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Measurement of specific heat capacity via fast scanning calorimetry—Accuracy and loss corrections

Quick, C.R., Schawe, J.E.K., Uggowitzer, P.J., Pogatscher, S.
Thermochimica acta 2019 v.677 pp. 12-20
calorimetry, heat flow, lead, specific heat, temperature, uncertainty
This study explores specific heat capacity (cp) measurements via fast scanning calorimetry, with a focus on correcting measured heat flow by accounting for temperature dependent heat losses. Using MultiSTAR-UFS1 sensors with the Mettler-Toledo Flash-DSC 2+, cp of Pb (99.998% purity) was measured in dependence of the sample mass and scanning rate. Masses from 0.3–5 μg were evaluated at rates of 100, 1000 and 2000 K s−1 in the temperature range −20 to 320 °C. Two correction methods are shown and compared to cp results without corrections. Heat loss corrections are mandatory when measuring cp, but are in particular important for low masses and rates. High consistency was found between the two proposed correction procedures giving good confidence in their viability. A slight but consistent overestimation of cp compared to literature casts uncertainty upon the determined sample mass. Whilst the systems under study in this work encompass only pure Pb, the arguments and procedures of the shown method of cp determination are applicable to any system in the absence of physical transformations.