Laser Raman spectroscopy (LRS) was used to characterize the hydrated and dehydrated states of surface-supported Mo6+ on Davison 952 silica gel. Silica-supported Mo samples were prepared from MO2(eta3-C3H5)4 and (eta5-C5H5)2Mo2(CO)4. Metal loadings of 5.1-7.8 wt% Mo were studied. Crystallites of MoO3 were not observed at these high loadings. An upper limit for dispersing dehydrated, isolated Mo6+ was found at about 1 Mo atom/nm2, which corresponds to the isolated silanol density of silica.