Degradation, thermal method

The sample temperature is increased in a linear fashion, while the property in question is evaluated on a continuous basis. These methods are used to characterize compound purity, polymorphism, solvation, degradation, and excipient compatibility [41], Thermal analysis methods are normally used to monitor endothermic processes (melting, boiling, sublimation, vaporization, desolvation, solid-solid phase transitions, and chemical degradation) as well as exothermic processes (crystallization and oxidative decomposition). Thermal methods can be extremely useful in preformulation studies, since the carefully planned studies can be used to indicate the existence of possible drug-excipient interactions in a prototype formulation [7]. 

In both cases, the samples from contaminated sites were rinsed with a solvent to obtain an extract of contaminated transformer oil. The effects of biological degradation were investigated by using a commercial mixture of microorganisms and pure strain under aerobic and anaerobic condition. In the thermal method, a laboratory plasma system was used to decompose the contaminated transformer oil by a direct injection of the oil extract into the plasma system or by melting the extract samples with power plant fly ash in the plasma reactor. For the contaminated transformer oil both methods showed a destruction efficiency of 99.99% and the products of destruction were environmentally friendly. 

As its name suggests, supercritical fluid extraction (SEE) relies on the solubilizing properties of supercritical fluids. The lower viscosities and higher diffusion rates of supercritical fluids, when compared with those of liquids, make them ideal for the extraction of diffusion-controlled matrices, such as plant tissues. Advantages of the method are lower solvent consumption, controllable selectivity, and less thermal or chemical degradation than methods such as Soxhlet extraction. Numerous applications in the extraction of natural products have been reported, with supercritical carbon dioxide being the most widely used extraction solvent. However, to allow for the extraction of polar compounds such as flavonoids, polar solvents (like methanol) have to be added as modifiers. There is consequently a substantial reduction in selectivity. This explains why there are relatively few applications to polyphenols in the literature. Even with pressures of up to 689 bar and 20% modifier (usually methanol) in the extraction fluid, yields of polyphenolic compounds remain low, as shown for marigold Calendula officinalis, Asteraceae) and chamomile Matricaria recutita, Asteraceae). " ... 

Gawin, D., Pesavento, F. and Schrefler, B.A. (2003) Modelling of hygro-thermal behaviour of concrete at high temperature with thermo-chemical and mechanical material degradation. Comput. Methods Appl. Mech. Engrg. 192, 1731-1771... 

The applications of simultaneous TG-FTIR to elastomeric materials have been reviewed in the past. Manley [32] has described thermal methods of analysis of rubbers and plastics, including TGA, DTA, DSC, TMA, Thermal volatilisation analysis (TVA), TG-FTIR and TG-MS and has indicated vulcanisation as an important application. Carangelo and coworkers [31] have reviewed the applications of the combination of TG and evolved gas analysis by FTIR. The authors report TG-FTIR analysis of evolved products (C02, NH3, CHjCOOH and olefins) from a polyethylene with rubber additive. The TG-FTIR system performs quantitative measurements, and preserves and monitors very high molecular weight condensibles. The technique has proven useful for many applications (Table 1.6). Mittleman and co-workers [30] have addressed the role of TG-FTIR in the determination of polymer degradation pathways. 

DSC is often used in conjunction with TA to determine if a reaction is endothermic, such as melting, vaporization and sublimation, or exothermic, such as oxidative degradation. It is also used to determine the glass transition temperature of polymers. Liquids and solids can be analyzed by both methods of thermal analysis. The sample size is usually limited to 10-20 mg. Thermal analysis can be used to characterize the physical and chemical properties of a system under conditions that simulate real world applications. It is not simply a sample composition technique. Much of the data interpretation is empirical in nature and more than one thermal method may be required to fully understand the chemical and physical reactions occurring in a sample. Condensation of volatile reaction products on the sample support system of a TA can give rise to anomalous weight changes. 

Thermal methods as it is the DMA technique are not well suited to investigate the thermal degradation of PUs, as long as thermal degradation involves chemical... 

Acquisitions typically range in the 30-60-s timeframe. This is very important in gathering melt-state thermal conductivity because it dramatically reduces the possibility of thermal degradation. Scanning methods have been devised, permitting the automated acquisition of data at different temperatures, so that measurements over a wide range of temperatures are possible. With this, the same sample that was used for the melt-state measurements is used for solid-state measurements, thereby permitting measurements across the melt-to-solid transition. 

Rychly, J. Vesely, K. Gal, E. Kummer, M. Jancar, J. Rychla, L. Use of thermal methods in the characterization of the high-temperature decomposition and ignition of polyolefins and EVA copolymers filled with Mg(OH)2, Al(OH)3 and CaCOs. Polym. Degrad. Stab. 1990, 30, 57-72. 

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