Analytical pyrolysis is a technique currently used for investigating structural features of complex macromolecular materials. However, pitfalls appear td be widespread in pyrolysis studies of humic substances, and serious limitations can be experienced during the analytical procedure due to thermal reactions and configuration of the pyrolysis units-and chromatographic systems. Pyrolysis presents inconsistencies for chemical studies, and the interpretation of the chemical structure of humic substances in light of information provided by pyrolysis data is, to say the least, hazardous. This paper examines possible solutions to some of the problems encountered in pyrolysis.