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Abstract  

Crystallization and glass-transition phenomena were studied for amorphous chlorobenzene (CB)/toluene (TL) binary systems as the function of composition. Samples were prepared by vapor-deposition onto cold substrates, and their structural changes due to temperature elevation were monitored with Raman scattering and light transmission. It was found that the crystallization temperature (T c) of CB-rich amorphous samples increases as the TL concentration is increased. This is similar to the linear dependence of glass-transition temperatures (T g) of many organic compounds on the concentration of additive. Also found was that T c of TL-rich supercooled-liquids decrease as the CB concentration is increased. Issues related to the two kinds of T c are discussed briefly.

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Abstract  

We investigated the features of the glass transition relaxation of two room temperature ionic liquids using DSC. An important observation was that the heat capacity jump, that is the signature of the glass transition relaxation, shows a particularly strong value in this type of new and promising materials, candidates for a range of applications. This suggests a high degree of molecular mobility in the supercooled liquid state. The study of the influence of the heating rate on the temperature location of the glass transition signal, allowed the determination of the activation energy at the glass transition temperature, and the calculation of the fragility index of these two ionic glass-formers. It was concluded that this kind of materials belong to the class of relatively strong glass-forming systems.

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Abstract  

The thermal behaviour of salicylsalicylic acid (CAS number 552-94-3) was studied by differential scanning calorimetry (DSC). The endothermic melting peak and the fingerprint of the glass transition were characterised at a heating rate of 10C min-1. The melting peak showed an onset at T on = 144C (417 K) and a maximum intensity at T max = 152C (425 K), while the onset of the glass transition signal was at T on = 6C. The melting enthalpy was found to be ΔmH = 28.90.3 kJ mol-1, and the heat capacity jump at the glass transition was ΔC P = 108.10.1 J K-1mol-1. The study of the influence of the heating rate on the temperature location of the glass transition signal by DSC, allowed the determination of the activation energy at the glass transition temperature (245 kJ mol-1), and the calculation of the fragility index of salicyl salicylate (m = 45). Finally, the standard molar enthalpy of formation of crystalline monoclinic salicylsalicylic acid at T = 298.15 K, was determined as ΔfHm o(C14H10O5, cr) = - (837.63.3) kJ mol-1, by combustion calorimetry.

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strength and corrosion resistance. Recently, new Mg-based amorphous alloys such as the Mg–TM–RE (TM = transition metal, RE = rare earth metal) systems with high tensile strength, good ductility and a wide supercooled liquid region have been obtained by

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In spite of their cryobiological efficacy, minimum-volume vitrification methods suffer from the risk of microbiological contamination and are technically and/or manually demanding. In this study, the effects of a traditional, slightly modified vitrification method and vitrification using supercooled liquid nitrogen (VitMaster) applied for rabbit morula-stage embryos were compared. Embryos were equilibrated in a solution containing 1,2-propanediol (2.72 M) and glycerol (1.36 M) for 7 min and vitrified in 0.25-ml insemination straws after 1-min exposure to a vitrification solution containing additionally 1.0 M sucrose. Cooling was performed in ‘normal’ or supercooled liquid nitrogen. Regardless of the cooling method applied, high in vitro survival and development rates of vitrified embryos were obtained. All embryos were intact after warming, and 61 out of 65 (93.8%) and 23 out of 24 (95.8%) embryos developed to the blastocyst stage after 48-h in vitro culture of embryos vitrified in ‘normal’ or supercooled liquid nitrogen, respectively. The results suggest higher developmental ability of embryos vitrified in supercooled liquid nitrogen (91.7% vs . 83.1% of embryos vitrified traditionally developed to more advanced, expanding and/or hatching blastocyst stages). In vivo survival rate, tested for the traditional vitrification system only, revealed that 36.8% of embryos developed to term. The results show promise for establishing a fully successful method for rabbit embryo vitrification.

