Ym. Jin et B. Wunderlich, SINGLE-RUN HEAT-CAPACITY MEASUREMENT BY DSC - PRINCIPLE, EXPERIMENTALAND DATA-ANALYSIS, Thermochimica acta, 226, 1993, pp. 155-161
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.