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Abstract  

Attempt was made to evaluate the usefulness of thermoanalytical methods, combined with X-ray phase analysis and chemical analyses, for the study of thermal decomposition of waste materials to be subjected to thermal treatment. The object of the studies were petrochemical waste materials intended to be decomposed in a rotary furnace. Results are given of the studies of five selected waste materials.

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Abstract  

Coupled TG-FTIR technique was used for identification of gaseous compounds evolved at thermal treatment of six coal samples from different deposits (Bulgaria, Russia, Ukraine). The experiments were carried out under dynamic heating conditions up to 900C at heating rates of 5, 10 or 50 K min–1 in a stream of dry air. The emission of CO2, H2O, CO, SO2, COS, methane, methanol, formic acid, formaldehyde, acetaldehyde, chlorobenzene was clearly identified in FTIR spectra of the samples studied. The formation of ethanol, ethane, ethylene and p-xylene, at least on the level of traces, was also identified. At the heating rate of 5C min–1 the temperature of maximum intensities of the characteristic peaks of COS was 270C, of formaldehyde, formic acid, ethane and methanol 330C, of SO2, CO, acetic acid, ethylene and p-xylene 400C and of chlorobenzene 500C. At 10C min–1 and 50C min–1 these temperatures were shifted, respectively, by 70–300C and 150–450C towards higher temperatures and the respective absorption bands in FTIR spectra were, as a rule, more intensive.

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In biomaterial field, the introduction of new types of composites presents a great interest for orthopaedic surgeons. In this work, geopolymers which are a family of aluminosilicates were synthesised and mixed with biphasic mixture (hydroxyapatite and of tricalcic phosphate). The optimised thermal treatment causes the reduction of pH to 7 units and favours the expansion of composites. Consequently, the increasing of porosity percentage was induced. These properties offer a good opportunity for applied composite as potential osseous biomaterial. To study the consequences of thermal treatment in the initial amorphous structure of composites some physico-chemical techniques like SEM, MAS-NMR and FTIR were employed. These methods permitted to evaluate the porosity, different links in composites and contributions of different groups of Si and Al before and after thermal treatment.

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Thermal treatment and analysis

The art of adjacent (near-equilibrium) studies

Journal of Thermal Analysis and Calorimetry
Author: J. Šesták

Abstract  

Heating and/or cooling of substances is one of the oldest and basic methods for preparing materials with defined properties. This always leaves a definitive fingerprint of the thermal history. Beside knowing the structure we need to specify such materials by their thermodynamic behaviour, i.e., stability/metastability, phase relations and transitions, particularly establishing corresponding characteristic points. All this can be based on ordinary thermodynamics but its validity must be approved for non-equilibrium conditions of temperature changes where equilibrium and kinetic effects overlap. The slower the phase transition proceeds the greater is the deviation of the system state (kinetic curve) from its equilibrium state (equilibrium background). This makes possible to locate the actual phase boundary between two states investigated, resulting in the so-called kinetic phase diagrams. Most of modern technologies are intentionally based on non-equilibrium phenomena in order to create metastable/nonstable phases of specific properties. In this sense thermal analysis is understand as the method for determining the sample state on the basis of the sample interactions with the surroundings whose intensive parameters are controlled. Temperature is here considered as a basic parameter that connects all thermophysical measurements and thermal treatments.

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Journal of Thermal Analysis and Calorimetry
Authors: F. Mezahi, H. Oudadesse, A. Harabi, A. Lucas-Girot, Y. Le Gal, H. Chaair, and G. Cathelineau

Abstract  

The dissolution kinetic and structural behaviour of natural hydroxyapatite (N-HA) and synthetic hydroxyapatite (S-HA) was studied vs. sintering temperature and using ‘in vitro’ experiments. Obtained results highlight the chemical stability of N-HA. Any structural modification was observed until 1200°C. In the fact S-HA undergoes some modifications. XRD diagrams show the tricalcium phosphate (TCP) phase formation between 800 and 1100°C and tetracalcium phosphate (TetCP) phase formation at 1200°C. The ‘in vitro’ assay shows that the dissolution was occurred more in N-HA than in S-HA. The formed TCP activated the dissolution kinetic and then the precipitation phenomena when a continuous dissolution of TetCP leaded to slow down the kinetic precipitation.

