Determination of cell asymmetry in temperature-modulated DSC |
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Authors: | A Boller I Okazaki K Ishikiriyama G Zhang B Wunderlich |
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Institution: | (1) Department of Chemistry, The University of Tennessee, 37996-1600 Knoxville, TN;(2) Chemical and Analytical Sciences Division, Oak Ridge National Laboratory, 37831-6197 Oak Ridge, TN, USA |
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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.On leave from Toray Industries, Inc., Otsu, Shiga 520, JapanOn 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-AC0S-96OR22464. Support for instrumentation came from TA Instruments, Inc. and Mettler-Toledo, Research support was also given by ICI Painls, and Toray Industries, Inc. |
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Keywords: | asymmetry correction calibration heat flux calorimeter heat capacity power compensated calorimeter temperature modulated differential scanning calorimetry TMDSC |
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