Proteus software v6

Thermogravimetry–Differential Scanning Calorimetry (TGA-DSC) analyses were performed on a TGA-DSC STA449C Netzsch. Dry samples of ca. 10 mg were weighted in 25 µL aluminum pans equipped with pierced lids. A heating rate of 1 °C/min up to 10 °C/min was applied between 20 and 260 °C under a helium atmosphere. Data treatment was performed by using Netzsch Proteus^® software v6.1. The chemical nature of escaping gases during heating was identified by using a Netzsch QMS 403 C mass spectrometer coupled with the 449C TGA/DSC apparatus.

DSC analyses were performed using a DSC 214 Polyma (Netzsch). Samples were weighed in 25 µL aluminum pans and submitted to a heating rate of 5 °C/min under a dry nitrogen atmosphere. Data treatment was performed by using Netzsch Proteus^® software v6.1.
As far as the construction of binary phase diagrams is concerned, the onset temperature of the observed peaks was considered for the melting and solid–solid transition of the pure compounds and for solvus inferior, solidus and invariant transitions of binary mixtures. For the liquidus, the peak value was considered.
The various DMU–water mixed samples were analyzed by DSC in the temperature range [−50–80 °C] with a heating rate of 5 °C/min.
Crucibles containing recrystallized DMU were placed in a desiccator at 20 °C with a saturated salt solution of sodium chloride in order to control the relative humidity (75% at 20 °C) due to its deliquescent character [26 (link)]. DMU samples were then enriched in water. The percentage of water absorbed in each powder sample was determined by weighing accurately the crucible before and after storage in the desiccator. Furthermore, after this conditioning, crucibles were hermetically sealed with lids in order to keep the amount of water constant all along DSC analyses. The latter were started immediately after sample preparation.