924 resultados para thermal degradation
Resumo:
Thermal decomposition and combustion of lithium perchlorate ammine:ammonium perchlorate (LPA:AP) and magnesium perchlorate ammine:ammonium perchlorate (MPA:AP) pellets have been studied using DTA, TG, and strand burner techniques. The DTA results of the ammine:AP pellets show that the addition of ammines lowers the ignition temperature of AP. However, isothermal TG of the ammine:AP pellets show that in the case of LPA:AP pellets the extent of decomposition increases with the increase in the concentration of LPA; whereas in the case of MPA:AP pellets the extent of decomposition decreases with the increase in the concentration of MPA. Similarly, LPA:AP pellets show higher burning rates compared to AP pellets. On the other hand, MPA:AP pellets show lower burning rates compared to AP pellets. Increasing the concentration of MPA in MPA:AP pellets completely suppresses the combustion. These results are explained on the basis of the thermal characteristics of the additives and their decomposition products.
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Pressurised hot water extraction (PHWE) exploits the unique temperature-dependent solvent properties of water minimising the use of harmful organic solvents. Water is environmentally friendly, cheap and easily available extraction medium. The effects of temperature, pressure and extraction time in PHWE have often been studied, but here the emphasis was on other parameters important for the extraction, most notably the dimensions of the extraction vessel and the stability and solubility of the analytes to be extracted. Non-linear data analysis and self-organising maps were employed in the data analysis to obtain correlations between the parameters studied, recoveries and relative errors. First, pressurised hot water extraction (PHWE) was combined on-line with liquid chromatography-gas chromatography (LC-GC), and the system was applied to the extraction and analysis of polycyclic aromatic hydrocarbons (PAHs) in sediment. The method is of superior sensitivity compared with the traditional methods, and only a small 10 mg sample was required for analysis. The commercial extraction vessels were replaced by laboratory-made stainless steel vessels because of some problems that arose. The performance of the laboratory-made vessels was comparable to that of the commercial ones. In an investigation of the effect of thermal desorption in PHWE, it was found that at lower temperatures (200ºC and 250ºC) the effect of thermal desorption is smaller than the effect of the solvating property of hot water. At 300ºC, however, thermal desorption is the main mechanism. The effect of the geometry of the extraction vessel on recoveries was studied with five specially constructed extraction vessels. In addition to the extraction vessel geometry, the sediment packing style and the direction of water flow through the vessel were investigated. The geometry of the vessel was found to have only minor effect on the recoveries, and the same was true of the sediment packing style and the direction of water flow through the vessel. These are good results because these parameters do not have to be carefully optimised before the start of extractions. Liquid-liquid extraction (LLE) and solid-phase extraction (SPE) were compared as trapping techniques for PHWE. LLE was more robust than SPE and it provided better recoveries and repeatabilities than did SPE. Problems related to blocking of the Tenax trap and unrepeatable trapping of the analytes were encountered in SPE. Thus, although LLE is more labour intensive, it can be recommended over SPE. The stabilities of the PAHs in aqueous solutions were measured using a batch-type reaction vessel. Degradation was observed at 300ºC even with the shortest heating time. Ketones and quinones and other oxidation products were observed. Although the conditions of the stability studies differed considerably from the extraction conditions in PHWE, the results indicate that the risk of analyte degradation must be taken into account in PHWE. The aqueous solubilities of acenaphthene, anthracene and pyrene were measured, first below and then above the melting point of the analytes. Measurements below the melting point were made to check that the equipment was working, and the results were compared with those obtained earlier. Good agreement was found between the measured and literature values. A new saturation cell was constructed for the solubility measurements above the melting point of the analytes because the flow-through saturation cell could not be used above the melting point. An exponential relationship was found between the solubilities measured for pyrene and anthracene and temperature.
Resumo:
Thermal analysis of hydrazinium metal sulphates, (N2H5)2 M(SO4)-I, and their hydrazinates, (N2H5)2−M(SO4)23N2H4−II, whereM=Fe, Co and Ni have been investigated using thermogravimetry and differential thermal analysis. Type II compounds on heating decompose through an intermediate I and metal suphlate to the respective metal oxides.
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Trioxalatocobaltates of bivalent metals KM2+[Co(C2O4)3]·x H2O, with M2+ = Ba, Sr, Ca and Pb, have been prepared, characterized and their thermal behaviour studied. The compounds decompose to yield potassium carbonate, bivalent metal carbonate or oxide and cobalt oxide as final products. The formation of the final products of decomposition is influenced by the surrounding atmosphere. Bivalent metal cobaltites of the types KM2+CoO3 and M2+CoO3—x are not identified among the final products of decomposition. The study brings out the importance of the decomposition mode of the precursor in producing the desired end products.
