2-Acetylpyridine-4-phenyl-3-thiosemicarbazone (APPT) ligand was incorporated onto Amberlite XAD-2 resin through an azo spacer and characterized by FTIR spectroscopy, elemental analysis, TGA, and SEM analysis. The synthesized resin was used for the preconcentration of Pb(II), Zn(II), Co(II), Ni(II), Cu(II), and Cd(II) ions. The sorbed metal ions were eluted with 10 mL of 2.0 mol L-1 HCl and determined by microsample injection coupled flame atomic spectrometry (MIS-FAAS). The recoveries of studied metal ions were >= 95.1% with RSD >= 4.0% at optimum pH 8; resin amount, 300 mg; flow rates, 2.0 mL min(-1) (of eluent) and 3.0 mL min(-1) (sample solution). The limits of detection (LOD) and limits of quantifications (LOQ) of the studied metal ions were 0.11, 0.05, 0.07, 0.08, 0.09, and 0.03; and 0.37, 0.17, 0.21, 0.13, 0.31, and 0.10 mu g L-1, respectively, with a preconcentration factor of 500 for the 6 studied metal ions. The total saturation capacity of the resin was 0.36, 1.20, 1.50, 1.61, 1.07, and 0.71 mmol g(-1), respectively.