Differential scanning calorimetry dynamic method

Tg can be measured by dilatometry, refractive index, differential scanning calorimetry, dynamic mechanical methods and by dielectric relaxation techniques. 

The kinetics of copolymerization or curing of epoxy resins with cyclic anhydrides initiated by tertiary amines was investigated by chemical analysis 52,65,73,74,90) differential scanning calorimetry isothermal methods electric methods , dynamic differential thermal analysis , IR spectroscopy dilatometry or viscometry Results of kinetic measurements and their interpretation differ most authors agree, however, that the copolymerization is of first order with respect to the tertiary amine. 

Thermal analysis is well suited for characterizing and identifying plastics, as their properties are temperature dependent. It involves methods in which the substance is subjected to a controlled temperature program and the changes in the physical and chemical properties are measured as a function of temperature or time. The ambient atmosphere also influences the properties of plastic. Thermal analysis comprises traditional techniques differential scanning calorimetry (DSC), differential thermal analysis, thermogravimetric analysis, thermomechanical analysis, and more recent methods pressure differential scanning calorimetry, dynamic mechanical analysis, and differential photocalorimetry. 

Glass-transition temperatures are commonly determined by differential scanning calorimetry or dynamic mechanical analysis. Many reported values have been measured by dilatometric methods however, methods based on the torsional pendulum, strain gauge, and refractivity also give results which are ia good agreement. Vicat temperature and britde poiat yield only approximate transition temperature values but are useful because of the simplicity of measurement. The reported T values for a large number of polymers may be found ia References 5, 6, 12, and 13. 

Most of the physical properties of the polymer (heat capacity, expansion coefficient, storage modulus, gas permeability, refractive index, etc.) undergo a discontinuous variation at the glass transition. The most frequently used methods to determine Tg are differential scanning calorimetry (DSC), thermomechanical analysis (TMA), and dynamic mechanical thermal analysis (DMTA). But several other techniques may be also employed, such as the measurement of the complex dielectric permittivity as a function of temperature. The shape of variation of corresponding properties is shown in Fig. 4.1. 

Provder, T., Holsworth, R. M., Grentzer, T. H., and Kline, S. A. (1983). Use of the single dynamic temperature scan method in differential scanning calorimetry for quantitative reaction kinetics. In Polymer Characterization, Craver, C. D. (Ed.), Advances in Chemistry 203, pp. 233-253. Am. Chem. Soc., Washington, DC. 

Electron microscopy (5,40,52,63, 64), on the other hand, can provide direct information on the domain structure under favorable conditions, such as when the domains are crystalline. When the samples exhibit a semicrystalline superstructure, small-angle light scattering and polarized microscopy have been used in addition to electron microscopy to study the spherulitic structure. These methods are complemented by differential scanning calorimetry, and various techniques for studying dynamic mechanical behavior which can be interpreted to give additional, if somewhat less direct, information on domain structure. 

From the late 1960 s to the early 1970 s, more direct approaches to the investigation of protein dynamics were intensively developed. Such investigations featured the application of physical methods, such as physical labeling, NMR, optical spectroscopy, fluorescence, differential scanning calorimetry, and X-ray and neutron scattering. The purposeful application of the approaches made it possible to obtain detailed information on the mobility of different parts of protein globules and to compare this mobility with both the functional characteristics and stability of proteins, and with results of the theoretical calculation of protein dynamics. 

Many relatively slow or static methods have been used to measure Tg. These include techniques for determining the density or specific volume of the polymer as a function of temperature (cf. Fig. 11-1) as well as measurements of refractive index, elastic modulus, and other properties. Differential thermal analysis and differential scanning calorimetry are widely used for this purpose at present, with simple extrapolative eorrections for the effects of heating or cording rates on the observed values of Tg. These two methods reflect the changes in specific heat of the polymer at the glass-to-rubber transition. Dynamic mechanical measurements, which are described in Section 11.5, are also widely employed for locating Tg. 

We have used X-ray methods to compare the crystallite size of RIM specimens prepared with and without use of a polyether diamine (PEDA) additive. These results are compared with differential scanning calorimetry data on the hard domain melting behavior and dynamic-mechanical studies of the extent of phase separation. Mechanical data on flexural modulus, elongation, impact strength, and heat sag behavior have been obtained for the same specimens and have been correlated with the structural analyses. 

Differential scanning calorimetry (DSC) is a calorimetric method that finds widespread use in many fields, including protein dynamics, polymers, pharmaceuticals, and inorganic materials. DSC measures energy (heat) flow into a sample and a reference substance as a function of controlled increase or decrease of temperature. In a typical power-compensated DSC (Fig. 3.2), the sample and reference are placed on metal pans in identical furnaces each containing a platinum resistance thermometer (thermocouple) and heater. During a thermal transition (e.g., when a physical change in the sample occurs),... 

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