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Treatment of N. crassa cultures with cycloheximide followed by washing and incubation in drug-free fresh medium results in a rapid decline in cytochrome oxidase activity. This is associated with the degradation of higher molecular weight subunits of cytochrome oxidase under these conditions. The protease activity associated with the mitochondrial preparation decreases during cycloheximide treatment and rapidly returns to normal levels on subsequent washing and transfer to drug-free fresh medium. It is suggested that the steady-state level of cytochrome oxidase is governed by a rapidly turning over cytoplasmically synthesized mitochondrial protease.
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Abstract is not available.
Resumo:
Indospicine toxicosis was reported in sheep, goats and cattle fed on Indigofera, a leguminous plant rich in indospicine. Recent death report on dogs as a result of dietary ingestion of indospicine contaminated camel meat has raised concern about the distribution of this toxin in camels fed on Indigofera. This in vitro study aimed at measuring the degradability of indospicine in Indigofera spicata by camel-foregut fluid and attempted at explaining indospicine accumulation in meat tissue. In the first experiment, in vitro dry matter digestibility and indospicine disappearance were evaluated by using foregut fluid from 15 feral camels. Foregut fluid was collected post mortem from a nearby abattoir. In the second experiment, a composite foregut fluid obtained from three feral camels was used to examine the time-dependent degradation of indospicine. Results indicated that 99 of the dietary indospicine was degraded after 48 h of incubation. The time-dependent degradation study showed rapid degradation (11 µg/h) during the first 18 h of incubation, followed by a much slower rate (2 µg/h) between 18-48 h. Results demonstrated the ability of the camel microbiota to degrade indospicine and suggest the presence of a by-pass mechanism that enables the toxin to escape degradation and reaches the intestine.
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Thermal behaviour of ammonium perchlorate-aluminium composites is studied using differential thermal analysis, thermogravimetry and differential scanning calorimetry. Electrical resistivity studies throw light on the mechanism of ammonium perchlorate decomposition at different aluminium contents. The differences observed in burning behaviour by earlier authors is explained in terms of porosity and thermal conductivity of the composite.
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Precise measurements of the ultrasonic velocities and thermal expansivities of amorphous Se80Te20 and Se90Te10 alloys are reported near the glass transition. The samples are produced by liquid quenching. The longitudinal and transverse velocities are measured at 10 MHz frequency using the McSkimin pulse superposition technique. The thermal expansivities,agr, are measured using a three-terminal capacitance bridge. Theagr-values show a sharp maximum near the glass transition temperature,T g. The ultrasonic velocities also show a large temperature derivative, dV/dT nearT g. The data are discussed in terms of existing theories of the glass transition. The continuous change inagr shows that the glass transition is not a first-order transition, as suggested by some theories. The samples are found to be deformed by small loads nearT g. The ultrasonic velocities and dV/dT have contributions arising from this deformation.
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Metal oxalate hydrazinates MC2O4·2 N2H4 where M=Mg, Mn, Fe, Co, Ni, Cu, Zn and Cd have been prepared and characterised by chemical analysis and infrared spectra. Thermal reactivity and decomposition of these oxalato complexes have been studied using thermogravimetry and differential thermal analysis. Hydrazinates of Mn, Fe, Co, Ni and Cu oxalates exhibit autocatalytic decomposition behaviour whereas the others do not. This phenomenon can be attributed to the presence of a bridged hydrazine as well as the thermal stability of the anhydrous metal oxalates.
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The phase transition in gamma-irradiated triglycine sulphate (TGS) has been investigated by using a method based on the measurement of thermal noise. The results of a study of the polarization switching characteristics of gamma irradiated TGS and sodium nitrite (NaNO2) have also been presented. The effect of irradiation on the phase transition and the switching processes has been discussed.
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A simple technique for determining the energy sensitivities for the thermographic recording of laser beams is described. The principle behind this technique is that, if a laser beam with a known spatial distribution such as a Gaussian profile is used for imaging, the radius of the thermal image formed depends uniquely on the intensity of the impinging beam. Thus by measuring the radii of the images produced for different incident beam intensities the minimum intensity necessary (that is, the threshold) for thermographic imaging is found. The diameter of the laser beam can also be found from this measurement. A simple analysis based on the temperature distribution in the laser heated material shows that there is an inverse square root dependence on pulse duration or period of exposure for the energy fluence of the laser beam required, both for the threshold and the subsequent increase in the size of the recording. It has also been shown that except for low intensity, long duration exposure on very low conductivity materials, heat losses are not very significant.