Journal of Thermal Analysis and Calorimetry
Volume/Issue:
Volume 54: Issue 2
A Detailed Comparison of First Order Transitions by DSC and TMC
Authors:
A. Boller The University of Tennessee Department of Chemistry Knoxville TN 37996-1600 Knoxville TN 37996-1600

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M. Ribeiro The University of Tennessee Department of Chemistry Knoxville TN 37996-1600 Knoxville TN 37996-1600

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B. Wunderlich The University of Tennessee Department of Chemistry Knoxville TN 37996-1600 Knoxville TN 37996-1600

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Pages:
545–563
Online Publication Date:
13 Dec 2004
Publication Date:
01 Nov 1998
Article Category:
Research Article
DOI:
https://doi.org/10.1023/a:1010190425284
Keywords:
frequency domain; heat-flux calorimeter; indium; integral analysis; melting transition; pseudo-isothermal analysis; quasi-isothermal measurement; reversible melting; saw-tooth modulation; sinusoidal modulation; temperature-modulated calorimetry; time-domain
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Abstract  

Indium was analyzed with both, standard differential scanning calorimetry (DSC) and temperature-modulated DSC (TMDSC) using sinusoidal and saw-tooth modulation. Instrument and sample effects were separated during nucleated, reversible melting and crystallization transitions, and irreversible crystallization with supercooling. The changes in heat flow, time, and sample and reference temperatures were correlated as functions of heating rate, mass, and modulation parameters. The transitions involve three regions of steady state (an initial and a final region before and after melting/crystallization, a region while melting/crystallization is in progress) and one region of approach to steady state (melting peak to final steady state region). Analyses in the time domain show promise when instrument lags, known from DSC, are used for correction of TMDSC. A new method of integral analysis is introduced for quantitative analysis even when irreversible processes occur in addition to reversible transitions. The information was derived from heat-flux calorimeters with control at the heater block or at the reference temperature sensor.

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Cover Journal of Thermal Analysis and Calorimetry
Journal of Thermal Analysis and Calorimetry
Print ISSN:
1388-6150
Online ISSN:
1572-8943

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Journal of Thermal Analysis and Calorimetry
Language English
Size A4
Year of
Foundation		 1969
Volumes
per Year		 1
Issues
per Year		 24
Founder Akadémiai Kiadó
Founder's
Address		 H-1117 Budapest, Hungary 1516 Budapest, PO Box 245.
Publisher Akadémiai Kiadó
Springer Nature Switzerland AG
Publisher's
Address		 H-1117 Budapest, Hungary 1516 Budapest, PO Box 245.
CH-6330 Cham, Switzerland Gewerbestrasse 11.
Responsible
Publisher		 Chief Executive Officer, Akadémiai Kiadó
ISSN 1388-6150 (Print)
ISSN 1588-2926 (Online)

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