We describe a new method of solid-state analysis of mechanochemical reactions using T1-T2* relaxation correlation plots. A simple saturation recovery sequence, with full FID data collected, was employed to acquire T1-T2* data from the solid-like samples. A short instrument deadtime was essential to capturing the solid-like signal. Zn-MOF-74 and ZIF-8 were mechanochemically synthesised in a ball mill and monitored using T1-T2* correlation maps.