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Abstract  

Processes taking place during formation of B-C-N ceramics by thermal treatment of organic precursors were investigated using emanation thermal analysis (ETA), differential thermal analysis (DTA) and thermogravimetry (TG). An additional information about thermal behavior of precursors used for preparation of BC4N, BN and CNx ceramic systems by heating in argon up to 1100C was obtained. The ETA enabled us to characterize microstructure changes in the samples at in situ conditions of thermal treatment. A good agreement of ETA, TG and DTA results was found.

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Abstract  

Zeolite-4A is a hydrated aluminosilicate which becomes more hydrated when exchanged with transition metals. In this work, the dehydration kinetics of cobalt, nickel and copper(II)-exchanged zeolite-4A were studied by means of TG and DTA over the temperature range from 20 to 500C, and the numbers of water molecules in the metal-exchanged zeolite samples were calculated. It was observed that, as the ionic radius of the hydrated metal increased, the number of water molecules also increased. The loss of water from the zeolite samples generally occurred in the temperature range 100–300C and was manifested in the DTA graphs by an extended endothermic effect. The DTA curves demonstrated that the peak position shifted towards lower temperatures as the metal concentration increased or, in other words, the water of hydration increased. The kinetic parameters (order of reaction and activation energy) were calculated via the Coats and Redfern method. The process of dehydration was found to follow first-order kinetics.

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Investigation of surface phenomena on solid catalysts by simultaneous TG and DTA

Part IV. Adsorption of ammonia on the surface of zeolites and silica-alumina gels treated with sodium hydroxide

Journal of Thermal Analysis and Calorimetry
Authors:
M. Malinowski
,
S. Malinowski
, and
S. Krzyżanowski

Simultaneous TG and DTA were used to investigate the phenomena of adsorption, desorption and surface reactions of ammonia on NaX and X type exchanged zeolites and silica-alumina gels (Ketjen) treated with sodium hydroxide. On the basis of the quantitative results it is possible to give an interpretation of these surface phenomena and to establish the existence of various active centres on the surface of the catalysts. In the case of the adsorption of ammonia on silica-alumina gels, the quantity of adsorbed ammonia is much smaller than on silica-alumina gel treated with sodium hydroxide.

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The reaction between equimolar silica and barium carbonate powders in oxygen, air or carbon dioxide was studied by means of TG and DTA. The particle size of the silica showed appreciable effects on the reactivity of the silica, on the activation energy of the reaction, and on the formation of an intermediate silicate, Ba2SiO4. The formation of Ba2SiO4 is depressed by a decrease in the silica particle size or by an increase in the partial pressure of carbon dioxide in the ambient atmosphere.

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Abstract  

Complexes of adenine, AdH, with cobalt, nickel and copper chlorides were prepared and their thermodynamic functions were determined. The complexing processes are endothermic in nature. The thermal behaviour of complexes was followed up by using TG and DTA analyses. The stoichiometry of thermal decomposition of the investigated complexes was suggested.

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Thermal analyses was performed on Egyptian date kernels to assess the value of the products as possible sources of valuable compounds. It also furnished technical data necessary for determination of the optimum degree of temperature for the design and operation of units for the pyrolytic processing of date kernels.

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Abstract  

This work is a study, by simultaneous thermogravimetry (TG) and differential thermal analysis (DTA), of the oxidation of a water resistant aluminum nitride powder which has a special protective coating, and an uncoated AlN powder which has become partially hydrated during its use. The activation energy for oxidation is estimated by the Kissinger and isoconversional methods. In the former method, the temperatures of the oxidation peaks were obtained from DTA and DTG curves. The activation energies for oxidation of the water resistant AlN, obtained by the Kissinger method, are 35710 kJ mol–1, 39212 kJ mol–1 using respectively DTG and DTA data. For the uncoated AlN, the values are 2437 and 2578 kJ mol–1, respectively. By the isoconversional method, the average values obtained for coated and uncoated samples are, respectively, 32310 and 2247 kJ mol–1. Therefore, the special coating, which protects the aluminum nitride from humidity action, also provides a higher resistance to oxidation.

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Abstract  

Thermogravimetry and differential thermal analysis, using only a combustion step with oxygen, were used to characterize carbonaceous products. Binary composition of alumina and wood charcoal, coke, carbon black, petroleum coke or carbon graphite were prepared containing 5 wt% of each. They were characterized by the burnout onset and DTA and DTG peak temperatures, which range from 476°C for wood charcoal to 790°C for carbon graphite. Complementary characterization of each product was also performed by estimating the ash content from the TG curves, and the calorific value from the DTA curves. The results indicate that these thermal analysis techniques, with only one oxygen burnout step, can be applied both for quality control of each raw material, and to determine the appropriate processing temperatures of the ceramic compositions in which they are used.

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Investigation of surface phenomena on solid catalysts by simultaneous TG and DTA

Part III. Adsorption of water on the surface of ion-exchange zeolites, silica and alumina gels treated with sodium hydroxide

Journal of Thermal Analysis and Calorimetry
Authors:
M. Malinowski
,
S. Malinowski
, and
S. Krzyżanowski

Simultaneous thermogravimetry and DTA were used to investigate the phenomena of adsorption, desorption and surface reactions of water vapour on NaX and NaYtype and NaX-exchanged zeolites, and silica and alumina gels treated with sodium hydroxide. On the basis of the quantitative results, it was possible to give an interpretation of the surface phenomena and to establish the existence of various active centres on the surface of the catalysts. Water in zeolites is probably bound by oxygen-alkali metal bonds.

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