Abstract The chemical reactions which occur when Illinois No. 6 (hv C) and Rawhide (SBB C) coals are thermally pretreated at 100°C and when Illinois No. 6 coal is subsequently oxidized at 100°C with O 2 have been studied using in-situ FT-i.r. differende spectroscopy. Significant spectroscopic changes were seen. Vacuum drying at 100°C resulted in the decomposition of carboxylic acid species to form a variety of new carbonyl species (in Rawhide) and decarboxylated or decarbonylated coal (Illinois No. 6). Oxidation of predried Illinois No. 6 coal leads to the formation of new carbonyl species. The assumption that drying does not alter the chemical composition of coal may not be correct. Thus, overall spectroscopic (and chemical) changes observed in moderate temperature reaction studies may depend upon sample pretreatment, drying and storage. In addition, the time/temperature profile used in a reaction study may affect the overall changes observed by altering the relative contribution of the different reactions.