In situ synchrotron tomography is a unique technique to study 3D microstructure evolution during solidification due to the high brilliance of the beam and the short acquisition time of the detector systems. In this work, in situ synchrotron tomographic observations were performed during the solidification of Mg–5Nd–5Zn (wt%) alloy with a cooling rate of 5, °C/min. The experiment was performed at the TOMCAT beamline of the Swiss Light Source (Paul Scherrer Institute (PSI), Villigen, Switzerland). The sample was melted using a laser-based heating system and then cooled until completely solidified. 3D tomograms were acquired during solidification. The microstructural analysis starts after the coherency point until the end of solidification. A differential thermal analysis (DTA) experiment was performed to estimate the liquidus and solidus temperature of the alloy. These values were used to correct the measured temperature from the in situ solidification experiment. Different microstructural parameters such as the volume fractions of the phases, i.e. α-Mg dendrites, interdendritics and pores, as well as the interconnectivity and skeletonization results are discussed.