This thesis is an investigation into the properties of heterogeneous metal catalysts prepared by wet impregnation, solid-solid wetting and Metal Oxide Vapour Synthesis (MOVS) methodologies. Recent studies indicated that MOVS catalysts were more active relative to the standard catalysts prepared. All catalysts were characterised by isopropanol decomposition, a probe reaction to determine the acid/base properties of catalysts. Surface species on the catalytic supports were determined by FT-Raman spectroscopy, while redox properties were determined by methanol partial oxidation studies. Observations by FT-Raman and the probe reactions lead to the conclusion that by isolating the MOVS species as a precipitate, β-MoO\sb3 is produced rather than a solid containing dual dioxo dimolybdenum species proposed to be present in other MOVS studies. However, the existence of these dual dioxo dimolybdenum species cannot be precluded since the catalysts tested using the precipitate proved to have different acid/base activities.