Qualitative and quantitative determination of radicals formed during the photocatalytic process. A) EPR spectra recorded during the illumination of rutile Au‐TiO2 in water with methanol for 20 min. Signals marked with an asterisk (★) belong to the oxidation product of DMPO, 5,5‐dimethyl‐2‐oxopyrroline‐1‐oxyl (DMPOX).12 Signals marked with triangles (▾) belong to the spin adduct .DMPO–OH, and signals marked with circles (•) belong to the spin adduct .DMPO–CH2OH from methanol.13 Reaction conditions: [Au‐TiO2]=5 g L−1, [DMPO]=30 mm, [methanol]=100 mm, RT, under illumination. B) Time course of the photocatalytic umbelliferone generation from coumarin as a specific detection method for .OH radicals. Reaction conditions: 60 mm phosphate buffer (pH 7), [Au‐TiO2]=5 g L−1, [coumarin]=0.1 mm, [methanol]=0 (⧫) or 250 mm (▪), T=30 °C, under illumination.