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Differential scanning calorimetry enthalpy change determination

Although there are other ways, one of the most convenient and rapid ways to measure AH is by differential scanning calorimetry. When the temperature is reached at which a phase transition occurs, heat is absorbed, so more heat must flow to the sample in order to keep the temperature equal to that of the reference. This produces a peak in the endothermic direction. If the transition is readily reversible, cooling the sample will result in heat being liberated as the sample is transformed into the original phase, and a peak in the exothermic direction will be observed. The area of the peak is proportional to the enthalpy change for transformation of the sample into the new phase. Before the sample is completely transformed into the new phase, the fraction transformed at a specific temperature can be determined by comparing the partial peak area up to that temperature to the total area. That fraction, a, determined as a function of temperature can be used as the variable for kinetic analysis of the transformation. [Pg.275]

Differential thermal analysis (DTA) measures the amount of heat released or absorbed by a sample as it is heated at a known rate." When the enthalpy change is determined, the method is called differential scanning calorimetry (DSC). The presence of exothermic or endothermic processes at certain temperatnres provides information about the nature of phase changes and chemical reactions occurring in the material as it is heated. DTA can often be used as a sensitive method for establishing the presence or absence of secondary phases in samples if these phases undergo phase transformations at known temperatures. ... [Pg.46]

The other common category of calorimetry is differential methods, in which the thermal behavior of the substance being measured is compared to that of a reference sample whose behavior is known. In differential scanning calorimetry (DSC), the instrument measures the difference in power needed to maintain the samples at the same temperature. In differential thermal analysis (DTA), the samples are heated in a furnace whose temperature is continuously changed (usually linearly), and the temperature difference between the sample and the reference sample as a function of time can yield thermodynamic information. DSC and DTA are most commonly used for determining the temperature of a phase transition, particularly for transitions involving solids. In addition, DSC experiments can yield values for the enthalpy of a phase transition or the heat capacity. Commercial DSC and DTA instruments are available. [Pg.23]

The changes in enthalpy that occur at the LCOT of a P( /-S-f>-nBMA) copolymer (Mw=85K) were measured using differential scanning calorimetry (DSC). The volume change of the transition was determined by specular x-ray reflectivity measurements of the copolyma as a function of temperature. From the Kiessig fringes in the reflectivity profile, the thickness of the sample can be determined very... [Pg.262]

A common method to locate phase transitions and to determine the associated transition enthalpy in soft materials is differential scanning calorimetry (DSC). The differential power necessary to maintain a given temperatnre for two pans containing the material and a reference sample is recorded. A discontinuous phase transition is indicated by a sharp endotherm or exotherm which causes changes in the differential power supplied to the sample. [Pg.33]


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