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Abstract  

The phase transitions in the LaCrO3 were studied using bulk dilatometry and high temperature X-ray diffractometry from room temperature to 1050 and 1200°C, respectively. LaCrO3 was prepared at 500°C from oxalate precursor employing microwave heating technique. Bulk shrinkage measurements on LaCrO3 pellets were carried out using dilatometer designed and fabricated in our own laboratory. Dilatometric curves of LaCrO3 showed two peaks in ΔL/L vs. temperature curves in the range 200–400 and 800–1000°C, respectively. These phase transitions have been confirmed using high temperature X-ray diffractometry. The role of simple technique like bulk dilatometry in detecting and monitoring the polymorphic transformations in solids is discussed for lanthanum chromates.

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Abstract  

119Sn conversion electron Mössbauer spectroscopy, X-ray diffractometry and energy dispersive X-ray analysis (EDAX) were employed to investigate microstructure, composition and phases present in as-electroplated Sn-Cr and Sn-Cr-Zn alloys deposited on copper substrates. In the Sn-Cr deposits Cu, -Sn, Cr-Sn phases can be identified by X-ray diffractometry. The phase composition is significantly different between the samples prepared with relatively higher and lower current densities. In the diffractograms of Sn-Cr-Zn deposits Cu, -Sn, Zn phases can be well identified. A small intensity amorphous peak is also present, which can perhaps be associated with the presence of some amorphous Zn and Sn alloy. 119Sn Mössbauer spectra of Sn-Cr deposits exhibit an asymmetric broad main line centered near the isomer shift characteristic of -Sn as well as they contain a small component near the zero velocity which can be attributed to a SnO2 phase based upon its characteristic. 119Sn Mössbauer spectra of Sn-Cr-Zn deposits are roughly similar to those of Sn-Cr deposits although the Mössbauer parameters of the third phase are different and vary with the Zn content. The presence of SnO2 on the surface mainly in the Sn-Cr samples can be attributed to the corrosion process in the air.

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Thermal analysis methods and X-ray diffractometry provided data on and permitted practical use of the eutectic mixture between Na2O·2SiO2 and SiO2, which melts at 790°C. Based on this, water glass was used as a binder to obtain artificial cluster granules, ceramically hardened by heating at 800°C. The process of water glass hardening in the presence of hardening reagents such as Na2SiF6, NH4Cl, silica gel and ultra-fine silica was studied by thermal analysis. In the first stage, gelification of the SiO2 sol takes place by neutralization of the NaOH deflocculant, while the second stage involves tridimensional cross-linking by polycondensation, promoted by powders rich in SiO2.

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Temperature-resolved X-ray diffractometry as a thermoanalytical method

A powerful tool for determining solid state reaction kinetics

Journal of Thermal Analysis and Calorimetry
Authors: M. Epple and H. K. Cammenga

Development and experimental setup of the time-, and temperature -resolved X-ray powder diffractometry are described. This method allows far deeper insight into solid state reactions than conventional thermoanalytical methods like differential scanning calorimetry (DSC) or thermogravimetry. As an example, the dehydration of caffeine hydrate was investigated. We found that in earlier stages the reaction is nucleation controlled, whereas for higher extent of reaction diffusion limitation becomes rate-controlling.

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Abstract

The laboratory micro X-ray diffraction (μ-XRD) technique is a suitable method to study minerals in-situ in whole-rock specimens without any sample preparation or in polished thin sections, and even in small amounts in powdered form. The micro X-ray diffraction method uses the conventional, closed-tube X-ray generator, but modifications were needed in the diffraction column, sample holder and detector in order to achieve μ-XRD capability.

In this paper, we present a case study of the capillary method used in µ-XRD on hydrothermal clay mineral assemblages that formed in the Velence Mts (Hungary). The capillary method in µ-XRD has many advantages in the investigation of small amounts of clay minerals: (1) easy and rapid preparation of randomly oriented, powdered samples; (2) rapid measurements; (3) accurate diffraction patterns. By using the capillary method, the formation of preferred orientation can be eliminated; thus the (hkl) reflection of the clay minerals can be precisely measured. Illite polytype quantification and the investigation of (060) reflection of clay minerals can be used satisfactorily in µ-XRD.

