This article introduces a comparative study for the simultaneous separation and preconcentration of Fe(III) and Zn(II) traces in various water samples using three well-known ligands as chelating agents and activated carbon (AC) derived from Ramelak bark as a new bio-sorbent prior to the determination by FLame atomic absorption spectrometry. The chelating agents were 4,4'-[(4-Cyano-phenyl)methylene]bis(3-methyl-1-phenyl-1H-pyrazol-5-ol) (CMBM), diethyldithiocarbamate (DDTC) and ammonium pyrrolidine dithiocarbamate (APDC). CMBM was synthesized by a procedure reported in the literature. The newly prepared AC was characterized by Scanning Electron Microscopy (SEM) and Fourier-Transform Infrared (FTIR) Spectrometry. The analytical parameters affecting the separation efficiency of the analytes including pH, shaking time, chelating agent volume (concentration), sorbent mass, sample FLow rate and elution conditions were investigated and discussed. Common coexisting ions did not seriously interfere with the separation, showing the good selectivity of the proposed method. The calibration graph was linear in the range of 0.35-70, 0.50-80, 0.9-100, 0.55-75, 0.75-90 and 1.0-120 ng mL(-1) for Fe-CMBM, Fe-DDTC, Fe-APDC, Zn-CMBM, Zn-DDTC and Zn-APDC, respectively. Under optimized conditions, the limits of detection were 0.11, 0.13, 0.27, 0.16, 0.22 and 0.30 ng mL(-1) for Fe-CMBM, Fe-DDTC, Fe-APDC, Zn-CMBM, Zn-DDTC and Zn-APDC, respectively. The proposed method has been applied to the determination of Fe(III) and Zn(II) in different water samples with satisfactory recovery percentages. The developed method, validated with standard reference materials, was used successfully in determining the concentrations of metal ions in water samples.