In the present study, the combined oxidation–emulsification was used to desulfurize diesel fuel with a hydrogen peroxide–acetic acid oxidation system. A full 20 central composite design response surface method was employed to study the effect of 5-20% oxidant range, 40-100ᵒC temperature range and 20-90 min time. A 0.781% sulfur content was obtained at 12.5 wt% oxidant ratio, 65ᵒC temperature 60 min via the oxidation process. The effect of emulsification desulfurization on oxidized diesel fuel was investigated using five surfactants: cetyltrimethylammonium chloride (cationic), nonylphenol ethoxylates (nonionic), alkylbenzene sulfonate (anionic), tween 80 (nonionic), and 1-hyroxy-2-(trimethylammonio) ethane-1-sulfonate (Amphoteric). A 0.598% sulfur content was obtained using alkylbenzene sulfonate. The desulfurize diesel fuel was charactizied using GC-MASS, IREX, and FTIR. The results indicated that the combined oxidation–emulsification process may be used to desulfurize diesel.