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Abstract  

The quality of measurement of heat capacity by differential scanning calorimetry (DSC) is based on strict symmetry of the twin calorimeter. This symmetry is of particular importance for temperature-modulated DSC (TMDSC) since positive and negative deviations from symmetry cannot be distinguished in the most popular analysis methods. The heat capacities for sapphire-filled and empty aluminum calorimeters (pans) under designed cell imbalance caused by different pan-masses were measured. In addition, the positive and negative signs of asymmetry have been explored by analyzing the phase-shift between temperature and heat flow for sapphire and empty runs. The phase shifts change by more than 180° depending on the sign of the asymmetry. Once the sign of asymmetry is determined, the asymmetry correction for temperature-modulated DSC can be made.

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Abstract  

The quality of measurement of heat capacity by differential scanning calorimetry (DSC) is based on the symmetry of the twin calorimeters. This symmetry is of particular importance for the temperature-modulated DSC (TMDSC) since positive and negative deviations from symmetry cannot be distinguished in the most popular analysis methods. Three different DSC instruments capable of modulation have been calibrated for asymmetry using standard non-modulated measurements and a simple method is described that avoids potentially large errors when using the reversing heat capacity as the measured quantity. It consists of overcompensating the temperature-dependent asymmetry by increasing the mass of the sample pan.

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Journal of Thermal Analysis and Calorimetry
Authors: Luiz Carlos Machado, Marcos Tadeu D’Orlando de Azeredo, Hamilton Perez Soares Corrêa, Jivaldo do Rosário Matos, and Ítalo Odone Mazali

-TCH) function14 with the asymmetry correction described by Finger et al. [ 15 ] to account for the asymmetry due to the beam axial divergence. In order to account for the anisotropy in the half width of the reflections, the bi-dimensional model described by

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pan, respectively, and Δ C cell is the cell asymmetry correction which can be obtained in the first run; K ″ is the calibration constant related to the experimental conditions determined by the sapphire standard in the second run; mC p is the heat

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