scholarly journals Visualizing the three-step freezing process and three-phase reaction not predicted by the (NH4) 2SO4/H2O phase diagram

Author(s):  
Anatoli Bogdan

According to the conventional phase diagrams, aqueous solutions freeze at the liquidus and are frozen/solid below the eutectic solidus. Herein, using differential scanning calorimetry (DSC) and optical cryo-microscopy (OC-M), we demonstrate that hy-poeutectic, eutectic 40 wt% (NH4)2SO4 and hypereutectic (NH4)2SO4/H2O remain liquid well below the eutectic solidus before freezing in three steps: fast-slow-fast. The first fast freezing produces a ramified ice microstructure (IM) and freeze-concentrated solution (FCS) containing up to ~70 wt% (NH4)2SO4. As temperature decreases further, the slow freezing of FCS precedes its fast freezing, which produces a striped IM and (NH4)2SO4 microcrystals. Videos recorded upon warming of frozen (NH4)2SO4/H2O reveal a new three-phase reaction, which is the recrystallization of ice and (NH4)2SO4 microcrystals into the lamellar eutectic ice-(NH4)2SO4 superlattice. This work demonstrates limitations of the (NH4)2SO4/H2O phase diagram and pro-poses an effective strategy for studying other deeply supercooled solutions whose behavior is not predicted by the phase dia-gram.

1995 ◽  
Vol 382 ◽  
Author(s):  
T.P. Weihs ◽  
T.W. Barbee ◽  
M.A. Wall

ABSTRACTThe exothermic, solid state reaction of Al and Zr has been studied in thick AL/Zr multilayers using Differential Scanning Calorimetry and X-ray diffraction. The multilayersamples were magnetron sputter deposited into highly textured alternate layers of Al and Zr with nominal composition A13Zr. The samples used in this study were 47μm thick with a 427Å period. When samples were isochronally scanned from 25º to 725ºC, a large exotherm at ˜350ºC was followed by one or two smaller exotherms at ˜650ºC. The first exotherm is dominated by a diffusionbased reaction of Al and Zr that produces two phases in isochronal scans: amorphous AI-Zrand cubic A13Zr, and two additional phases in isothermal anneals: A12Zr and tetragonal AI3Zr. The exothermic heat from this multi-phase reaction is measured using isochronal scans and isothermal anneals, and the heat flow is analyzed using a l-D diffusion based model. An average activation energy and a diffusion constant are determined. In the isothermal scans, the total exothermic heat increases linearly with √ime, and layer thicknesses vary linearly with heat.


1996 ◽  
Vol 274 ◽  
pp. 231-242 ◽  
Author(s):  
H.E. Gallis ◽  
F. Bougrioua ◽  
H.A.J. Oonk ◽  
P.J. van Ekeren ◽  
J.C. van Miltenburg

2015 ◽  
Vol 39 (3) ◽  
pp. 1938-1942 ◽  
Author(s):  
Yohann Corvis ◽  
Marie-Claude Menet ◽  
Philippe Espeau

The exact solid–liquid equilibrium between ascorbic acid and acetaminophen was established combining high performance liquid chromatography and differential scanning calorimetry.


2012 ◽  
Vol 10 (5) ◽  
pp. 1584-1589 ◽  
Author(s):  
Viorica Meltzer ◽  
Elena Pincu

AbstractThe solid — liquid phase equilibria for binary mixture of citric acid with tartaric acid were measured using differential scanning calorimetry. The phase diagram showed the existence a simple eutectic behavior. The thermal properties of this system as heat of mixing, entropy of fusion and excess thermodynamic functions were computed using enthalpy of fusion values. The composition of eutectic was determined using a Tammann diagram.


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