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Cell asymmetry correction for temperature modulated differential scanning calorimetry
Authors:K. Ishikiriyama  B. Wunderlich
Affiliation:(1) Department of Chemistry, The University of Tennessee, 37996-1600 Knoxville, TN;(2) Chemistry and Analytical Sciences Division, Oak Ridge National Laboratory, 37831-6197 Oak Ridge, TN, USA
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.On leave from Toray Research Center, Inc., Otsu, Shiga 520, JapanThis work was supported by the Division of Materials Research, National Science Foundation, Polymers Program, Grant # DMR 90-00520 and the Division of Materials Sciences, Office of Basic Energy Sciences, U.S. Department of Energy at Oak Ridge National Laboratory, managed by Lockheed Martin Energy Research Corp. for the U.S. Department of Energy, under contract number DE-AC05-960R22464.
Keywords:asymmetry correction  calibration  heat capacity  heat flux calorimeter  phase angle  TMDSC
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