Gas release behavior from aluminum and Al 7075 alloy powders during heating in argon was investigated by in-situ gas chromatography. Water vapor, hydrogen, carbon mono-oxide were detected as individual evolution spectra against heating temperature and time. The mechanisms of water and hydrogen evolutions were studied in detail for the determination of effective degassing condition. The adsorbed water and aluminum hydrate on the particle surfaces were considered to be the sources for the released water. Hydrogen peaks were formed from released gases through the reaction of aluminum and magnesium with adsorbed and hydrated water, and from liberated hydrogen that would have been excessively occluded during atomization. For the alloy powder magnesium was found to lower the hydrogen evolution temperature to enhance overall hydrogen release.