An ICP-OES method using a new poly(acrylphenylamidrazone-phenylhydrazide) chelating fiber to enrich and separate trace Au(III) and Ru(III) ions from solution samples is established. The results show that 50-500 ng/mL of Au or Ru ions can be enriched quantitatively by 0.1 g of the fiber at pH 4, with recoveries > 96%. The ions can be desorbed quantitatively with 10 mL of 4 M HCl and 3.0% CS(NH2)(2) solution from the fiber column, with recoveries > 97%, and 200-1000-fold excesses of Cu(II), Zn(II), Ca(II), Mg(II), Mn(II), Cr(III), Fe(III), Ba(II), and AI(III) caused little interference in the determination of these ions by ICP-OES. The chelating fiber can be reused eight times, and the recoveries are all > 95%. The relative standard deviations for enrichment and determination of 50 ng/mL of Au and Ru are in the range 1.8-1.9% (1.9% for Au and 1.8% for Ru). The recoveries of trace Au and Ru ions added to real waste water and alloy samples are 96-98%. The concentration of each ion found in the alloy samples was in good agreement with that provided by the plant.