Basic Principles of Thermoanalytical Techniques and Their Applications in Preparative Chemistry

Abstract

The investigation of thermodynamic properties and reactivity yields interesting insights into the chemistry of newly synthesized substances. With thermal analysis extensive information can be gained from small samples (often only a few milligrams). In addition, the data obtained by thermal analysis can be used to plan and optimize a synthesis. Among the most important applications are identification and purity analysis, and the determination of characteristic temperatures and enthalpies of phase transitions (melting, vaporization), phase transformations, and reactions. Investigations into the kinetics of consecutive reactions and decomposition reactions are also possible. With the instruments available today such analyses can usually be performed quickly and easily. In this review the fundamentals of thermoanalytical methods are described and illustrated with selected examples of applications to low and high molecular weight compounds.

Syntheses and Reactivity of Analogues of Grubbs’ Second Generation Metathesis Catalyst with Fluorous Phosphines: A New Phase‐Transfer Strategy for Catalyst Activation

“…DSC and TGA data were recorded with a MettlerToledo DSC821 instrument and treated by standard methods. [33] Elemental analyses were conducted with a Carlo Erba EA1110 instrument.…”

Determination of the melting temperature, heat of fusion, and purity analysis of different samples of zidovudine (AZT) using DSC

“…The principal applications in this area have included determining the degree of purity of drugs (Windmann, Scherrer, 1991), the conducting of the analyses of thermal stability and the kinetics of decomposition, the study of possible drug-drug and/or drug-excipient interactions in the pre-formulation phase (Iglesias et al, 1998;Saesma et al, 1991;Araújo et al, 2003), and in the characterization of raw materials and finished products (Ford, Timmins, 1989;Canotilho et al, 1992;Cammenga, Epple, 1995;Giron, , 1999Brown, Glass, 1999;Thompson, 2000). Canotilho and collaborators (1992) reported that the resources and potential of thermal analysis in the pharmaceutical field are considerable not only for the study of polymorphism, but also for their versatility in other applications.…”

Crystalline and Glassy Phases in the Ternary System Tl/Bi/Cl: Synthesis and Crystal Structures of the Thallium(I) Chloridobismutates(III) Tl3BiCl6 and TlBi2Cl7

“…The relation of the absolute glass transition temperature to the melting temperature allows within limits for information on the structural properties of amorphous networks. For highly symmetric polymers, made up from small monomeric units, T g /T m is generally 0.5 or lower, for the broad majority of polymers, however, this relation amounts 2/3 [22]. For the amorphous TlBi 2 Cl 7…”