A range of materials representative of carbonaceous near-Earth asteroids was subjected to stepwise heating in vacuum to investigate volatiles release and capture behavior in space. Results show that most of the mass lost during heating is predictable by well-known reactions: dehydroxylation, dehydration, and pyrolysis. Cryotrapping was shown to effectively capture the volatiles produced. These findings form a base for additional investigations, so that the trade space of potential processes for extracting volatile compounds from carbonaceous solar system bodies can be explored effectively.