AbstractIn situ synchrotron diffraction experiments were performed during Differential Scanning Calorimetry (DSC) of AS31, AS33 and AS35 alloys. The samples were encapsulated in stainless steel crucibles during the measurement using an empty crucible as the reference. The samples were heated up to 680°C, melted and solidified in the beginning of the experiment in order to fill the crucible. This short cycle was followed by three subsequent cycles between 400°C and 680°C with 5, 10 and 20 K/min heating and cooling rates with 5 min of holding time in the molten state. The diffraction patterns were recorded every 6 s during the DSC program by a Perkin-Elmer XRD 1622 Flatpanel detector including an acquisition time of 3 s and the collection of reference images. The endothermic and exothermic peaks are in correlation with the dissolution and formation of new diffraction patterns, respectively. During cooling from the liquid state, first, α-Mg dendrites solidify, followed by the formation of Mg2Si and Mg17Al12 intermetallics. The results are correlated with those obtained by thermodynamic simulations performed with the software Pandat.