Thermal Analysis DTA and Differential Scanning Calorimetry DSC

Difl erential thermal analysis (DTA) and differential scanning calorimetry (DSC) are the other mainline thermal techniques. These are methods to identify temperatures at which specific heat changes suddenly or a latent heat is evolved or absorbed by the specimen. DTA is an early technique, invented by Le Chatelier in France in 1887 and improved at the turn of the century by Roberts-Austen (Section 4.2.2). A... 

Thermal analytical techniques such as thermogravimetry (TG), differential thermal analysis (DTA) and differential scanning calorimetry (DSC) have all been successfully employed in studying the pyrotechnic reactions of energetic materials such as black powder, as well as of binary mixtures of the constituents. 

Differential thermal analysis (DTA) and differential scanning calorimetry (DSC) are the most widely used thermal analysis techniques. Both techniques have the same objective to examine thermal events in a sample by heating or cooling without mass exchange with its surroundings. The thermal events examined by DTA and DSC include solid phase transformation, glass transition, crystallization and melting. Differential emphasizes that analysis is based on differences between sample material and a reference material in which the examined thermal events do not occur. 

DIFFERENTIAL THERMAL ANALYSIS (DTA) AND DIFFERENTIAL SCANNING CALORIMETRY (DSC)... 

Differential thermal analysis (DTA) and differential scanning calorimetry (DSC) are also useful methods for structure determination. These methods can detect crystallization of amorphous alloy catalysts as a result of heat treatment (21, 23, 41-44) or as a result of the action of reacting gases, such as in the case of hydrogenation of carbon monoxide (53) or ammonia synthesis (22). 

In thermal methods of analysis, either temperature change is measured or the temperature is manipulated to produce the measured parameter. Thermogravimetry (TG), differential thermal analysis (DTA), and differential scanning calorimetry (DSC) are the three major methods that use temperature change as the independent variable. Thermometric titration (TT) and direct-injection enthalpimetry (DIE) use temperature as the dependent variable. These five methods will be discussed primarily from an analytical point of view. Each method has its unique characteristics and capabilities for that reason, the major aspects of each method are considered individually. 

Differential thermal analysis (DTA) and differential scanning calorimetry (DSC) are similar techniques. They measure change in the heat capacity of a sample. These techniques can be used to determine various transition temperatures (T , Tg, T , Tp, etc.), specific heat, heat of fusion, percent crystallinity, onset of degradation temperature, induction time, reaction rate, crystallization rate, etc. A DSC instrument operates by compensating electrically for a change in sample heat. The power for heating is controlled in such a way that the temperature of the sample and the reference is the same. The vertical axis of a DSC temperature scan shows the heat flow in cal/s. 

Both differential thermal analysis (DTA) and differential. scanning calorimetry (DSC) are concerned with the measurement of energy changes, and as such are applicable in principle to a wider range of processes than TG. From a practical standpoint DSC may be regarded as the method from which quantitative data are most easily obtained. The use of DSC to determine absolute thermodynamic quantities is discussed in Sections 26.2.3.2 and 26.2.4.1. Types of processes amenable to study by these methods are summarized in Table 2. 

The crystallization kinetics of amorphous materials can be investigated either isothermally or non-isothermally by using thermal analysis techniques. In the isothermal method, the sample is heated above the glass transition temperature and the heat absorbed during the crystallization process is measured as a function of time. On the other hand, in the non-isothermal method, the sample is heated at a fixed rate and then the change in enthalpy is recorded as a function of temperature. Thermal analysis techniques such as differential thermal analysis (DTA) and differential scanning calorimetry (DSC) are quite popular for kinetic analysis of crystallization processes in amorphous solids (Araujo Idalgo, 2009 Malek, 2000 Prasad Varma, 2005). 

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