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

A single-run heat capacity measurement has been proposed based on standard heat-conduction-type differential scanning calorimetry (DSC) equipment. The experimental tests were in the range 130-560 K. The equipment used was the dual sample DSC and autosampler from TA Instruments, The RMS error of all measurements when compared to well-established adiabatic calorimetry is <1% above 300 K, <3% below 200 K, and <2% between 200 and 300 K. Software for data analysis has been developed with options for all necessary corrections, namely temperature lag, heating rate, asymmetric correction, non-linear temperature calibration, etc. Since the initial setup of the instrument, more than 30 different samples have been analyzed. It is shown in this paper that this technique can improve the precision and reduce the experimental time compared to the normal, triple-run DSC. For the low-temperature experiment, some important modifications of the instrument have been made which improve the baseline performance. Some hands-on experience is discussed.