A novel poly(acryl-benzoylamidrazone-acryl-benzoylhydrazine) chelating fiber was synthesized simply from nitrilon (polyacrylonitrile fiber). The structure of the chelating fiber was verified with the help of FT-IR spectrum. The parameters influencing the efficiency of the fiber for concentrating trace amounts of Au(III) and Pd(IV) were investigated in detail. Trace Au(III) and Pd(IV) were enriched and separated from real sample solutions and detected using inductively coupled plasma atomic emission spectrometry (ICP-AES) with satisfactory results. The experiments show that the method is rapid, precise, simple and convenient to use.