Cell asymmetry correction for temperature modulated differential scanning calorimetry

被引:33
作者
Ishikiriyama, K [1 ]
Wunderlich, B [1 ]
机构
[1] OAK RIDGE NATL LAB,DIV CHEM & ANALYT SCI,OAK RIDGE,TN 37831
来源
JOURNAL OF THERMAL ANALYSIS | 1997年 / 50卷 / 03期
关键词
asymmetry correction; calibration; heat capacity; heat flux calorimeter; phase angle; TMDSC;
D O I
10.1007/BF01980494
中图分类号
O414.1 [热力学];
学科分类号
摘要
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. Tn 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 degrees depending on the sign of the asymmetry. Once the sign of asymmetry is determined, the asymmetry correction for temperature-modulated DSC can be made.
引用
收藏
页码:337 / 346
页数:10
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