Search results for "DIFFERENTIAL SCANNING CALORIMETRY"

Crystallization kinetics of iPP: Influence of operating conditions and molecular parameters

2007

An analysis of the crystallization kinetics of different grades of isotactic polypropylene (iPP) is here presented. To describe the crystallization kinetics as a function of molecular and operating parameters, the methodological path followed was the preparation of quenched samples of known cooling histories, calorimetric crystallization isotherms tests, differential scanning calorimetry cooling ramps, wide angle X-ray diffraction (WAXD) measurements, and density determination. The WAXD analysis performed on the quenched iPP samples confirmed that during the fast cooling at least a crystalline structure and a mesomorphic one form. The diffractograms were analyzed by a deconvolution procedur…

Characterization of Dielectric Anomaly in Solid Solution Based on BaTiO3

2011

The influence of Zr doping on a structure and dielectric properties of Ba0.8Sr0.2TiO3 were studied. For this purpose Ba0.8Sr0.2Ti0.75Zr0.25O3 ceramics were obtained by a conventional method and were determined by an X-ray diffraction (XRD) and scanning electron microscopy (SEM) for crystallographic, surface morphological and compositional studies. The temperature and frequency dependence of dielectric permittivity were studied in the temperature range from 150 to 500 K and the frequency between 20 Hz and 1000000 Hz. The thermal behavior of the Ba0.8Sr0.2Ti0.75Zr0.25O3 ceramics were also studied using Differential Scanning Calorimetry. A diffusivity coefficient γ was calculated.

Phase transitions in i-butylammonium halogenoantimonate(III) and bismuthate(III) crystals

1997

Abstract Differential scanning calorimetry, dielectric, thermal expansion, infrared and preliminary X-ray diffraction studies on i-butylammonium halogenoantimonate(III) and bismuthate(III) crystals are reported. All crystals: (i-C4H9NH3)2BiCl5, (i-C4H9NH3)2SbBr5, (i-C4H9NH3)3BiCl6, (i-C4H9NH3)3Bi2Br9, (i-C4H9NH3)3Sb2Br9, show one or more structural phase transitions of first order type. The values of the transition entropies suggest that the most of the phase transitions are of the order-disorder type. The infrared studies confirmed the contribution of the i-butylammonium cations in the phase transition mechanism.

Structural characterization, thermal, dielectric and spectroscopic properties of di(n-pentylammonium) pentabromoantimonate(III): [n-C5H11NH3]2[SbBr5]

2008

Abstract The di( n -pentylammonium) pentabromoantimonate(III) compound has been synthesized and studied by means of a single-crystal X-ray diffraction, differential scanning calorimetry, thermal expansion, dielectric and IR techniques. Two solid–solid phase transitions of first order: at 416/388 K and 225/224 K (heating/cooling) have been revealed. The crystal structure of [ n -C 5 H 11 NH 3 ] 2 [SbBr 5 ] has been solved at 298 K, Pna 2 1 (phase II) and at 86 K P 2 1 2 1 2 1 (phase III). The crystal structure is composed of the SbBr 5 2 - anions which form an infinite chain and four independent n -pentylammonium cations. The dielectric studies have been made in the frequency range 500 Hz–1 …

1989

Some structurally disordered models for poly(tetrafluoroethylene) were elaborated and the corresponding calculated X-ray diffraction patterns compared with experimental patterns. This and differential scanning calorimetry results suggest some differences between the virgin powder and a sintered polycrystalline plate of poly(tetrafluoroethylene). These differences may be related to the crystal phase transitions that occur in a range of temperatures close to room temperature.

Differential scanning calorimetry investigation of phase transition in $BaZr_{x}Ti_{1-x}O_{3}$

2009

ABSTRACT Lead-free BaZrxTi1-xO3 (x = 0; 0.025; 0.125) ceramics have been obtained by a conventional method. A single-phase perovskite structure of the ceramics was identified by the X-ray diffraction method. EDS analysis, performed for the individual grains of the tested sample, showed a good homogeneous distribution of all elements throughout the grains. The thermal behaviour of BaZrxTi1-xO3 (x = 0; 0.025; 0.125) ceramics was studied using the Differential Scanning Calorimetry (DSC). Measurements showed the influence of Zr addition on the character of phase transition in the BaTiO3 structure. The results were compared with these ones obtained for pure BaTiO3.

Peracetylated β‐cyclodextrin as solubilizer of arylphosphines in supercritical carbon dioxide

2006

Abstract Effect of peracetylated β-cyclodextrin on the solubility of diphenyl(4-phenylphenyl)phosphine in supercritical carbon dioxide medium has been investigated. As shown by gravimetric measurements, the presence of cyclodextrin (CD) (1 equivalent) allows to increase the solubility of phosphine (P) in supercritical carbon dioxide (scCO 2 ) (40 °C, 35.2 MPa, nominal system density 0.89 g/mL). This solubility enhancement was attributed to host–guest interactions in scCO 2 as the P was recovered in the form of an inclusion complex. Furthermore, a diffuse reflectance spectroscopy study on the samples recovered after the experiments and on various CD/P solid mixtures obtained by co-grinding i…

New binary solid dispersion of indomethacin with surfactant polymer: From physical characterization to in vitro dissolution enhancement

2009

This article investigated preparation of solid dispersions containing a poor water-soluble drug, indomethacin (IND), and a new surfactant polymer, polyoxyethylene 32 distearate (POED). Solid dispersions were prepared by the melting method and characterized by DSC, hot-stage microscopy (HSM), X-ray diffraction (XRD) and scanning electron microscopy (SEM). DSC and HSM analyses performed on IND/POED physical mixtures indicated that IND could dissolve in liquid POED. The materials showed complete miscibility at liquid state. Combination of DSC, XRD, and SEM revealed that these materials had limited miscibility at the solid state. Up to 20% w/w IND in POED, we did not detect significant modifica…

Uncovering the metastable γ-Ag2WO4 phase: a joint experimental and theoretical study

2017

The synthesis of metastable solid phases is a pivotal starting point for innovative materials research. Here, we report the synthesis by means of a precipitation method of the metastable cubic γ-Ag2WO4 phase under ambient conditions. Different experimental techniques such as X-ray diffraction (XRD) with Rietveld refinement, field emission scanning electron microscopy (FE-SEM), micro-Raman/ultraviolet-visible (UV-vis) diffuse reflectance, photoluminescence spectroscopies, and differential scanning calorimetry (DSC) were employed. To complement the experimental data, the geometry, morphology, vibrational and electronic structure of γ-Ag2WO4 were characterized and evaluated using first-princip…

Evaluation of entropies of fusion of polychlorinated naphthalenes by model congeners: A DSC study

2006

Abstract Thirteen congeners of polychlorinated naphthalenes (PCN) were synthesized and studied by differential scanning calorimetry (DSC). Melting points (Tm) were obtained for all thirteen, and enthalpies of fusion (ΔHf) were obtained for nine congeners. Melting points of other PCNs, except for five, were found in literature. In addition, experimental ΔHf values determined by DSC were found only for 1- and 2-mono-chloronaphthalenes in the literature. The missing or uncertain values of the eight melting points and 64 enthalpies of fusion were estimated by multiple linear regressions using a set of thirteen molecular descriptors as candidates for independent variables. The stepwise model of …