On-line preconcentration procedures for the determination of Ag(I) and Pd(II) by flame atomic absorption spectrometry have been described. A new chelating resin, poly (N,N'-dipropionitrilemetha-crylamide-co-divinylbenzene-co-2-acrylamido-2-methyl-1-propane sulfonic acid) was synthesized and used as a new adsorbent material. The resin was characterized by Fourier transform infrared spectroscopy and elemental analysis. Ag(I) was adsorbed on the chelating resin at pH 5.0 and eluted with 1.0 mol L-1 HNO3. Pd(II) was retained at pH 9.5 and eluted with 1.5 mol L-1 HCl. The experimental parameters (pH, type and concentration of eluent, flow rates of sample and eluent solutions, elution time and the effect of interfering ions) for both Ag(I) and Pd(II) were investigated in detail. The detection limit for Ag(I) was 2.4 mu g L-1 and the relative standard deviation was 2.9% for 0.2 mu g mL(-1) Ag(I). The detection limit for Pd(II) was 1.7 mu g L-1 and the relative standard deviation was 2.8% for 0.3 mu g mL(-1) Pd(II). Accuracy was confirmed by analyzing a certified reference material (TMDA-70), recovery studies on real samples and comparison with electrothermal atomic absorption analysis. The proposed methods were successfully applied to the on-line determination of Ag(I) in bottled water, pharmaceutical cream and anode slime samples and Pd(II) in bottled water and catalytic converter samples. (C) 2012 Elsevier B.V. All rights reserved.