Search results for "Thermal analysis"
showing 10 items of 208 documents
Intermediate valencies of vanadium cations appearing during oxidation of vanadium–iron spinels
2000
Abstract The oxidation state of vanadium cations in nanosized vanadium–iron spinels at stoichiometry and at oxidative nonstoichiometry has been investigated by associating X-ray diffraction, thermal analysis (DSC), infrared and X-ray photoelectron spectroscopies. It has been established that, during oxidation, the V3+ cations present several intermediate valencies before to realize the final oxidation state +5. A comparison was made with the oxidation of V2O3.
Comparative Study of Different Methods for the Prediction of Drug–Polymer Solubility
2015
In this study, a comparison of different methods to predict drug-polymer solubility was carried out on binary systems consisting of five model drugs (paracetamol, chloramphenicol, celecoxib, indomethacin, and felodipine) and polyvinylpyrrolidone/vinyl acetate copolymers (PVP/VA) of different monomer weight ratios. The drug-polymer solubility at 25 °C was predicted using the Flory-Huggins model, from data obtained at elevated temperature using thermal analysis methods based on the recrystallization of a supersaturated amorphous solid dispersion and two variations of the melting point depression method. These predictions were compared with the solubility in the low molecular weight liquid ana…
DSC Studies and Stability of Frozen Foods
1991
This paper discusses the role played by the “WLF decrease in viscosity” above the temperature of the glass transition (Tg) in the temperature dependence of the stability of frozen foods. In the first part, the complex features observed before the melting endotherm on DSC/DTA thermograms of sugar-water solutions are examined; they are suggested to be representative of a glass transition associated with enthalpy relaxation. In the second part, the values of Tg for some complex foods are discussed. It is shown that ice melting adds an important contribution to the WLF effect on the decrease of the viscosity of the freeze-concentrated phase. The temperature dependence of the deterioration proce…
A Promising New Method to Estimate Drug-Polymer Solubility at Room Temperature
2016
The established methods to predict drug-polymer solubility at room temperature either rely on extrapolation over a long temperature range or are limited by the availability of a liquid analogue of the polymer. To overcome these issues, this work investigated a new methodology where the drug-polymer solubility is estimated from the solubility of the drug in a solution of the polymer at room temperature using the shake-flask method. Thus, the new polymer in solution method does not rely on temperature extrapolations and only requires the polymer and a solvent, in which the polymer is soluble, that does not affect the molecular structure of the drug and polymer relative to that in the solid st…
Determination of water intrusion heat in hydrophobic microporous materials by high pressure calorimetry
2010
International audience; The understanding of interactions between a solid surface and a non-wetting liquid still remains of fundamental interest in numerous research fields, from chemistry to biology. This work focuses on the mechanisms of water intrusion in hydrophobic microporous materials through the thermal analysis of the phenomenon. A specific calorimetric technique coupled to high pressure equipment has been developed to investigate equilibrium thermal effects in such thermodynamic systems from 0 to 400 MPa under isothermal conditions. First validation tests of this method were carried out by compressing degassed water in a constant volume V with successive small pressure increments …
Study of the structural phase transformation of iron oxide nanoparticles from an Fe2+ ion source by precipitation under various synthesis parameters …
2015
Abstract Magnetite nanoparticles were precipitated from a pure aqueous ferrous salt solution in an air atmosphere. The influence of the solution molarity, the rate of precipitator agent addition, stirring time and annealing temperature was studied. The morphology, crystalline phase purity and magnetic properties of the obtained powders were studied by X-Ray powder diffraction (XRD), Scanning electron microscopy (SEM), Differential thermal analysis (DTA), X-ray photoelectron spectroscopy (XPS), X-ray absorption spectroscopy (XAS) and Vibrating sample magnetometer (VSM). The synthesis conditions were seen to have an effect on phase composition. It was possible to obtain near stoichiometric Fe…
The complementary structural studies of the double metal cyanide type catalysts for the ring opening polymerization of the oxiranes
2016
Przeprowadzono badania strukturalne katalizatorów dimetalocyjankowych (DMC) z dwoma rodzajami ligandów organicznych. Zaproponowano wyjaśnienie etapów przebiegu krzywych otrzymanych metodą analizy termograwimetrycznej i różnicowej kalorymetrii skaningowej (TG/DSC) badanych katalizatorów. Wykazano obecność kilku stopni związania ligandów w kompleksach DMC. Na podstawie wyników badań z wykorzystaniem absorpcji rentgenowskiej (XAS) stwierdzono, że centrum aktywne katalizatora stanowi atom cynku. W bezpośrednim sąsiedztwie atomów Zn wykryto obecność atomów Cl, natomiast w najbliższych sferach koordynacyjnych atomu Zn nie wykryto atomów tlenu.
A contribution to the study of staling of white bread: effect of water and hydrocolloid
1996
Abstract Staling of white bread at ambient temperature was studied using differential scanning calorimetry and dynamic mechanical thermal analysis. During storage, sample hydration varied slightly, from 0 to 0.4% per day, depending on packaging conditions. An increase in rigidity was observed, which was attributed both to starch retrogradation and to changes in the organization of the amorphous part of crumb. The glass transition temperature of crumb was not significantly modified by these structural changes. Hydrocolloids did not affect the overall shape of the viscoelastic behavior of crumb in the temperature range from −40°C to 80°C, and had a limited influence on the kinetics of starch …
New Route to Polynuclear Ni(II) and Cu(II) Complexes with Bridging Oxime Groups That Are Inaccessible by Conventional Preparations
2019
A series of new polynuclear complexes of divalent Ni and Cu with 2-cyano-2-oximino-acetic acid (later AACO2-) were obtained as the result of the ligand modification reaction in the process of complexation, using 2-cyano-2-oximino-acetates such as methyl- (later as MeCO), and ethyl- (as ECO later on). Synthesized compounds were characterized by spectroscopic methods, thermal analysis, magnetochemistry, and X-ray crystallography. Crystal data revealed the formation of the dimeric [Ni(AACO)(H2O)3]2·H2O (1), trimeric K2[Ni3(AACO)4(H2O)4]·4H2O (2), and K2[Cu3(AACO)4(H2O)4]·4H2O (3) complexes, with bridging NO-groups cyanoxime dianions. In the latter two compounds, the AACO2– anions adopt cis-arr…
Phase transitions in some n-alkanes and petroleum waxes — investigation by photoacoustic and exoelectron emission techniques
2000
Abstract The use of the photoacoustic (PA) effect and photostimulated exoelectron emission (EEE) technique in the investigation of first- and second-order phase transitions in pure n -alkanes such as n -C 22 , n -C 28 and n -C 32 and in three petroleum waxes having different carbon number distributions, have been examined. Changes in the amplitude and phase of the PA signal with temperature and the temperature dependence of the intensity of photostimulated EEE across the phase transitions have been measured. These measurements have shown that both the polymorphic phase transitions and melting of these hydrocarbons are accompanied by jumps or peaks of the PA amplitude and phase and EEE inten…