Transition metal (Me = V, Fe, and Cr) incorporated into MCM-41 mesoporous molecular sieves (Si/Me = 80) have been synthesized by hydrothermal methods and were loaded with TiO2 utilizing a sol-gel technique. These materials were found (refs 22, 23) to be photoactive fur the destruction of organics with visible light. A combination of various physicochemical techniques such as N-2 physisorption, O-2 chemisorption, diffuse reflectance UV-vis (DR-UV-vis), X-ray diffraction (XRD), Raman, temperature program reduction (TPR), and X-ray photoelectron spectroscopy (XPS) were used to characterize the chemical environment of these transition metals in the prepared photocatalysts. The dispersion of transition metals as determined by O-2 chemisorption suggests that they are well dispersed inside the MCM-41 framework, but the dispersion values decreased with the loading of TiO2. This indicates that the loaded titanic promotes the transformation of incorporated metal ions into different phases. DR-UV-vis spectra of the; Me-Ti-MCM-41 materials exhibit substantial absorption of visible light in the range of 400-600 am. However, the same materials loaded with titanic show higher absorption in the UV range (250-400 am) because of the presence of titania. XRD patterns of Me-Ti-MCM-41 are similar to that of siliceous MCM-41 and demonstrate that the transition metals are atomically dispersed in the framework. The titanic loaded onto the Me-Ti-MCM-41 was of low anatase crystallinity as shown by Raman. The TPR results fur Me-Ti-MCM-41 revealed a lower number of reduction transitions than the titanic loaded Me-Ti-MCM-41. These reduction transitions depend on the nature of transition metal species in the MCM-41 framework. The Me/Ti and Me/Si surface; atomic ratios, which are determined by XPS measurements, reveal that considerable diffusion of transition metal ions to the surface occurs upon loading of titanic. The XPS line shapes, binding energies, and surface atomic ratios for Me-Ti-MCM-41 indicated one type of surface electronic level such Me-O-Si, whereas two types of surface electronic levels were found in the case of 25% TiO2/Me-Ti-MCM-41, which corresponds to Me-O-Si and Me-O-Ti. The Me/Si and Me/Ti surface atomic ratios show that the incorporated transition metals interact preferable with the loaded titanic as in the form of Me-O-Ti heterojunction instead of staying inside the framework as in the form of Me-O-Si electronic level.