Thermal behaviour of Hofmann-type complexes of di- and triethanolamine with cobalt, nickel, copper and cadmium was studied in dynamic nitrogen atmosphere by DTA, DTG and TG techniques. The first decomposition stage corresponds to dehydration. Kinetic analysis of dehydration data indicates that dehydration follows a low energetic process. Subsequently, release of di- or triethanolamine takes place to form bimetallic cyanides as intermediates and the final decomposition stage is the decomposition of cyanide to yield the respective metals.