Temperature-programmed diffuse reflectance infrared Fourier transform
spectroscopy (TPDRIFTS) is proposed to follow in situ temperature-prog
rammed reduction (TPR) and temperature-programmed desorption (TPD) exp
eriments of catalytic systems, as a method for observing relationships
between the surface structure and the reducibility of the catalyst un
der the actual reaction conditions. TPDRIFTS studies of desorption and
reduction of a conv entional V2O5TiO2 catalyst have been carried out,
showing the presence in both processes of four stages. Both desorptio
n and reduction experiments result in similar DRIFTS spectra for tempe
ratures below 400 degrees C, accounting for two processes: (1) water d
esorption and (2) condensation of highly dispersed vanadium species in
between V2O5 islands on the anatase surface. V2O5 reduction by H-2 ta
kes place between 400 and 680 degrees C, being characterized by elimin
ation of the first-overtone bands of V=O groups. DRIFTS is shown to be
a very powerful tool to characterize both hydrogen-consuming and nonc
onsuming processes such as O- migration above 725 degrees C (stage IV)
. Relationships between the area of V=O overtones bands obtained by TP
DRIFTS and the oxidation state of vanadium are proposed as a method to
estimate this parameter under actual reaction conditions.