caa a22 4500 463189655 CHVBK 20180406164905.0 cr unu---uuuuu 170326e20071201xx s 000 0 eng 10.1007/s10973-007-8568-8 doi (NATIONALLICENCE)springer-10.1007/s10973-007-8568-8 Temperature calibration of a high-pressure DSC for measurements in ammonia [Elektronische Daten] Dependence of calibration parameters on pressure [P. van Ekeren, E. Bevers] In this paper the temperature calibration of a Mettler Toledo DSC27HP high-pressure DSC for measurements in an ammonia atmosphere is described. Measurements were performed on the melting process of three reference substances in golden crucibles: indium, tin and lead. The procedure described by the German Society for Thermal Analysis and Calorimetry, GEFTA, was applied: to correct for temperature gradients in the DSC-cel extrapolated onset temperatures of the endothermic melting peaks were measured as a function of heating rate to find by extrapolation the extrapolated onset temperature at zero heating rate, which should be a temperature corrected for temperature gradients. However, measurements performed at different pressures (between 1.5 and 8.4 bar) showed that the evaluated extrapolated onset temperatures at zero heating rate decreased with increasing pressure. This observation cannot be explained by the known dependence of melting temperatures on pressure. Therefore pressure dependence of the extrapolated onset temperatures must be caused by experimental issues. It is assumed that, although the results were extrapolated to zero heating rate, results are still influenced by temperature gradients in the DSC-cell. As a mean value, the extrapolated onset temperatures at zero heating rate decreased by 0.053°C when the pressure was raised by 1 bar. Since the software package does not allow for the pressure dependence of calibration parameters, measurement results must be corrected manually for this effect. Springer Science+Business Media, LLC., 2007 calibration nationallicence high-pressure DSC nationallicence van Ekeren P. Department Energetic Materials, TNO Defence, Security and Safety, BU3 Protection, Munition and Weapons, P. O. Box 45, 2280 AA, Rijswijk, The Netherlands aut Bevers E. Chemical Thermodynamics Group, Department of Chemistry, Utrecht University, Padualaan 8, 3584 CH, Utrecht, The Netherlands aut Journal of Thermal Analysis and Calorimetry Springer US; http://www.springer-ny.com 90/3(2007-12-01), 931-934 1388-6150 90:3<931 2007 90 10973 https://doi.org/10.1007/s10973-007-8568-8 text/html Onlinezugriff via DOI 1 research-article jats NATIONALLICENCE 856 40 https://doi.org/10.1007/s10973-007-8568-8 text/html Onlinezugriff via DOI NATIONALLICENCE 700 1- van Ekeren P. Department Energetic Materials, TNO Defence, Security and Safety, BU3 Protection, Munition and Weapons, P. O. Box 45, 2280 AA, Rijswijk, The Netherlands aut NATIONALLICENCE 700 1- Bevers E. Chemical Thermodynamics Group, Department of Chemistry, Utrecht University, Padualaan 8, 3584 CH, Utrecht, The Netherlands aut NATIONALLICENCE 773 0- Journal of Thermal Analysis and Calorimetry Springer US; http://www.springer-ny.com 90/3(2007-12-01), 931-934 1388-6150 90:3<931 2007 90 10973 Metadata rights reserved Springer special CC-BY-NC licence nationallicence BK010053 XK010053 XK010000 NATIONALLICENCE NATIONALLICENCE NL-springer