion, the concentration of NH 2 OHrHCl, and the temperature of conversion. The cloth produced had a large capacity for Cu(II) and Pb(II) of 71.2 and 450 mg g 01 (1.12 and 2.17 mmol g 01 ) respectively, and adequate physical properties suitable for rigorous use. Sorption profiles of Pb(II) and Cu(II) were similar to those of chelate ion exchange resins and fibers containing the amidoxime group. The rate of uptake of metals by the cloth was found to be dependent on the percent surface area converted to amidoxime groups, the concentration and type of metal being tested for, and the time of exposure. Anomalous kinetics of sorption for Pb(II) and Cu(II) by cloth of increasing amidoxime group content were explained by a two-part sorption mechanism. Distribution coefficients of 3.5 1 10 6 and 1.5 1 10 6 for Cu(II) and Pb(II) were observed, and the average rates of uptake for Cu(II) and Pb(II) were 600 and 200 mg g 01 day 01 (9.4 and 0.96 mmol g 01 day 01 ), respectively, from dilute solution ([Cu] Γ
5.9 mg L 01 , [Pb] Γ
2.8 mg L 01 ). Treatment of the cloth with aqueous NaOH did not improve the capacities for Pb(II) and Cu(II).