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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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Abstract  

40% w/w sucrose/water solutions were analyzed by Modulated Differential Scanning Calorimetry [1] in the sub-ambient temperature region. At these temperatures, the solutions exhibit a complex, two-step thermal event. The lower-temperature event is believed to be the glass transition of the amorphous sucrose phase. The nature of the higher-temperature event is the subject of controversy. This event has been shown to have distinct second-order characteristics, and as such is believed to be a second T g. Others feel that this event is the onset of melting. The temperature region between these events contains a devitrification exotherm. Through the use of MDSC, both in scanning and stepwise quasi-isothermal modes, improved sensitivity and resolution of MDSC provides new insight into the nature of these transitions.

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Abstract  

In this study, polycardanol, which was synthesized by enzymatic oxidative polymerization of thermally treated cashew nut shell liquid (CNSL) using fungal peroxidase, was partially or fully cured using methyl ethyl ketone peroxide (MEKP) as initiator and cobalt naphthenate (Co-Naph) as accelerator. The curing behavior of polycardanol was extensively investigated in terms of curing temperature, curing time, concentration of initiator and accelerator, and the monomer-to-polymer conversion of polycardanol by means of differential scanning calorimetry (DSC). The curing behavior significantly depends on the thermal condition given and it was monitored with the change of the exotherms as a function of temperature. The optimal conditions for fully curing polycardanol are 1 wt% MEKP, 0.2 wt% Co-Naph, curing time 120 min, and curing temperature 200 °C. This study suggests that a polycardanol with high monomer-to-polymer conversion would be useful for processing a polycardanol matrix composite under the optimal conditions of curing.

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Journal of Thermal Analysis and Calorimetry
Authors: A. Vasconcelos, M. Dantas, M. Filho, R. Rosenhaim, E. Cavalcanti, N. Antoniosi Filho, F. Sinfrônio, I. Santos, and A. Souza

Abstract  

The influence of drying processes in the biodiesel oxidation was investigated by means of the oxidative induction time obtained from differential scanning calorimetry data. For this purpose, corn biodiesel was dried by different methods including: chemical (anhydrous sodium sulfate) and thermal (induction heating, heating under vacuum and with microwave irradiation). The drying efficiency was evaluated by monitoring IR absorption in the 3,500–3,200 cm−1 range and by the AOCS Bc 2-49 method. In general, the oxidative induction times increased inversely to the heating degree, except that of microwave irradiation, which was selective to water evaporation and caused low impact over the unsaturation of biodiesel. The DSC technique was shown to be a powerful tool to evaluate with high level of differentiation the influence of the drying process on the oxidative stability of biodiesel.

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Confinement of the glass-forming regions in the nanometer range influences the α-relaxation which is associated with the glass transition. These effects were investigated for semicrystalline poly(ethylene terephthalate) by dielectric spectroscopy and differential scanning calorimetry. The results are discussed within the concept of cooperative length, i.e. the characteristic length of the cooperative process of glass transition. Both experiments showed a dependence of the glass transition on the mean thickness of the amorphous layers. For the dielectric relaxation, the loss maximum was found to shift to higher temperatures with decreasing thickness of the amorphous layers, but no differences were observed in the curve shape for the differently crystallized samples. For the calorimetric measurements, in contrast, there was no correlation for the glass transition temperature, whereas the curve shape did correlate with the layer thickness of the mobile amorphous fraction. From the structure parameters, a characteristic length of approximately (2.5±1) nm was estimated for the unconfined glass relaxation (transition).

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Abstract  

Adiabatic calorimetry is a technique that has been introduced as an important approach to hazard evaluation of exothermically reactive systems. In this paper the free radical polymerization of methyl methacrylate (MMA) has been studied. One of the most important aspects of MMA polymerization is its exothermicity and autoaccelerating behaviour, these characteristics can generate the occurrence of a runaway reaction.In a runaway situation the reacting system is close to adiabatic behaviour because it is unable to eliminate the heat that is being generated. An even worse situation can be reproduced in the laboratory with the Phi-Tec pseudo-adiabatic calorimeter. Process design parameters that are usually calculated from thermodynamic data or using semiempirical rules, such as adiabatic temperature rise or maximum attainable pressure, can be directly determined.The existence of the ceiling temperature has been experimentally demonstrated.

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The modulated differential scanning calorimetry (MDSC) technique superimposes upon the conventional DSC heating rate a sinusoidally varying modulation. The result of this modulation of the heating rate is a periodically varying heat flow, which can be analysed in various ways. In particular, MDSC yields two components (‘reversing’ and ‘non reversing’) of the heat flow, and a phase angle. These each show a characteristic behaviour in the glass transition region, but their interpretation has hitherto been unclear. The present work clarifies this situation by a theoretical analysis of the technique of MDSC, which introduces a kinetic response of the glass in the transition region. This analysis is able to describe all the usual features observed by MDSC in the glass transition region. In addition, the model is also able to predict the effects of the modulation variables, and some of these are discussed briefly.

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Abstract  

The application of differential scanning calorimetry (DSC) for purity determination is well documented in literature and is used amongst others in the analysis of pure organic crystalline compounds. The aim of this work is to examine whether the DSC method for purity determination consistently produces values for the purity of polycyclic aromatic hydrocarbons (PAHs) which are sufficiently accurate as required for the certification of reference materials. For this purpose, 34 different existing PAH certified reference materials were tested. The DSC results are shown to be consistent with the results obtained by other methods assessing the organic impurities content in PAHs, like gas chromatography (GC), high performance liquid chromatography (HPLC) and mass spectrometry. Significant differences between the measured values and the certified purity values were observed only in a limited number of cases.

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Abstract  

The phase diagram for the AgNO3−KNO3 system has been determined using differential scanning calorimetry (DSC). Eutectic point has been found at 391 K andX Ag=0.580 mole fraction AgNO3. The DSC curves indicate the existence of an intermermediate compound (AgNO3·KNO3) in the KNO3-rich region of the phase diagram. This compound was identified in the solid phase by X-ray diffraction. The melting and the crystallization processes were followed with the aid of a hot stage microscope, too.

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Abstract  

Thermal analysis of the binary system KCl-LiCl in the composition range 0.368–0.812 mol fraction of LiCl was studied by differential scanning calorimetry (DSC). On the basis of the DSC curves, the experimental data for the phase-diagram, the latent heat of fusion, and the average specific heat in the liquid and solid states are presented as a function of the composition of the mixture. The experimental results compared with literature data. The following empirical correlation between the heat of fusion (ΔH) and of compositions of the mixture in mol fraction of LiCl (x) was obtained: ·GH=26.95−50.20x+43.06x2 with a minimum value of 11.8 kJ(g mol)−1 at the eutectic point of 0.587 mol fraction of LiCl at 354.4°C. These results are required as basic data to develop thermal energy storage materials, based on the phase change of a molten mixture of KCl-LiCI.

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