A new <i>in situ</i> electrical calibration system for high temperature Calvet calorimeters

Razouk, Refat; Hay, Bruno; Himbert, M.

doi:10.1063/1.4821876

Cited by 14 publications

(17 citation statements)

References 13 publications

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“…La caractérisation métrologique du calorimètre a été réalisée avec ce nouveau système d'étalonnage afin d'étudier l'influence de certains paramètres (énergie, température, durée de dissipation) sur la détermination de la sensibilité des thermopiles. Les résultats de cette caractérisation métrologique ont été publiés par Razouk [12]. Ce moyen de référence et les procédures d'étalonnage et de mesure ont ensuite été utilisés pour la détermination des enthalpies de fusion de l'indium, l'étain et l'argent.…”

Section: Introductionunclassified

Qualification d’un calorimètre à flux pour la caractérisation de matériaux de référence en enthalpie de fusion jusqu’à 1 000 °C

Razouk¹,

HAY²,

HAMEURY³

et al. 2015

R. franç. métrol.

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Le Laboratoire commun de métrologie LNE-Cnam (LCM) a développé un moyen de référence en calorimétrie permettant des mesures précises d'enthalpie de fusion et de capacité thermique massique sur la plage de température [23 • C, 1 000 • C]. La solution métrologique retenue a été d'améliorer un calorimètre de type Calvet, et de mettre au point des procédures d'étalonnage et de mesure permettant d'atteindre des incertitudes de mesure suffisamment faibles pour la certification de matériaux de référence. Cet article décrit un système d'étalonnage fonctionnant à haute température qui a été spécifiquement conçu et intégré dans le calorimètre afin d'effectuer son étalonnage en énergie par substitution électrique. Ce système permet de réaliser successivement des étalonnages par effet Joule et des mesures d'enthalpie de fusion, sans modification des conditions expérimentales. Ce nouveau calorimètre de référence ainsi que la méthode de mesure associée ont été qualifiés en mesurant les enthalpies de fusion de métaux purs (indium, étain et argent). Les résultats obtenus sur ces trois matériaux métalliques sont en très bon accord avec les données obtenues par d'autres laboratoires nationaux de métrologie.

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Section: Introductionunclassified

Qualification d’un calorimètre à flux pour la caractérisation de matériaux de référence en enthalpie de fusion jusqu’à 1 000 °C

Razouk¹,

HAY²,

HAMEURY³

et al. 2015

R. franç. métrol.

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“…This temperature is defined by the intersection of the interpolated baseline and the tangent drawn at point of inflection of the rising side of the peak. The assumption of the linearity of the sensitivity versus temperature between T1 and T2 was previously verified [12].…”

Section: Calibration and Measurement Proceduresmentioning

confidence: 99%

“…An acquisition system with calibrated devices has been assembled in order to perform accurate and traceable measurements of the energy released in the calorimeter during the calibration process, and of the electromotive force (EMF) delivered by the two thermopiles in both calibration and enthalpy measurement steps. More information on this calibration system has already been published [12]. …”

Section: Figure 1 Instrumented Calibration Cruciblementioning

confidence: 99%

“…It can be used to perform the heat calibration of the calorimeter by electrical substitution (Joule effect) and the enthalpy measurements without modification of the apparatus, so that the experimental conditions during both steps remain unchanged. The performances of this new calibration system as well as the metrological features (repeatability, linearity…) of the calorimeter were evaluated by investigating the impact of some influence parameters (level of energy, temperature, dissipation time) on the determination of the sensitivity factor of its thermopiles (the results of this metrological characterisation were presented in a previous paper [12]). This reference facility, and the procedures of calibration and measurement associated, have been then applied to the determination of the enthalpies of fusion of indium, tin, silver, and of an eutectic alloy (Ag-28Cu).…”

Section: Introductionmentioning

confidence: 99%

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Toward New High Temperature Reference Materials for Calorimetry and Thermal Analysis

Razouk

Hay

Himbert

2014

EPJ Web of Conferences

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Abstract. The French National Metrology Laboratory LNE-LCM has developed a high temperature reference facility for accurate measurements of the specific heat capacity and of the enthalpy of fusion of materials over the temperature range [23 °C, 1000 °C]. The metrological approach was to modify a commercial Calvet calorimeter in order to lower the uncertainty of measurement and to insure the metrological traceability of the measurements to the SI units, in particular by designing a new calibration system. The enthalpies of fusion of pure metals (indium, tin and silver) and of a binary alloy Ag-28Cu have been measured. The results obtained on the three pure metallic materials are in very good agreement with data obtained by other National Metrology Institutes (NMIs) using adiabatic calorimetry.

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“…Sensitivities from 2.8 µV mW −1 (Setaram HT1000, operation temperature from room temperature to 1000 • C) (Razouk et al, 2013), through 15 µV mW −1 (proprietary instrument with an operating temperature between −73 and 317 • C) (Handy et al, 1993), to 30 µV mW −1 (Setaram C80, operation temperature up to 300 • C) (SETARAM Instrumentation, 2016) can be reached. These data, however, indicate that for TianCalvet calorimeters the maximum operation temperature and the sensitivity behave inversely.…”

Section: The Tian-calvet Calorimeter and Its Special Featuresmentioning

confidence: 99%

First steps to develop a sensor for a Tian–Calvet calorimeter with increased sensitivity

Schubert

Gollner²,

Kita

et al. 2016

J. Sens. Sens. Syst.

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Abstract. Initial steps to apply a ceramic multi-layer technique to build a new sensor for a Tian-Calvet calorimeter are presented in this contribution. The new sensor has a stacked design of ceramic sensor discs and insulating rings. The development was finite-element method (FEM) supported to design the sensor disc. In the next step, the function of the sensor disc was proven up to a temperature of 600 • C. Finally, the entire stack was tested at room temperature, delivering a resolution of 5 µW and a maximum sensitivity of 8.5 µV mW −1 . The time constant is strongly dependent on the mass of the cuvette. We show that the time constant of the sensor can be more exactly characterized when using a novel low temperature co-fired ceramic (LTCC) cuvette with a low mass and an integrated heater. Then, the time constant can be reduced to T 1/e = 118 s. The new sensor shows similar specifications as commercial devices and presents a good starting point for future high temperature applications.

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A new in situ electrical calibration system for high temperature Calvet calorimeters

Cited by 14 publications

References 13 publications

Qualification d’un calorimètre à flux pour la caractérisation de matériaux de référence en enthalpie de fusion jusqu’à 1 000 °C

Qualification d’un calorimètre à flux pour la caractérisation de matériaux de référence en enthalpie de fusion jusqu’à 1 000 °C

Toward New High Temperature Reference Materials for Calorimetry and Thermal Analysis

First steps to develop a sensor for a Tian–Calvet calorimeter with increased sensitivity

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