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The Pleistocene travertine of Buda Vár-hegy (Castle Hill) has been studied in subsurface galleries and cellars. Lithological variations, sedimentary features of the travertine and the underlying friable chalky carbonates and calcareous clays were described in the field. Four lithotypes and several microfacies types of travertine have been identified. The stratal pattern of travertine, distribution of lithotypes, the macrofauna, and the presence of microbial sediments suggests that the travertine was deposited in a shallow lake environment. The lake was fed by lukewarm springs from the central part (probably from Szentháromság-tér [Szentháromság Square] area), where the thickest travertine deposits are found. Direct evidence of cascade deposits or terraced tetarata deposits have not been found in the studied sections. The intense cementation and recrystallisation appear in the form of at least four, mostly phreatic, cement generations, including micrite envelopes, thin fibrous rims, thick radiaxial spars and pore occluding mosaics.

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The thermal decomposition of NaHCO3

Renewed studies by DSC, SEM and FT-BR

Journal of Thermal Analysis and Calorimetry
Authors: L. Dei and G. Guarini

Abstract  

New EGA findings revealed that the small endothermal event preceding that of the main decomposition of commercial NaHCO3 involves the simultaneous evolution of water and CO2. At very high sensitivity, EGA experiments evidenced that the above (limited) evolution of gases also took place from the recrystallized material for which thermal methods gave no indication of endotherms. Careful reexamination of previous DSC results indicated that for one kind of recrystallized material a very small endotherm had been neglected. Renewed experiments revealed that this endotherm can be enhanced if the samples are prepared by crushing and sieving in a wet atmosphere. Parallel FT-IR experiments on commercial and recrystallized materials demonstrated the presence of carbonate in samples that had previously been taken just beyond the first small endotherm; this confirmed the EGA results. SEM experiments showed that surface texture changes take place when samples are heated to temperatures just above that of the preliminary endotherm. On the basis of these new findings, the interpretation previously given to the small endotherm is revised and detailed knowledge is gained on the mechanism of decomposition of NaHCO3.

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Abstract  

The systematics of isotopic exchange in a heterogeneous batch system between a dilute aqueous solution and an adsorbate or the solid adsorbent are discussed. In particular, the influence of the experimental precision on the detection of an eventual non-reactive fraction of the adsorbate is considered, down to ~ 5% of which is detectable. The exchange with the solid adsorbent is illustrated by the case of45Ca2+ and calcite. The minimum layer thickness observable in surface exchange is ~ 0.05 m. The same formalism can be applied to uptake due to recrystallization of the solid. It enables distinction between this phenomenon and diffusion into the solid.

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Abstract  

Isomorphic substitution, accompanied by surface adsorption, of a trace cation into a crystalline host matrix from its saturated solution can be studied by a double radiotracer experiment. Recrystallization of the matrix and uptake of the trace cation are thus measured simultaneously. This paper gives the formulation of the radiotracer experiment and the precision with which mole fractions of the trace cation in both phases, may be derived from it. The final result is thus a set of coexisting mole fractions and their uncertainties as a function of time. As an illustration, the case of calcite as the host matrix and CdII as the trace cation is considered.

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Abstract  

The compound BR-A657 is an angiotensin II receptor antagonist. The objective of this work was to investigate the existence of polymorphs and pseudopolymorphs of BR-A657 and the transformation of crystal forms. Three crystal forms of BR-A657 have been isolated by recrystallization and characterized by powder X-ray diffractometry, differential scanning calorimetry, and thermogravimetric analysis. After storage of three days at 0% RH (silica gel, 20°C), 52% RH (saturated solution of Na2Cr2O7·2H2O/20°C) and 95% RH (saturated solution of Na2HPO4/20°C), Forms 2 and 3 were transformed to Form 1.

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Journal of Thermal Analysis and Calorimetry
Authors: P. Espeau, B. Nicolaï, R. Céolin, M. Perrin, L. Zaske, J. Giovannini, and F. Leveiller

Abstract  

Investigation into the thermal behavior of orthorhombic Forms I and II of spironolactone, by means of differential scanning calorimetry and high-resolution X-ray powder diffraction, showed that Form I melts then recrystallizes into Form II at 373–393 K, i.e. in the temperature range within which high resolution X-ray powder diffration showed that Form I transforms into Form II. Refinements of the lattice parameters of the two forms indicated that Form I is denser than Form II in the range from 298 K up to the temperature at which it melts.

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Abstract  

Thermal characterization is proposed as analytical methodology for the purity assay of lapachol, and for determination of the quality parameters of capsules containing this molecule. The TG data revealed that lapachol is more stable in the presence of adjuvants, showing the good quality of the formulation. The kinetic parameters obtained were lower for lapachol drug than for the formulated lapachol. The DSC data demonstrated good compatibility between lapachol drug and the adjuvant in the formulated lapachol, and did not reveal impurities such as secondary products of the isolation and recrystallization processes. The data were confirmed by the DSC-photovisual findings.

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Abstract  

Differential scanning calorimetry (DSC) was used to construct phase diagrams of binary mixtures of alkylcyclohexanes and to characterize metastable phases formed in the binary mixtures. The experimentally measured liquidus curves were compared to the liquidus curves calculated using ideal solution theory. The measured phase diagrams of pentadecylcyclohexane/nonadecylcyclohexane and octadecylcyclohexane/nonadecylcyclohexane binary mixtures are consistent with theoretical phase diagrams constructed based on the assumption that these mixtures form eutectic systems. It was also observed that a metastable phase formed in some binary mixtures of pentadecylcyclohexane/nonadecylcyclohexane under fast cooling conditions. It is hypothesized that this metastable phase recrystallizes into the eutectic phase upon heating.

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Abstract  

Temperature-modulated DSC (TMDSC) was used to enhance the perfection of crystals of different poly(p-phenylene sulfide) samples formed during slow cooling from the melt. The sample preparation was made with modulated cooling using a cool-heat mode. Re-heating the samples prepared by slow conventional and modulated coolings indicated that the melting point of the samples prepared by modulated cooling is considerably higher than the melting point of the samples crystallized with conventional cooling. Thus, the perfection of crystallites can be improved if the outer layers just deposited on their surface are re-melted and re-crystallized immediately.

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Journal of Thermal Analysis and Calorimetry
Authors: M. Matthews, I. Atkinson, Lubaina Presswala, O. Najjar, Nadine Gerhardstein, R. Wei, Elizabeth Rye, and A. Riga

Abstract  

Dielectric analysis (DEA), supported by thermogravimetric analysis (TG), differential scanning calorimetry (DSC), powder X-ray diffraction analysis (PXRD) and photomicrography, reveal the chiral difference in the amino acids. The acids are classified as dielectric materials based on their structure, relating chirality to the vector sum of the average dipole moment, composed of the constant optical (electronic) and infra-red (atomic) polarizabilities, as well as dipole orientation. This study encompasses 14 L-and D-amino acid isomers. Physical properties recorded include AC electrical conductivity, charge transfer complexes, melting, recrystallization, amorphous and crystalline phases, and relaxation spectra, activation energies and polarization times for the electrical charging process.

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