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Supporting characterization thermal analysis

Of all the methods available for the physical characterization of solid materials, it is generally agreed that crystallography, microscopy, thermal analysis, solubility studies, vibrational spectroscopy, and nuclear magnetic resonance are the most useful for characterization of polymorphs and solvates. However, it cannot be overemphasized that the defining criterion for the existence of polymorphic types must always be a non-equivalence of crystal structures. For compounds of pharmaceutical interest, this ordinarily implies that a non-equivalent X-ray powder diffraction pattern is observed for each suspected polymorphic variation. All other methodologies must be considered as sources of supporting and ancillary information, but cannot be taken as definitive proof for the existence of polymorphism by themselves. [Pg.2940]

Morphological Characterization via Thermal Analysis and Polarized Optical Microscopy Support for Partially Crystallizabie Urethane-Rich Hard Domains... [Pg.117]

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. [Pg.301]

In the third simulation example, we carried out an analysis of some of the aspects that characterize the case of the mass transfer of species through a membrane which is composed of two layers (the separative and the support layers) with the same thickness but with different diffusion coefficients of each entity or species. To answer this new problem the early model has been modified as follows (i) the term corresponding to the source has been eliminated (u) different conditions for bottom and top surfaces have been used for example, at the bottom surface, the dimensionless concentration of species is considered to present a unitary value while it is zero at the top surface (iii) a new initial condition is used in accordance with this case of mass transport through a two-layer membrane (iv) the values of the four thermal diffusion coefficients from the original model are replaced by the mass diffusion coefficients of each entity for both membrane layers (v) the model is extended in order to respond correctly to the high value of the geometric parameter 1/L. [Pg.118]

Beryllium-silicon bonds are a recent development. They are likewise prepared by the reaction of the metal halide with alkali metal silyls, but unlike the Mg analogues, both of the well-characterized Be examples are base-free. While [(te/T-Bu3Si)BeCl] is oligomeric, the molecular structure of (tert-Bu3Si)2Be features a perfectly linear Si-Be-Si unit. CpBe(SiMe3), prepared from CpBeCl and trimethylsilyllithium in pentane, exhibits an intriguing thermal chemistry. The identity of the primary thermolysis products, Scheme 14, implies the participation of silylene intermediates, a contention supported by DFT/NBO (density functional theory/natural bond order) analysis. ... [Pg.317]


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