In order to investigate a practical application of fibrous adsorbents to heavy metal ions, amidoxime fibers, as a particular class of solid chelate agents, were prepared by hydroxylamine treatment for acrylic fibers in a recipe of neutralization. Among the important problems from plant effluents are toxic concentrations of heavy metals such as copper. Accordingly, the properties of Cu (Ⅱ) adsorption and its chelates were studied. The results obtained are as follows; The fibrous adsorbents have the property of increasing the swelling volumes by amidoximation. The adsorption of Cu (Ⅱ) ion is characterized by an endothermic reaction, which is estimated as the plus values in the enthalpy change (AH=1.30 Kcal/mol. and 3.14 Kcal/mol.). The Cu (Ⅱ) ions are adsorbed in the range of pH 3∼8 and the maximum adsorptions are occurred about pH 8. Owing to the anions (NO_3-,Cl-) of copper salts, amidoxime fibers form 1:1 and 2:1 (ligand:metal) chelating complexes with Cu (Ⅱ). The nitrate anion chelates to amide I (NH) of amidoxime groups and the chlorine anion does to nitrosyl (NO). These effects relate to the crystallization of the complex and the thermal property.