Hydrogen peroxide concentrations in the Gulf of Mexico were measured on two cruises in May and August, 1982, in a variety of locations ranging from oligotrophic oceanic stations to highly productive coastal sites. Measurements were made using a fluorescence decay technique. Depth profiles of H2O2 exhibit surface maxima of 1-2 × 10-7 mol L-1 and decreasing concentrations with depth. Peroxide concentrations decreased only slightly or were invariant with depth in the mixed layer but decreased sharply to below the limit of detection (5 × 10-9 mol L-1) in the region of the pycnocline at the base of the mixed layer. Surface concentrations were generally highest in coastal regions but did not vary by more than a factor of three among all stations studied. There was a marked diel variation in peroxide profiles, with the highest values occurring during the late afternoon, and the lowest values occurring at dawn. Diel variations were more pronounced in coastal surface waters than in oligotrophic waters. The observations are consistent with photochemical formation of H2O2 by photooxidation of dissolved organic matter. However, other formation pathways, such as biological formation or atmospheric deposition, cannot be ruled out at this point. © 1985.