DSC And X-Ray Diffraction Coupling

Abstract

A new technique, that allows simultaneous time-resolved synchrotron X-ray diffraction as a function of temperature (XRDT) and high sensitivity DSC to be carried out in the same apparatus, has been developed. Microcalorimetry and XRDT scans can be performed at any rate between 0.01 and 10°C min⁻¹ with a 0.01°C temperature resolution in the temperature range, 30–130°C and at lower cooling rates but the same heating rates in the −30–+30°C range. The use of a single and very small sample (1 to 20 μl) contained in a thin glass capillary for both measurements and simultaneous data collection prevents any temperature shift between recordings and any possible difference in the thermal histories of the samples.