The crystallisation of complex mixed oxide and metal phosphate oxidation catalysts prepared using a number of synthetic methods have been studied using in situ synchrotron radiation techniques. Some of these synthesis procedures have previously been employed to produce catalysts whilst others were new methods, making use of hydrothermal technology and zeolite precursors. For the iron phosphates catalysts studied it was observed that all of the synthetic methods employed produced a catalyst precursor having the chemical composition FePO4.2H2O. During calcination this phase transformed into the tridymite and quartz forms of FePO4 although, the material produced by hydrothermal methods was found to be the most phase pure and possess a higher surface area. A comparative study of the three catalytically active forms of bismuth molybdate revealed similar findings with two of the three phases observed (by EDXRD) to form directly from a precursor gel with an Avrami-Erofe'ev kinetic analysis of the crystallisation process suggesting that the mechanisms of formation were different for each phase. Hydrothermal methods were also used to prepare cobalt and manganese substituted aluminophosphate structures API and AEI, which were found to be efficient catalysts for the methanol to olefin reaction. However, it was also observed that during calcination to remove the structure-directing agent, that some of the cobalt and manganese in the tetrahedral framework sites underwent oxidation from 2+ to 3+ although the extent of this was found to be dependent upon both structure type and metal ion. Finally an investigation was carried out into the use of ion-exchanged zeolites as precursors for the low temperature crystallisation of the spinel structure CoA12O4. The results from this study suggested that very small spinel particles formed within the XRD amorphous collapsed zeolites although both zeolite structure type and cobalt salt were thought to have an effect on phase formation.