Differential scanning calorimetry amorphous aqueous solutions

Titanium sulfate supported on zirconia catalysts were prepared by drying of powdered Zr(OH)4 with titanium sulfate aqueous solution followed by calcining in air at high temperature. The characterization of prepared catalysts was performed using Fourier transform infrared (FTIR), X-ray diffraction (XRD), differential scanning calorimetry (DSC), and by the measurement of surface area. The addition of titanium sulfate to zirconia shifted the phase transition of ZrOa from amorphous to tetragonal to higher temperature because of the interaction between titanium sulfate and zirconia. The catalytic activities for both reactions, 2-propanol dehydration and cumene dealkylation were correlated with the acidity of catalysts measured by ammonia chemisorption method. 

After a multicomponent aqueous solution has been freeze-concentrated to the limit and the ice has been sublimed, any residual unfrozen water must be removed from the remaining solid solution by diffusion, desorption and evaporation (transfer to the condenser). This process is termed secondary drying . For an amorphous preparation, the amount of unfrozen water remaining after the removal of ice may be typically 20-30% w/w, but much higher values, even >50% w/w, have been found in some formulations. Attempts are on record to measure the amount of water that remains in the freeze-concentrated solution phase at 7, mainly by differential scanning calorimetry but such... 

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