Using modulated DSC to investigate the origin of multiple thermal transitions in frozen 10% sucrose solutions

Modulated differential scanning calorimetry (MDSC) was used to investigate the effect of annealing on multiple thermal transitions in frozen aqueous sucrose solutions. Two thermal transitions were detected from the reversing heat flow. Here, to maintain consistency with terminology used in the practice of freeze-drying 1], the higher temperature is denoted, T^′g, and the lower transition is given the symbol, T^″g. The transition at low temperature is usually believed to be a true glass transition. However, the origin of the transition at high temperature is still highly controversial. Based upon a study of 10% sucrose solutions with different cooling histories and annealing conditions, we suggest that the transition at high temperature is also a glass transition. We conclude that the lower transition is a glass transition of a phase plasticized by a higher than equilibrium amount of unfrozen water, and the higher transition, T^′g, corresponds to a glass transition in a maximally freeze-concentrated solute phase.