Measurement of specific heat capacity via fast scanning calorimetry—Accuracy and loss corrections
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In: Thermochimica Acta, Vol. 677.2019, No. June, 13.06.2019, p. 12-20.
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TY - JOUR
T1 - Measurement of specific heat capacity via fast scanning calorimetry—Accuracy and loss corrections
AU - Quick, C. R.
AU - Schawe, J. E.K.
AU - Uggowitzer, P. J.
AU - Pogatscher, S.
PY - 2019/6/13
Y1 - 2019/6/13
N2 - This study explores specific heat capacity (c p ) 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+, c p 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 c p results without corrections. Heat loss corrections are mandatory when measuring c p , 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 c p 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 c p determination are applicable to any system in the absence of physical transformations.
AB - This study explores specific heat capacity (c p ) 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+, c p 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 c p results without corrections. Heat loss corrections are mandatory when measuring c p , 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 c p 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 c p determination are applicable to any system in the absence of physical transformations.
KW - Chip calorimetry
KW - Fast scanning calorimetry
KW - Metals
KW - Specific heat capacity
M3 - Article
AN - SCOPUS:85063410160
VL - 677.2019
SP - 12
EP - 20
JO - Thermochimica Acta
JF - Thermochimica Acta
SN - 0040-6031
IS - June
ER -