High surface area tungsten oxynitride has been prepared by the tempera
ture programmed reaction (TPR) of WO3 with NH3. All samples were chara
cterized by x-ray diffraction (XRD), nitrogen physisorption, CO chemis
orption, and elemental analysis. Samples were prepared at different he
ating rates (beta), and a Redhead analysis yielded an activation energ
y for nitridation of 109 kJ mol(-1). A heating rate of 0.016 K s(-1) g
ave optimal synthesis conditions. Solid state intermediates were studi
ed by interrupting the temperature program at various stages. No disti
nct suboxide phases were found using XRD. The nitridation step was det
ermined to be a continuous transformation from oxide to oxynitride. Su
rface area, CO uptake, and nitrogen weight % were all found to increas
e as the reaction progressed. Reactivity experiments showed reasonable
hydrodeoxygenation (HDO) and hydrodenitrogenation (HDN) activity, but
little hydrogenation (HYD) or hydrodesulfurization (HDS) activity.