Adsorption processes are frequently applied to separate traces of hazardous and toxic substances from gas streams. Hence, knowledge of sorption characteristics of these substances on standard adsorbents is essential. Sorption of hexanal and acetaldehyde from a nitrogen gas stream in trace concentrations on activated carbon and ordered mesoporous carbon-based adsorbents (CMK) is studied. A magnetic suspension balance and an attached gaschromatograph-mass spectrometer were used to analyze the sorption process both gravimetrically and spectrometrically. Both types of adsorbents show a higher capacity for hexanal than acetaldehyde. The activated carbon exhibits considerable differences in regard to desorption of hexanal compared to the mesoporous CMK.