Crystallization of progesterone polymorphs using polymer-induced heteronucleation (PIHn) method

Progesterone is a natural hormone steroid used in humans for several treatments and in livestock for artificial insemination, which exhibits two polymorphic forms at ambient conditions: form 1 and form 2. Form 2 is metastable and more soluble than form 1; however, it is not suitable to use as powder raw material because it transforms into form 1 by the effects of grinding. A polymorphic screening of progesterone based on polymer-induced heteronucleation method was performed as an alternative to prepare the metastable form. Polyvinyl alcohol, hydroxypropyl methylcellulose (HPMC), dextran, gelatin, polyisoprene (PI) and acrylonitrile-butadiene (NBR) copolymer were used. Crystals were prepared from 0.5, 10 and 40?mg/mL solutions in acetone at room temperature by solvent evaporation. The samples were characterized by X-ray powder diffraction, differential scanning calorimetry (DSC), scanning electron microcopy and attenuated total reflectance infrared Fourier transform spectroscopy. Form 1 was nucleated from 40?mg/mL solutions on the six polymers and from 10?mg/mL solutions on PI and NBR. The mixture of form 1 and form 2 was obtained from 10?mg/mL solution on HPMC, dextran and gelatin and from 0.5?mg/mL solution crystallizations. Therefore, the polymeric devices, which crystallized the metastable and more soluble polymorph (2) of progesterone, would be a promissory alternative for the pharmaceutical applications.     

Sicherheitstechnische Maßnahmen bei der thermischen Abluftreinigung

Safety measures in thermal waste air purification units . Safety problems may arise in thermal waste air purification units from the occasional explosive nature of the exhaust gases, which may cause a flashback into the production plant. This must be avoided by the installation of safety devices that arrest a flashback. The number of such safety devices is determined by the probability of formation of explosive waste air, according to the zone classification of the explosion-protection guide. The principal explosion arrestor devices installed between combustion chamber and production plant are liquid submersion systems, detonation barriers, and dynamic flashback-free inlets into the combustion chamber, all of which must be operated under instrumental surveillance. This report presents a state-of-the-art summary of all suitable procedures and safety devices permitting safe design of systems for thermal air cleaning problems encountered in practice.     

Model reactions on roast aroma formation

Summary From model roastings of mixtures containing serine, threonine and sucrose about 350 volatile compounds were separated and identified by GC/MS. Among them there were more than 100 monocyclic furans, 13 furanones and 8 bicyclic furans, the mass spectra and retention indices of which are recorded. The most important mass spectrometric fragmentation pathways are described. Spectra obtained from roasting coffee under identical conditions are compared with the spectra from model roastings.

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Modell-Reaktionen zur Röstaroma-BildungII. Die massenspektrometrische Identifizierung von Furanen und Furanonen aus der Reaktion von Serin und Threonin mit Saccharose unter den Bedingungen der Kaffeeröstung

Zusammenfassung Aus Modellröstungen von Gemischen aus Serin, Threonin und Saccharose unter den Bedingungen der Kaffeeröstung wurden etwa 350 flüchtige Verbindungen mittels GC/MS getrennt und identifiziert. Unter ihnen befanden sich über 100 monocyclische Furane und 13 Furanone sowie 8 bicyclische Furane, deren Massenspektren und Retentions-indices angegeben werden. Die wichtigsten massenspektrometrischen Fragmentierungswege werden beschrieben. -Die aus einer gleich behandelten Röstung von Rohkaffee erhaltenen Spektren werden mit denen der Modellröstungen verglichen.

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Dissertation Gloria Bochmann, TU Berlin 1984     

Characterization of colloidal polymer particles through stability ratio measurements

We propose a general methodology for the estimation of the doublet formation rate constant (proportional to the stability ratio of primary particles) in colloidal dispersions from measurements obtained by common optical techniques, such as dynamic light scattering, static light scattering (nephelometry) or turbidimetry. In contrast to previous approaches relying on the initial slopes of the measured quantities, such as the mean hydrodynamic radius, scattered light intensity or turbidity, we introduce a transformation of the measurables to properly scaled quantities, which grow linearly in time with a slope proportional to the doublet formation rate. Analysis of systematic and random errors allows one to control the error in the estimated value of the aggregation rate. Using this approach, we measured the aggregation rate constant of colloidal polymer particles prepared by surfactant-free emulsion copolymerization of styrene and 2-hydroxyethyl methacrylate (HEMA). It was found that the stability ratio at constant ionic strength decreases with increasing dilution of the original polymer latex. This can be explained by the presence of non-reacted stabilizing species (most likely oxidized HEMA) that desorb from the particle surface upon latex dilution and thus diminish the repulsive interactions between particles. In order to check if the stability of latex particles is influenced by reversibly adsorbed species it is always necessary to perform aggregation experiments at various dilutions.     

Importance of out-of-plane dispersion of the excitation spectrum of superconducting bilayers with Josephson coupling

We study the effect of Josephson coupling between adjacent superconducting layers on the BCS energy spectrum. We find that the interference between the gap functions of two layers can lead to vanishing condensation energy for perpendicular momenta corresponding to the formation of standing waves. We therefore predict a conventional energy spectrum for large interlayer spacings, if the gap of the single layers has no nodes, and in all cases a gapless spectrum for small spacings. Within the experimental error, our numerical results account for the low-temperature dependence of the penetration depth reported in Nd_1.85Ce_0.15CuO₄ and YBa₂Cu₃O_6.9.