Hydrogen removal from Mg-doped GaN is necessary to activate p-type conductivity, but the exact chemical process is not yet clear. We have investigated this issue by monitoring the intensity of an electron paramagnetic resonance (EPR) signal attributed to Mg through a series of isochronal and isothermal anneals between 600 and 1000 °C. Measurements made on GaN:Mg epitaxial layers deposited on SiC and annealed between 700 and 850 °C indicate that the Mg-related EPR signal increases with temperature as expected for depassivation of a Mg complex by removal of hydrogen. However, data obtained outside this temperature range suggest that additional processes may occur. For example, as-deposited films contain a signal resembling the Mg acceptor that is quenched by a 650 °C N2 anneal. Also, for all samples, N2 annealing at T>850 °C irreversibly decreases the signal thought to be due to Mg. Although the presence of the signal in the as-grown films is not fully understood, the effects observed at T>850 °C may be attributed to preferential N-desorption from Mg-N-H complexes.