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Abstract  

The physical stability of amorphous drug in solid dispersion was estimated using differential scanning calorimetry (DSC). Tolbutamide (TB) and flurbiprofen (FBP) were selected as insoluble drugs in water. Polyvinylpyrrolidone (PVP) was selected as a polymer for solid dispersion. Solid dispersions of various ratios of TB or FBP and PVP-K25 were prepared by solvent evaporation method and the induction period of crystallization from amorphous drug in solid dispersion was measured by DSC. Compared with FBP, the induction period of crystallization from TB was delayed by an addition of PVP. The improvement of the physical stability by the addition of PVP-K25 was estimated from the activation energy of diffusion of drug molecules and the interfacial free energy between drug crystal and supercooled liquid of drug in solid dispersion. From thses results, the hindrance of the diffusivity of the drug molecule might be mainly affected the delay of the induction period of crystallization of TB and FBP.

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Thermal and dielectric studies of 2,2’-dihydroxybenzophenone

Progress of crystal nucleation and growth below the glass transition temperature

Journal of Thermal Analysis and Calorimetry
Authors: S. Tomitaka, M. Mizukami, F. Paladi, and M. Oguni

Summary Thermal and dielectric properties of 2,2’-dihydroxybenzophenone were studied in relation with the potential progress of crystal nucleation and growth below the ordinary glass transition temperature, T . Differential scanning calorimetry was carried out in a range 100-350 K. The α glass transition was found to occur at T =239 K. Crystallization and fusion were observed to take place when the sample was cooled down to 103 K, but not observed when cooled to 203 K. Crystal nucleation was interpreted as having happened during annealing for a short time at 103 K which is much below the T . Heat capacities were measured in a range 7-350 K by an intermittent heating method with an adiabatic calorimeter. The temperature, enthalpy and entropy of fusion were determined to be 334.46 K, 20.07 kJ mol-1 and 60.01 J K-1mol-1, respectively. Crystal growth was found to proceed even at 220 K below the T , but no glass transition was detected below 220 K. Dielectric losses were measured in a temperature range of 100-250 K and a frequency range of 30Hz-10 kHz. β-Relaxation process was found dielectrically with the activation energy of 22.6 kJ mol-1, and the corresponding glass transition was expected to occur at 76.9 K. It is discussed, based on the “structurally ordered clusters aggregation” model for supercooled liquids and glasses, that the β process is potentially attributed to the crystal nucleation progressing at 103 K.

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Abstract  

The subjects of the paper are the mechanism of vitrification and the glass transition, and a definition of the temperature of the glass transition. A comprehensive description of the structural changes occurring in the amorphous phase (‘real’ and ‘semi-ordered’) in a vicinity of the glass transition is presented. One of the major motivation of our studies is to investigate the finite size effect of the glass transition that could be related to the cooperative motion in supercooled liquids. Also, new formula, describing the relaxation time temperature change, is applied in order to better reveal themechanismof the supermolecular formation under different internal and external factors. The results of the basic methods of thermal analysis, obtained for different polymeric systems, were used in this study. The proposed approach let us correlate the thermodynamic and the structural parameters, which are estimated from the experiments, and describe all well known shapes of the DSC traces, which can be recorded in the glass transition region. Based on positron annihilation lifetime spectroscopy and dilatometric results, the significance of the free and the specific volumes for the activation of the relaxing units is discussed.

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Journal of Thermal Analysis and Calorimetry
Authors: R. Golovchak, O. Shpotyuk, A. Kozdras, B. J. Riley, S. K. Sundaram, and J. S. McCloy

supercooled liquid over time [ 4 – 7 ]. To avoid this effect, the glasses with optimally-constrained covalent networks or almost saturated physical aging should be used in applications where the aging influence is detrimental on the desired glass properties

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. Interaction between soil hydrology and boundary-layer development. Bound.-Layer Meteorol. 38. 185–202. Reisner, J., Rasmussen, R. M. & Bruintjes, R. T., 1998. Explicit forecasting of supercooled liquid water in winter storms using

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