The thermal behaviour of humic acids and their sodium salts in oxygen has been studied. The sodium humates were prepared by neutralization of humic acids or by dialysis of their pseudosolutions in sodium hydroxide. Infrared and X-ray diffraction spectra of samples taken between the dissociation steps obtained from the DTA-TG-DTG curves suggest a double mechanism. Below 500°, sodium carbonate and carbon are formed. At 600°, the dissociation of carbonate starts. The residual carbon burns at once at 770°. The extent of reaction changes with the amount of sodium initially present.