TY - JOUR
T1 - Heat capacity of microgram oxide samples by fast scanning calorimetry
AU - Bonatti, L.
AU - Brugman, B. L.
AU - Subramani, T.
AU - Leinenweber, K. D.
AU - Navrotsky, A.
N1 - Funding Information:
This work was supported by the U.S. Department of Energy, Office of Basic Energy Sciences, Grant No. DE-SC0021987. We acknowledge the use of facilities within the Eyring Materials Center and the Facility for Open Research in a Compressed Environment (FORCE) at Arizona State University. We thank Logan Leinbach for the assistance with high-pressure experiments.
Funding Information:
This work was supported by the U.S. Department of Energy, Office of Basic Energy Sciences, Grant No. DE-SC0021987. We acknowledge the use of facilities within the Eyring Materials Center and the Facility for Open Research in a Compressed Environment (FORCE) at Arizona State University. We thank Logan Leinbach for the assistance with high-pressure experiments.
Publisher Copyright:
© 2023 Author(s).
PY - 2023/5/1
Y1 - 2023/5/1
N2 - Quantitative scanning calorimetry on microgram-sized samples opens a broad, new range of opportunities for studying the thermodynamic properties of quantity-limited materials, including those produced under extreme conditions or found as rare accessory minerals in nature. We calibrated the Mettler Toledo Flash DSC 2+ calorimeter to obtain quantitative heat capacities in the range 200-350 °C, using samples weighing between 2 and 11.5 μg. Our technique is applied to a new set of oxide materials to which it has never been used before, without the need for melting, glass transitions, or phase transformations. Heat capacity data were obtained for silica in the high pressure stishovite (rutile) structure, dense post-stishovite glass, standard fused quartz, and for TiO2 rutile. These heat capacities agree within 5%-15% with the literature values reported for rutile, stishovite, and fused SiO2 glass. The heat capacity of post-stishovite glass, made by heating stishovite to 1000 °C, is a newly reported value. After accurate calibrations, measured heat capacities were then used to calculate masses for samples in the microgram range, a substantial improvement over measurement in conventional microbalances, which have uncertainties approaching 50%-100% for such small samples. Since the typical uncertainty of heat capacities measured on 10-100 mg samples in conventional differential scanning calorimetry is typically 7% (1%-5% with careful work), flash differential scanning calorimetry, using samples a factor of 1000 smaller, increases the uncertainty of heat capacity measurements by a factor of <3, opening the door for meaningful measurements on ultra-small, high-pressure samples and other quantity-limited materials.
AB - Quantitative scanning calorimetry on microgram-sized samples opens a broad, new range of opportunities for studying the thermodynamic properties of quantity-limited materials, including those produced under extreme conditions or found as rare accessory minerals in nature. We calibrated the Mettler Toledo Flash DSC 2+ calorimeter to obtain quantitative heat capacities in the range 200-350 °C, using samples weighing between 2 and 11.5 μg. Our technique is applied to a new set of oxide materials to which it has never been used before, without the need for melting, glass transitions, or phase transformations. Heat capacity data were obtained for silica in the high pressure stishovite (rutile) structure, dense post-stishovite glass, standard fused quartz, and for TiO2 rutile. These heat capacities agree within 5%-15% with the literature values reported for rutile, stishovite, and fused SiO2 glass. The heat capacity of post-stishovite glass, made by heating stishovite to 1000 °C, is a newly reported value. After accurate calibrations, measured heat capacities were then used to calculate masses for samples in the microgram range, a substantial improvement over measurement in conventional microbalances, which have uncertainties approaching 50%-100% for such small samples. Since the typical uncertainty of heat capacities measured on 10-100 mg samples in conventional differential scanning calorimetry is typically 7% (1%-5% with careful work), flash differential scanning calorimetry, using samples a factor of 1000 smaller, increases the uncertainty of heat capacity measurements by a factor of <3, opening the door for meaningful measurements on ultra-small, high-pressure samples and other quantity-limited materials.
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U2 - 10.1063/5.0131946
DO - 10.1063/5.0131946
M3 - Article
C2 - 37158701
AN - SCOPUS:85159705816
SN - 0034-6748
VL - 94
JO - Review of Scientific Instruments
JF - Review of Scientific Instruments
IS - 5
M1 - 054905
ER -