We report here the synthesis and characterization of twonew classes of chelating fibers, namely, (1) polymercaptopropylsilsesquioxane (PMPS) and (2) copper(II)ferrocyanide complexed with poly[1-(2-aminoethyl)-3-aminopropyl]silsesquioxane (Cu-FC-PAEAPS) fibers. Thesefibers were evaluated for selective removal of traceamount of mercury and cesium ions respectively in thepresence of competing metal ions from water. The PMPSand Cu-FC-PAEAPS fibers were prepared by coatingtheir corresponding soluble prepolymers, which are derivedfrom mercaptopropyltrimethoxysilane and [1-(2-aminoethyl)-3-aminopropyl]trimethoxysilane monomers, respectively,on a glass fiber substrate, followed by a cross-linking stepat 120
C. The fibers were characterized through infraredspectroscopy, scanning electron microscopy (SEM),and thermogravimetric analysis (TGA). These novel materialsare extremely efficient in removing low concentrationsof mercury and cesium ions from water in the presenceof high concentrations of sodium or potassium ions. Theywere shown to remove trace mercury and cesiumcontaminants effectively to well below parts per billionconcentrations under a variety of conditions.