Differences were studied in humic (HA) and fulvic acid (FA) extracted from soils and streams in South Georgia by the Amberlite XAD‐8 resin and conventional NaOH method. Characterization analysis was performed by liquid13C NMR, infrared (IR) spectroscopy, scanning electron microscopy (SEM), and chemical analysis. The NMR spectra indicated that the resin method yielded black water HA and FA with spectroscopic, chemical and elemental characteristics different from those isolated by the conventional NaOH method. Humic acids from both the resin and conventional NaOH methods were composed of aliphatic, aromatics and carboxyl groups, but the “resin”; HA contained more aliphatic groups. These differences were also noticed between the FA fractions obtained by the two methods. The differences corresponded to differences in IR spectra. The IR spectrum of “resin”; FA exhibited only a weak shoulder at 1625/cm for the COO”; stretching vibration, in contrast to that of FA isolated by the conventional NaOH procedure. Apparently, the high aliphatic‐CH3group content has blocked the vibration above, as evidenced by methylation of HA. Fulvic acid extracted by the resin method was also higher in total acidity, but considerably lower in N content than FA obtained by the conventional NaOH method. Both methods yielded black water FA which was less aromatic in nature than black water HA, or soil FA.