Currently, there is a significant interest in magnesium (Mg) alloys for structural and functional applications. Mg alloys are lightweight materials (1.7–2.0 g/cm³), whose density is significantly lesser than that of titanium alloys and stainless steels. Furthermore, from the perspective of biomedical devices, they are biodegradable, bioresorbable and biocompatible. The objective of this work is to investigate the transition from grain boundary precipitation behaviour in the as-cast alloy to nanoscale precipitation during triaxial forging, with particular emphasis on exploring the application of small-angle X-ray scattering technique to investigate nanoscale precipitation and complement with the conventional approach of X-ray diffraction and electron microscopy.