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Abstract  

The thermal decomposition of the ammonium exchanged vermiculite takes place in three steps. A strong correlation exists between the mass loss of ammonia and water suggesting a simultaneous release. It is proposed that proton transfer from the ammonium ion to the hydroxyl units results in this simultaneous release. This behaviour could be explained by a mechanism where a resulting proton, produced by the release of ammonia out of ammonium cation, combines with a structural hydroxyl to form water. Sonication produces a substantial reduction in the particle size of the vermiculite sample. Thus, the macroscopic particle size of the untreated material is drastically reduced to the micrometers range while the structure as assayed by XRD remains unchanged. The particle size reduction produced by the sonication treatment modifies the thermal decomposition profile, mainly the mass percentages of the different steps.

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Abstract  

Roman ancient mortars have been widely studied, in connection with both diagnosis and application required for restoring. Thermoanalytical experiments performed on mortars from Pompeii and Herculaneum provided a very good understanding of the technology employed. The mortars from Pompeii were obtained by the proper mixing of lime and marble grains while mortars of Herculaneum by lime and silicates compounds. The position of the endothermic peak of calcite decomposition showed important variations in the different samples studied, which was assigned to the different crystallinity and particle sizes. Experiments under CO2 flow confirmed the presence of magnesium calcium carbonates.

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Journal of Thermal Analysis and Calorimetry
Authors: J. Poyato, L. Perez-Maqueda, M. Jimenez de Haro, J. Perez-Rodriguez, J. Šubrt, and V. Balek

Abstract  

Emanation thermal analysis (ETA), DTA, SEM, and XRD were applied for the characterization of the effect of Na+ and NH 4 + ions used for saturation of natural Mg-vermiculite on the microstructure during heating. The microstructure changes were characterized by ETA under in situ conditions of samples heating in air in the temperature range 20–1300°C. It was found that Na+ and NH 4 + ions have a significant effect on the microstructure changes during heat treatment of the natural Mg-vermiculite sample saturated with these ions. For Mg-vermiculite and Na+ saturated vermiculite thet emperatures of the onset of the collapse of interlaminar space were determined by ETA. Differences in thermal stability of the microstructure of dehydrated vermiculite samples were observed by ETA: the microstructure of dehydrated Mg-vermiculite, and Na-vermiculite was found stable until 650 and 350°C, respectively. For dehydrated NH4-vermiculite the annealing of the microstructure started at 730°C. The onset temperatures of the formation of new crystalline phases were indicated by ETA as the increase of the radon release rate. The onset temperatures of the ordering of the vermiculite structure or sintering under presence of the glassy stage (for Na-vermiculite), respectively, were determined from the decrease of the radon release rate. The ETA results were confirmed by DTA, XRD and SEM.

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Journal of Thermal Analysis and Calorimetry
Authors: V. Balek, J. Pérez-Rodríguez, L. Pérez-Maqueda, J. Šubrt, and J. Poyato

Abstract  

Thermal behaviour of natural vermiculite (Santa Olalla, Huelva, Spain) was investigated by TG, DTA, emanation thermal analysis (ETA) and high temperature XRD on heating in the temperature range from 30 to 1100°C before and after vibratory mill grinding. Microstructure changes of natural and ground vermiculite samples were characterized by using ETA under in situ conditions of heating. By comparing the ETA and XRD results it was demonstrated that a decrease of radon release rate measured by ETA characterized the decrease in the interlayer spacing of the vermiculite samples that followed the dehydration.

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Abstract  

We have studied the synthesis of polypyrrole-clay nanocomposites by the in situ oxidative polymerization of pyrrole in the interlayer space of vermiculites with different layer charges from Santa Olalla and Ojén, Spain. Moreover, the influence of different interlayer cations (Na+, Mg2+, Fe3+) on the interaction between pyrrole and the vermiculties was studied. The resulting materials were characterized by means of DTA-TG, XRD, FTIR and Mössbauer spectroscopy. In all samples polymerization of pyrrole was observed, presumably triggered by the structural iron. In most cases it was found to be externally deposited. An uptake of pyrrole in the interlayer space and PPy formation is observed in the case of the Fe3+-intercalated Ojén vermiculite, which has a lower layer charge than the Santa Olalla vermiculite.

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Journal of Thermal Analysis and Calorimetry
Authors: L. Pérez-Maqueda, V. Balek, J. Poyato, J. Pérez-Rodríquez, J. Šubrt, I. Bountsewa, I. Beckman, and Z. Málek

Abstract  

Emanation thermal analysis (ETA), thermogravimetry, DTA and XRD were used in thermal characterization of natural vermiculite (Santa Olalla, Huelva, Spain) and of Na+- and - exchanged vermiculite samples during heating in air in the range 25-1100C. A good agreement between the results of these methods was found. Changes in the radon release rate measured by ETA, which reflected the decrease and collapse of the interlayer space after the release of water as well as the formation of new crystalline phases were evaluated using a mathematical model. The model used for the evaluation was found suitable for the quantitative characterization of microstructure changes during in situ conditions of heating of vermiculite samples.

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Journal of Thermal Analysis and Calorimetry
Authors: V. Balek, L. Pérez-Maqueda, J. Poyato, Z. Černý, V. Ramírez-Valle, I. Buntseva, and J. Pérez-Rodríguez

Abstract  

The effect of grinding on thermal behavior of pyrophyllite and talc as commonly used ceramic clay minerals was investigated by DTA, TG, emanation thermal analysis (ETA), B.E.T. surface area (s.a.) measurements, X-ray diffraction (XRD) and scanning electron microscopy (SEM). A vibratory mill was used in this study, grinding time was 5 min. It was found that the grinding caused an increase in surface area and a grain size reduction of the samples. From TG and DTA results it followed that grinding caused a decrease of the temperature at which the structure bound OH groups released. The formation of high temperature phases was enhanced with the ground samples. For the ground talc sample the crystallization of non-crystalline phase into orthorhombic enstatite was observed in the range of 800°C. For ground pyrophyllite a certain agglomeration of grains was observed in the range above 950°C. Moreover, for both clays the ETA characterized a closing up of subsurface irregularities caused by grinding as a decrease of the emanation rate in the range 250–400°C. The comparison of thermal analysis results with the results of other methods made it possible to better understand the effect of grinding on the ceramic clays.

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Journal of Thermal Analysis and Calorimetry
Authors: L. Pérez-Maqueda, V. Balek, J. Poyato, J. Šubrt, M. Beneŝ, V. Ramírez-Valle, I. Buntseva, I. Beckman, and J. Pérez-Rodríguez

Abstract  

Thermal behavior of talc samples (from locality Puebla de Lillo, Spain) were characterized by emanation thermal analysis (ETA), DTA and TG. The ETA, based on the measurement of radon release rate from samples, revealed a closing up of surface micro-cracks and annealing of microstructure irregularities of the talc samples on heating in the range 200–500°C. For ground talc sample a crystallization of non-crystalline phase formed by grinding, into orthorhombic enstatite was characterized as a decrease of radon mobility in the range 785–825°C and by a DTA exothermal effect with the maximum at 830°C. ETA results characterized the microstructure development of the talc samples on heating and served to evaluate their radon mobility and transport properties on heating and cooling. Transport properties of the talc samples were evaluated by using ETA experimental data measured during heating to 600 and 1300°C, respectively, and subsequent cooling to room temperature.

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