SINGLE-RUN HEAT-CAPACITY MEASUREMENT BY DSC - PRINCIPLE, EXPERIMENTALAND DATA-ANALYSIS

Citation
Ym. Jin et B. Wunderlich, SINGLE-RUN HEAT-CAPACITY MEASUREMENT BY DSC - PRINCIPLE, EXPERIMENTALAND DATA-ANALYSIS, Thermochimica acta, 226, 1993, pp. 155-161
Citations number
31
Categorie Soggetti
Chemistry Analytical
Journal title
ISSN journal
00406031
Volume
226
Year of publication
1993
Pages
155 - 161
Database
ISI
SICI code
0040-6031(1993)226:<155:SHMBD->2.0.ZU;2-G
Abstract
A single-run heat capacity measurement has been proposed based on stan dard heat-conduction-type differential scanning calorimetry (DSC) equi pment. The experimental tests were in the range 130-560 K. The equipme nt used was the dual sample DSC and autosampler from TA Instruments, T he RMS error of all measurements when compared to well-established adi abatic calorimetry is <1% above 300 K, <3% below 200 K, and <2% betwee n 200 and 300 K. Software for data analysis has been developed with op tions for all necessary corrections, namely temperature lag, heating r ate, asymmetric correction, non-linear temperature calibration, etc. S ince the initial setup of the instrument, more than 30 different sampl es have been analyzed. It is shown in this paper that this technique c an improve the precision and reduce the experimental time compared to the normal, triple-run DSC. For the low-temperature experiment, some i mportant modifications of the instrument have been made which improve the baseline performance. Some hands-on experience is discussed.