X-ray photoelectron spectroscopy (XPS or ESCA) measurements were perfo
rmed on a photoreduced Mo allyl-based Mo/SiO2 catalyst (1.7 wt % Mo).
Photoreduction was carried out in CO at room temperature for increasin
g lengths of time. Factor analysis, deconvolution, and curve fitting w
ere used to determine the number and positions of components present i
n the series of XPS Mo 3d spectra obtained for the oxidic and photored
uced Mo/SiO2 catalyst. The results indicated the formation of a single
oxidation state Mo+ (Mo 3d(5/2) binding energy at 232.1 eV) after 2 h
of photoreduction and the appearance of Mo4+ as in MoO2 (Mo 3d(5/2) b
inding energy at 230.2 eV) with continued photoreduction. Average oxid
ation state studies indicated that the species designated as Mo-x+ sho
uld also be assigned to Mo4+ but in an environment different than that
of MoO2.