Hydrothermal clay mineral assemblages are indicative of temperature and pH. Their examination can determine the physicochemical parameters of the hydrothermal fluids that interacted with the host granite in the Velence Mts. The analyzed hydrothermal clay minerals from the western part of the mountains suggest lower temperatures (150–200 °C) and intermediate pH conditions. In contrast, the clay mineral assemblages' characteristics for the eastern part of the mountains indicate more intense argillization and higher temperatures (∼220 °C) and intermediate pH conditions.

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Summary Inclusion complexation between dimethyl-β-cyclodextrin and a very poorly water-soluble serum lipid-regulating agent, gemfibrozil, was studied. Products were prepared by several methods (physical mixing, kneading, spray-drying and ultrasonic treatment) in four different molecular ratios (2:1, 1:1, 1:2 and 1:3). The possibility of complex formation between the drug and the host molecule was studied by thermal analysis. Supplementary techniques, such as Fourier transformation-infrared spectroscopy and X-ray diffractometry, were also applied to interpret the results of thermal study of the products.

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Abstract  

The specimens studied in the present work consist of five terracotta fragments from an archaeological dig on the Libyan Tadrart Acacus massif, dating back to about 5000-8000 B.C. The specimens were analysed using thermogravimetric analysis (TG, DTG), differential thermal analysis (DTA), thermomechanical analysis (TMA), X-ray diffractometry, IR spectrophotometry and inductively coupled plasma spectroscopy (ICP). Analyses were aimed in particular to determine the most striking aspect of the finds, the difference in colour between the outer surface (reddish) and the darker inner portion of several of the specimens. The other main points investigated and discussed are related to the firing temperature and chemical and mineralogical composition, of terracotta specimens.

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Abstract  

Inclusion complexation between cyclodextrin derivatives (hydroxypropyl-β-cyclodextrin and methyl-β-cyclodextrin) and a very poorly water-soluble antifungal agent, ketoconazole, was studied. Solid products were prepared by physical mixing, kneading and spray-drying methods in four molecular ratios: 2:1, 1:1, 1:2 and 1:3. The possibility of complex formation between the drug and the cyclodextrins was studied by thermal analysis. Supplementary techniques, such as X-ray diffractometry and Fourier transformation-infrared spectroscopy, were also applied to interpret the results of the thermal study of the products.

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Abstract  

γ-Cyclodextrin and dimethyl-β-cyclodextrin were used as solubilizing agents for a very poorly water-soluble drug, an imidazole derivative antifungal agent, clotrimazole; with the aim of improving the physicochemical properties of the drug. Solid products were prepared by physical mixing, kneading, precipitation and spray-drying methods in 1:1 and 1:2 drug:cyclodextrin molar ratios. Drug interactions were studied by thermoanalytical methods such as DSC, DTA, TG and DTG, X-ray diffractometry and Fourier transformation-infrared spectroscopy. The results demonstrated the formation of inclusion complexes in some products.

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Journal of Thermal Analysis and Calorimetry
Authors: B. Pose-Vilarnovo, X2 Rodríguez-Tenreiro Sánchez, M. Pérez-Marcos, and J. Torres-Labandeira

Abstract  

The effect of cyclodextrin complexation of sulphamethizole (SM) was studied. Two systems were prepared with two cyclodextrin derivatives, β-cyclodextrin (BCD) and hydroxypropyl-β-cyclodextrin (HPBCD): binary complexes and multicomponent systems (cyclodextrins and a hydroxylpropylmethyl cellulose K4M). Inclusion complexes were prepared by freeze-drying and characterized by thermal analysis (DSC) and X-ray diffractometry. The presence of the polymer in the solution increases the effect of cyclodextrins – specially BCD – on the solubility of SM. In solid state, binary inclusion complexes enhance the dissolution behaviour of SM but, from the multi-component complexes, the polymer controls the release of the drug.

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