This paper summarises some applications of advanced thermal techniques for the characterisation and preparation of catalysts using different sample controlled thermal analysis (SCTA) methods. The techniques are applied to temperature programmed decomposition (calcination), oxidation, reduction, dehydration, desorption and reaction. SCTA methods can produce significant enhancements in the resolution of complex reactions, provide a detailed insight into the energetics of surface and bulk processes and, when applied to catalyst preparation, give improvements in the pore structure and uniformity of the resulting materials. The advantages and limitations of SCTA methods, in which the sample temperature or concentration of reactant gas is altered as some function of the rate of a thermally induced physico-chemical process, are discussed.