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Abstract  

Thermal stability and structural features of three newly synthesized 1:1 lattice compounds of theophylline (th) with ethylenediamine carbamate (enCO 2), 1,10-phenanthroline (phen), and 5-sulfosalicylic acid (sa-5-SO 3 H) have been studied in comparison with those of the theophylline compounds with ethanolamine (ea) and salicylic acid (sa). Simultaneous TG-DTA measurements, FTIR spectroscopy and X-ray diffraction have been carried out to get information on the various structural units of these solid inclusions, especially on the actual form (molecule, anion or cation) of theophylline moieties built in. Theophyllinate and theophyllinium ions have been found in the ethanolammonium-theophyllinate (1:1) (1, eaH + th -) and the theophyllinium salicylic acid 5-sulfonate monohydrate (1:1:1), (5, thH + saSO 3 H 2 O), respectively. Whilst the 1:1 complexes with 1,10-phenanthroline (2, thphen), ethylenediamine carbamate (3, thenCO 2), and salicylic acid (4, thsa) contain neutral theophylline moieties associated with H-bonds. In compound (3) the zwitterion of N-(2-ammonium-ethyl)carbamate (NH3 +-CH2-CH2-NH-CO- 2) is present.

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In the present study the solid and liquid phase behaviour of mandelic acid cyclodextrin systems were studied. The samples were prepared using dry grinding/kneading technique in the absence of any solvent. Thermoanalytical methods (TG, DSC, EGD) were used to characterise the solid compounds. In liquid phase the stoichiometry and the stability constants of the complexes formed were determined using UV spectrophotometry. Partial complex formation was found in case of all cyclodextrins used. The amount of uncomplexed mandelic acid varied between 10–20% of the total guest content.

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Journal of Thermal Analysis and Calorimetry
Authors: M. Crişan, Ana Brăileanu, M. Răileanu, D. Crişan, V. Teodorescu, R. Bîrjega, V. Marinescu, J. Madarász, and G. Pokol

Abstract  

Pure TiO2 and S-doped TiO2 sol–gel nanopowders were prepared by controlled hydrolysis-condensation of titanium alkoxides. The influence of different Ti-alkoxides (tetraethyl-, tetraisopropyl- and tetrabutyl-orthotitanate) used in obtaining TiO2 porous materials in similar conditions (water/alkoxide ratio, solvent/alkoxide ratio, pH and temperature of reaction) has been investigated. The relationship between the synthesis conditions and the properties of titania nanosized powders, such as thermal stability, phase composition, crystallinity, morphology and size of particles, BET surface area and the influence of dopant was investigated. The nature of the alkyl group strongly influences the main characteristics of the obtained oxide powders, fact which is pointed out by thermal analysis, X-ray diffraction, TEM and BET surface area measurements.

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Journal of Thermal Analysis and Calorimetry
Authors: J. M. Ginés, M. J. Arias, J. R. Moyano, Cs. Novak, G. Pokol, and P. J. Sánchez-Soto

A thermal study using DSC and Hot Stage Microscopy (HSM) was carried out to investigate the interaction in solid state of the binary system PEG 4000 — oxazepam, and to establish their phase diagram. The eutectic composition, which melting occurs at lower temperature as compared with the pure components, has been determined. The results obtained by DSC and HSM have indicated that PEG 4000 — oxazepam mixtures displays no obvious incompatibilities, and that the system shows a typical eutectic behaviour. However because of the closeness of the melting of PEG 4000 to the eutectic temperature, it was difficult to determine precisely the eutectic composition and temperature on the basis of DSC measurements alone. The use of heats of fusion corresponding to physical mixtures allowed an estimation of the eutectic composition at 6% w/w oxazepam. Additional information of temperature (57.6‡C) and composition (5–10% w/w oxazepam) of the eutectic was obtained by HSM using the contact method. This low melting temperature in this range of compositions offers advantages in terms of drug stability and easy manufacture.

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