Standards, calibration, and guidelines in microcalorimetry. Part 2. Calibration standards for differential scanning calorimetry* (IUPAC Technical Report)

Abstract

Differential scanning calorimeters (DSCs) are widely used for temperature, heat capacity, and enthalpy measurements in the range from subambient to high temperatures. The present recommendations describe procedures and reference materials (RMs) for the calibration of DSCs. The recommendations focus on the calibration of the response of the instrument and on the estimation of the measurement uncertainty. The procedures for temperature, enthalpy, and heat-flow rate calibration are given in detail. Calibration on cooling has also been considered. Recommended RMs are listed, and the relevant properties of these materials are discussed.

Influence of symmetry/asymmetry of the nanoparticles structure on the thermal stability of polyhedral oligomeric silsesquioxane/polystyrene nanocomposites

“…To this purpose two built‐in programs of processor, which use the fusion of indium for the enthalpy calibration and the melting points of three metals, indium, lead and zinc, for that of temperature, were employed. The calibration of enthalpy, checked by the melting of fresh indium, showed an agreement within 0.25% with the literature standard value of 3.273 kJ mol −1 [44, 45], while the accuracy of temperature, checked by several scans with fresh indium and tin, was within 0.08% in respect to literature data (156.6 and 231.9°C for indium and tin, respectively) [44, 45].…”

Thermal study on phenyl, hepta isobutyl‐polyhedral oligomeric silsesquioxane/polystyrene nanocomposites

“…The enthalpy and temperature calibrations of equipment were made by using two built‐in programs of processor, which employ the fusion of indium for the enthalpy calibration and the melting points of three metals, indium, lead, and zinc, for that of temperature. The calibration of enthalpy, checked by the melting of fresh indium, showed an agreement within 0.25% with the literature standard value of 3.273 kJ mol −1 [29, 30], while the accuracy of temperature, checked by several scans with fresh indium and tin, was within 0.08% in respect to literature data (156.6 and 231.9°C for indium and tin, respectively) [29, 30]. Calibrations were repeated every 2 weeks.…”

Low-Temperature Polymorphic Phase Transition in a Crystalline Tripeptidel-Ala-l-Pro-Gly·H2O Revealed by Adiabatic Calorimetry

“…The temperature difference between the ampule and an adiabatic shield was controlled by a four-junction copper–iron chromel thermo-couple. The sensitivity of the thermometric circuit was 1 × 10 −3 K and that of the analog-to-digital converter was 0.1 μ V. The accuracy of the calorimeter was verified using standard reference samples (K-2 benzoic acid and α -Al 2 O 3 ) 46,47 prepared by the Institute of Metrology of the State Standard Committee of the Russian Federation. The deviations of our results from the recommended values of NIST 46 are within 0.02 C p ,m between 6 and 20 K, 0.005 C p ,m between 20 and 40 K, and 0.002 C p ,m between 40 and 320 K. The standard uncertainty for the temperature was u ( T ) = 0.01 K, and the relative standard uncertainty for the enthalpies of transitions was u r ,(Δ tr , H ) = 0.002.…”