Coupling of time-resolved synchrotron X-ray diffraction
at both small and wide angles with differential scanning calorimetry is a
new technique that allows simultaneous characterization of thermal and structural
properties of a sample. The apparatus, called Microcalix, works between –30
and +230C at scanning rates comprised between 0.01 and 20C min–1
with a high sensitivity in both measurements using a single sample of small
volume (from about 1 to 20 μL). The last version of the instrument is
designed for laboratory bench and conventional source but preferably with
rotating anode or multilayered mirrors. Measurements under low pressure or
under shear as well as recordings of isothermal evolution are also possible.
The example of the study of polymorphism of a monounsaturated triglyceride
(PPO) will be presented as an application.