Infrared emission spectroscopy has been used to study the dehydroxylation behavior over the temperature range from 200 to 750°C of three major Al-minerals in bauxite: gibbsite (synthetic and natural), boehmite (synthetic and natural) and diaspore. A good agreement is found with the thermal analysis and differential thermal analysis curves of these minerals. Loss in intensity of especially the hydroxyl-stretching modes of gibbsite, boehmite and diaspore as function of temperature correspond well with the observed changes in the TGA/DTA patterns. The DTA pattern of gibbsite clearly indicates the formation of boehmite as an intermediate shown by a endotherm around 500°C. Dehydroxylation of gibbsite is followed by a loss of intensity of the 3620 and 3351 cm−1 OH-stretching bands and the corresponding deformation band around 1024 cm−1. Dehydroxylation starts around 220°C and is complete around 350°C. Similar observations were made for boehmite and diaspore. For boehmite dehydroxylation was observed to commence around 250°C and could be followed by especially the loss in intensity of the bands around 3319 and 3129 cm−1. The DTA pattern of diaspore is more complex with overlapping endotherms around 622 and 650°C. The dehydroxylation can be followed by the decrease in intensity of the OH-stretching bands around 3667, 3215 and 2972 cm−1. Above 550°C only a single band is observed that disappears after heating above 600°C corresponding to the two endotherms around 622 and 650°C in the DTA.