A comprehensive DTA study is reported of eight nitro-phenols and eight amino-phenols and of the corresponding p-phenylazobenzoylchloride, p-nitrobenzoylchloride and 3,5dinitrobenzoylchloride derivatives, prepared 'in situ' by heating intimate mixtures of phenol and acid chloride in a DTA system. The thermal analysis data and, in particular, the derivative formation temperatures, are interpreted in terms of the electronic and steric effects associated with the ring substituents of the phenol and acid chloride and the extent of interand intramolecular hydrogen bonding existing in these systems. These DTA data collectively, provide a comprehensive data base for the identification and characterisation of these phenols by DTA.