Temperature modulated differential scanning calorimetry - extension to high and low frequencies

被引：55

作者：

Shoifet, Evgeni ^{[1
,2
]}

Schulz, Gunnar ^{[1
]}

Schick, Christoph ^{[1
,2
]}

机构：

[1] Univ Rostock, Inst Phys, D-18051 Rostock, Germany

[2] Univ Rostock, Dept Life Light & Matter, Fac Interdisciplinary Res, D-18051 Rostock, Germany

来源：

THERMOCHIMICA ACTA | 2015年 / 603卷

关键词：

TMDSC; Frequency; Glass transition; 5PPE; Chip calorimeter; Calvet calorimeter; GLASS-TRANSITION MEASUREMENTS; AC-CHIP CALORIMETER; HEAT-CAPACITY; PHASE-ANGLE; PART; CALIBRATION; TMDSC; RELAXATION; ENTHALPY; DSC;

D O I：

10.1016/j.tca.2014.10.010

中图分类号：

O414.1 [热力学];

学科分类号：

摘要：

Common temperature modulated DSCs are limited in the accessible frequency range to about 0.1-0.001 Hz. We describe an extension of this frequency range towards lower and higher frequencies by using conventional DSCs (without TMDSC option). By applying steps in the temperature-time profile a simultaneous multi frequency analysis of the heating rate and the heat flow rate response yields heat capacity data over about 2 orders of magnitude in frequency from one single measurement. Based on this step response analysis we show on the example of a Calvet calorimeter, Setaram BT 2.15, an extension down to 10(-5) Hz and on the example of a chip calorimeter, Mettler Toledo Flash DSC 1, an extension up to 150 Hz. Details of the experimental procedures are provided and the influence of sample size on the obtained data and general limitations, particularly regarding temperature assignment, are discussed. A relaxation map is used to combine all calorimetric data and to compare them with dielectric data. (C) 2014 Elsevier B.V. All rights reserved..

引用

页码：227 / 236

页数：10

共 57 条

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