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Progress in Agricultural Engineering Sciences
Authors: István Dalmadi, Dávid Kántor, Kai Wolz, Katalin Polyák-Fehér, Klára Pásztor-Huszár, József Farkas, and András Fekete

., Berg, R. (2003) Combined high-pressure and thermal treatments for processing of tomato puree: evaluation of microbial inactivation and quality parameters, Innovative Food Science and Emerging Technologies , 4, 377

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Rice husk ash fired at different temperatures, 450, 700 and 1000°C, was mixed with different concentrations of lime (molar lime/silica ash ratio of 0.2, 0.5 and 1.0). Each dry mixture was first ground and hydrated in the suspension form (water/solid ratio = 10) for various time intervals within the range of 1 to 365 days. The surface properties of the unhydrated and hydrated samples were studied by means of nitrogen adsorption measurements. The results indicated that the surface areas and total pore volumes of unhydrated solid mixtures and hydrated lime-rice husk ash samples, prepared with lime/silica ash ratio of 1.0, decrease with increasing firing temperature of rice husk ash. The effect of varying the lime/silica ash ratio of the solid mixture on the surface area and pore structure was fully discussed. The results of surface area and pore volume measurements could also be related to the crystal structure of silica produced from rice husk ash.

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Abstract  

H2SO4 and HCl processes accompanied by thermal treatments at different stages are described for the industrial extraction of alumina from lateritic clay minerals, especially from kaolinite, an important component of lateritic bauxites. The effects of calcination at high temperatures on the pretreatments of the raw lateritic materials, as well as on the thermal transformations of the products (salts) resulting from the acid treatments of lateritic bauxites are analyzed. Beside energetic considerations, separation methods of Al from Fe and from other lateritic-metallic components are emphasized in the extraction and purification processes. The mechanism of a controlled HCl-extracting treatment performed on iron-bearing kaolinite is described, as well as its characterization by IR and DTA ad hoc methods, enabling to distinguish between Al and Fe in the structure of lateritic kaolinite. The location and quantification of Al in the structure of lateritic goethite is also considered.

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Abstract  

The prepared amorphous γ-ZrP\SiO2 composite had a complicated composition, since a part of γ-ZrP is converted to α-form during the exfoliation of it. The γ-ZrP\SiO2 composite have specific surface area of 421 m2g–1. The acidic P–OH groups of the lamellae species placed on the surface (it is ≈1.0 meq g–1), do not destroy until the temperature of 1030 K. During the thermal treatment the total mass loss of 7.79% was found. This value corresponds to 0.42 mole of H2O per molecule unit. The water loss process was found very slow, because of the placing of bilamellar species in the composite.

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Abstract  

The photoluminescence (PL) of barite is a noncharacteristic property and cannot be used for the investigation of its structure. After thermal treatment of barite at 600°C several luminescent centers were observed, providing information about different impurities. UO 2 2+ was determined from the vibrational structure and the long decay time of the luminescence band. Two different types of uranyl were detected, thin films of uranyl mineral (most probably, reserfordin) and a solid solution of uranyl ion in barite crystal. Characteristic green luminescence of UO 2 2+ may be used as indicative feature for the prospecting of uranium deposits and for the sorting of barite ores with the aim of cleaning from harmful U impurities. Eu2+ was determined from the spectral position, the half-width and the characteristic decay time of the luminescence band. Mn2+ and Ag+ were determined by comparing luminescence bands spectral parameters to those of synthesized BaSO4−Mn and BaSO4−Ag. Fe3+ or Mn4+ were determined from the spectral-kinetic parameters of the luminescence bands.

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