Calorimetric and spatial characterization of polymorphic transitions in caffeine using quasi-isothermal MTDSC and localized thermomechanical analysis.

We describe a novel integrated approach to the study of polymorphic transformation that includes quasi-isothermal modulated temperature differential scanning calorimetry (QI-MTDSC) and microthermal analysis (MTA), with a view to studying the thermal, kinetic and spatial characteristics of the process. Form II and I caffeine was prepared and conventional DSC and hot stage microscopy performed. The Form II to I transition at circa 413 K was associated with a change in crystal habit to needle shaped crystals.