The Oxidation desulfurization (ODS) process has been developed to control sulfur content in diesel. Researchers have tested a new oxidation system on a 1,000-ppm commercial diesel sample supplied by Saudi Aramco's Rabigh refinery. Hydrogen peroxide is commonly used as an oxidizing reagent due to its relatively low price, environmental compatibility, and commercial availability. The catalytic system was evaluated for the removal of sulfur-containing compounds in diesel. The new oxidation system was then tested on a commercial diesel sample supplied by Rabigh refinery. The hydrotreated diesel of boiling ranges 250-350°C has 1,100 ppm sulfur content. A selective sulfur detector, a pulse flame photometric detector (PFPD), monitored changes in the concentration of the different sulfur compounds existing in the diesel. The sulfur concentration was successfully reduced by ODS and then by extraction to more than 92% and 97%, respectively.