Nuclear magnetic resonance (NMR) is used to non-destructively measure the moisture and dehydration profiles in gypsum during one sided heating to temperatures of 400 degrees C reflecting the conditions during fire. The temperature and moisture profiles are recorded simultaneously. The gypsum used in the experiments was extensively characterised using TGA, DSC, MIP, and NMR. The influence of the initial moisture content on the drying and dehydration processes was tested by varying the moisture content of the samples: capillary saturated, 50% RH, and 0% RH. By calibrating the NMR signal with moisture content we have shown that it is possible to not only measure free or absorbed water with NMR, but also measure the degree of hydration of the gypsum. Furthermore, by comparing the NMR signal decays it is possible to distinguish between these two water populations. The measured water profiles reveal that during one sided heating of a gypsum sample the dehydration inside is taking place in a two-step reaction. Furthermore, the profiles indicate that the vapour produce by the dehydration reactions condensates and thereby increases the local moisture content. The condensated water forms a so-called moisture peak behind the dehydration front. To our knowledge the measurements described in this article are the first quantitative in-situ evidence for the existence of two dehydration fronts in gypsum during one sided heating. Furthermore, the built up of a moisture peak in gypsum behind the dehydration front has not been reported in the literature to our knowledge. The NMR heating experiments presented in this paper can be used to evaluate and validate hygro-thermal models in the field of fire research on building materials. (C) 2011 Elsevier Ltd. All rights reserved.