Search results for "DIFFERENTIAL SCANNING CALORIMETRY"

Crystallization, spectral, crystallographical, and thermoanalytical studies of succinobucol polymorphism.

2011

Four different polymorphs, A, C, D, and E, of succinobucol were isolated and characterized by means of solid-state nuclear magnetic resonance spectroscopy, single crystal and powder X-ray diffraction, differential scanning calorimetry, thermogravimetry, and attenuated total reflection–infrared spectroscopy. From a number of experiments, the same polymorphs (C, D, and E) and an equilibrium phase mixture B consisting of polymorphs C and D were repeatedly gained using different solvents or their mixtures. Although polymorph A was obtained directly from recrystallization only on few occasions, polymorphs C, D, and E proved to be metastable kinetic polymorphs, which slowly transform to a thermod…

Structural, Thermoanalytical and Molecular Modeling Studies on N-(3-hydroxypropyl) 3a,12a-Dihydroxy-5b-cholan-24-amide and Its Monohydrates

2007

The synthetic method for preparing N-(3-hydroxypropyl) 3 alpha,12 alpha-dihydroxy-5 beta-cholan-24-amide can lead to formation of at least three different crystal forms - an anhydrous compound and two monohydrates. The structural and thermal properties of these forms have been characterized by 13C-CP/MAS-NMR and IR spectroscopy, thermo- gravimetry, differential scanning calorimetry and by powder and single crystal x-ray crystallography. In addition, theoretical 13C-NMR chemical shift calculations were also performed for the anhydrous compound and for the first monohydrate, starting from single crystal structures and the structures of these species have now been verified. The first monohydra…

Irreversible gelation of thermally unfolded proteins:structural and mechanical properties of lysozyme aggregates

2010

The formation of protein aggregates is important in many fields of life science and technology. The morphological and mechanical properties of protein solutions depend upon the molecular conformation and thermodynamic and environmental conditions. Non-native or unfolded proteins may be kinetically trapped into irreversible aggregates and undergo precipitation or gelation. Here, we study the thermal aggregation of lysozyme in neutral solutions. We characterise the irreversible unfolding of lysozyme by differential scanning calorimetry. The structural properties of aggregates and their mechanisms of formation with the eventual gelation are studied at high temperature by spectroscopic, rheolog…

Syntheses and structural study of bile acid amidoalcohols.

2008

Preparation, structural and thermoanalytical characterization of fourteen N-hydroxyalkyl 5beta-cholan-24-amides have been performed in this study. The utilized techniques include liquid state and CP-MAS 13C NMR spectroscopy, thermogravimetry, differential scanning calorimetry, and also powder and single crystal X-ray crystallography. The results were discussed and compared to each other and also to previous findings on similar compounds. One pure hydrate form was obtained. Six new single crystal structures were determined, including one hydrated chloroform solvate. Decomposition temperatures were found to correlate with the side chain length, and the number of the hydroxyl groups. The spati…

Calorimetric Behavior of Phosphatidylcholine/Phosphatidylethanolamine Bilayers is Compatible with the Superlattice Model

2012

Differential scanning calorimetry was used to study the phase behavior of binary lipid bilayers consisting of phosphatidylcholine (PC) and phosphatidylethanolamine (PE) of varying acyl chain length. A two-state transition model was used to resolve the individual transition components, and the two-state transition enthalpy, the relative enthalpy, and the transition temperature of each component were plotted as a function of composition. Intriguingly, abrupt changes in these thermodynamic parameters were observed at or close to many "critical" X(PE) values predicted by the superlattice model proposing that phospholipids with different headgroups tend to adopt regular rather than random latera…

Reactive blending of a functionalized polyethylene with a semiflexible liquid crystalline copolyester

1996

Reactive blends (50/50 w/w) of a low molar mass polyethylene containing free carboxylic groups (PEox) and a semiflexible liquid crystalline polyester (SBH 1 : 1 : 2, by Eniricerche) have been prepared at 240 degrees C in a Brabender mixer, in the presence of Ti(OBu)(4) catalyst, for different mixing times (15, 60, and 120 min). In order to prove the formation of a PE-g-SBH copolymer, the blends have been fractionated by successive extractions with boiling toluene and xylene. The soluble fractions and the residues have been analyzed by Fourier transform infrared (FTIR) spectroscopy, thermogravimetry (TG and DTG), differential scanning calorimetry (DSC), and scanning electron microscopy (SEM)…

Reactive compatibilization of PA6/LDPE blends with an ethylene–acrylic acid copolymer and a low molar mass bis-oxazoline

2003

Abstract A sample of polyamide-6 (PA) was blended with low density polyethylene (LDPE) in the 80/20 wt/wt ratio, either without and with 2 phr of an ethylene–acrylic acid copolymer (EAA), Which was known to behave as a compatibilizer precursor, and the effect of the addition of small amounts (0.2 or 0.35 phr) of a fourth component, 2,2′-(1,3-phenylene)-bis(2-oxazoline) (PBO), was investigated. The reactions of PBO with EAA, PA and their blends were studied by recording as a function of time the torque applied to the blending apparatuses and by studying the solubility behavior of the products in formic acid. The PALDPE blends were prepared in a co-rotating twin screw extruder and were charac…

1995

About 340 g of a cycloaliphatic ionene (see formula given in the introduction) were fractionated by a continuous countercurrent extraction method (CPF). The efficiency of the separation was checked by viscometry and gel permeation chromatography (GPC). Ten different fractions with number average molecular masses between 16 000 and 29 000 D were obtained and their glass transition temperatures T g determined by differential scanning calorimetry (DSC) for their bromide and tetrafluoroborate salts. No molecular weight dependence of T g was found, in contrast to recently reported results with aliphatic ionenes, where - in case of the bromide - T g increases with rising molecular weight.

Structural and Thermal Properties of Ethylene-Norbornene Copolymers Obtained Using Vanadium Homogeneous and SIL Catalysts

2020

The series of ethylene-norbornene (E-NB) copolymers was obtained using different vanadium homogeneous and supported ionic liquid (SIL) catalyst systems. The 13C and 1H NMR (carbon and proton nuclear magnetic resonance spectroscopy) together with differential scanning calorimetry (DSC) were applied to determine the composition of copolymers such as comonomer incorporation (CNB), monomer dispersity (MD), monomer reactivity ratio (re), sequence length of ethylene (le) and tetrad microblock distributions. The relation between the type of catalyst, reaction conditions and on the other hand, the copolymer microstructure, chain termination reaction analyzed by the type of unsaturation are discusse…

Unraveling the packing pattern leading to gelation using SS NMR and X-ray diffraction: direct observation of the evolution of self-assembled fibers

2010

A detailed understanding of the mode of packing patterns that leads to the gelation of low molecular mass gelators derived from bile acid esters was carried out using solid state NMR along with complementary techniques such as powder X-ray diffraction (PXRD), differential scanning calorimetry (DSC), thermogravimetric analysis (TGA) and polarizing optical microscopy (POM). Solid state 13C{1H} cross polarization (CP) magic angle spinning (MAS) NMR of the low molecular mass gel in its native state was recorded for the first time. A close resemblance in the packing patterns of the gel, xerogel and bulk solid states was revealed upon comparing their 13C{1H}CPMAS NMR spectral pattern. A doublet r…