The major drawback of the industrial iron molybdate catalysts which is their deactivation problem has driven the study of alternative catalysts for formaldehyde production from methanol. In this paper, NO-doped beta-moO(3) was successfully synthesized from the commercial molybdic acid powder (H2MoO4) and characterized by differential thermal analysis (DTA), X-ray Diffraction (XRD), Raman spectroscopy and X-ray photoelectron spectroscopy (XPS). Results obtained from XRD and Raman spectroscopy indicated that the synthesized sample has all features of the well-known beta-moO(3) except for the presence of a new small peak. The curve-fitting of XPS spectra revealed that nitrogen-containing species may be present in the form of negatively charged nitrogen oxide in the prepared sample. Due to its metastable nature, NO-doped beta-moO(3) may be transformed into the thermally stable beta-MoO3 at temperature higher than 400 degrees C as pointed out by DTA study. However, when the reaction temperature was as low as 300 degrees C, the catalyst was stable for partial methanol oxidation with no significant change in activity during 30 h of catalytic study. Methanol conversion and formaldehyde selectivity were maintained at about 98% and 99%, respectively. (C) 2016 Elsevier B.V. All rights reserved.