Micronised particles of revatropate hydrobromide were observed to agglomerate when stored in uncontrolled conditions. Dynamic vapour sorption (DVS), isothermal microcalorimetry, microscopy and particle size measurement by laser diffraction have been used to study micronised revatropate hydrobromide. The rate and extent of agglomeration were dependent on the energy of the micronisation process, the sampling point for bulk within the mill and the humidity during storage. The agglomeration was attributed to the recrystallisation of disordered regions on the particles of revatropate hydrobromide generated during micronisation. This recrystallisation was assessed qualitatively and quantitatively, compared against spray-dried amorphous material, using DVS and isothermal microcalorimetry, respectively. A correlation was established between the energy of micronisation and the level of disorder within the micronised powder. A comparison of the DVS profiles of freshly prepared and aged micronised revatropate hydrobromide suggests an increased physical stability for the aged material.