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Investigation of the complex thermal behavior of fats

Combined DSC and X-ray diffraction techniques

Journal of Thermal Analysis and Calorimetry
Authors: G. Keller, F. Lavigne, C. Loisel, M. Ollivon, and C. Bourgaux

The thermal behavior of three ural fats (displaying very different composition), cocoa butter (CB)2, lard, and a stearin obtained from anhydrous milk-fat (AMF) fractionation, were studied by both DSC and X-ray diffraction as a function of temperature (XRDT). To perform temperature explorations between −30‡C and +80‡C, at rates identical to those used for DSC and ranging from 0.1 K min−1 to 10 K min−1, a new set of X-ray sample-holders, temperature-controlled by Peltier effect, has been developed. It is shown that the three more stable polymorphic forms of CB were easily characterized by either X-ray diffraction or DSC, and existence of two Β-3L forms was confirmed. On the contrary, the more complex polymorphism of lard and AMF required combined examination by DSC and XRDT and the brightness of the synchrotron source for studies at the highest heating rates. Quantitative analysis of the long spacings of XRDT recordings is invaluable for interpretation of thermal events. For instance, it was found that the simultaneous formation of two polymorphic forms, of apparent long spacing of 34 and 42 å, at the onset of lard crystallization might explain the difficulty of its fractionation.

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Journal of Thermal Analysis and Calorimetry
Authors: M. Ollivon, G. Keller, C. Bourgaux, D. Kalnin, P. Villeneuve, and P. Lesieur


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.

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