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Thermal gradients in differential scanning calorimetry

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Abstract

A combined static and dynamic temperature calibration is described. The static calibration corrects the instrumental dial temperature reading. The dynamic calibration has instrumental and material components and therefore varies from specimen to specimen. It is obtained from individual DSC curves and so removes uncertainties in sample temperature due to varying mass, geometry, and heating rate. The instrumental performance is improved and specific heats may be obtained to an accuracy of ±1%.

Résumé

On décrit un mode d'étalonnage de la température pour les essais statiques et dynamiques. L'étalonnage statique permet de corriger la valeur de la température lue sur le cadran de l'instrument. L'étalonnage dynamique varie avec les échantillons étudiés car il utilise des accessoires instrumentaux et des matériaux adapté aux études particulières. Il est fourni par des enregistrements individuels qui éliminent les incertitudes dues aux variations de masse, de géométrie et de vitesse de chauffage. Les caractéristiques instrumentales sont ainsi améliorées et les chaleurs spécifiques peuvent être obtenues avec une exactitude de ±1 P.c.

Zusammenfassung

Eine kombinierte statische und dynamische Temperatureichung wird beschrieben. Die statische Eichung korrigiert die Temperaturablesung an der Instrumentenscheibe. Die dynamische Eichung besteht aus instrumentellen und Stoff-Komponenten und ist deshalb in verschiedenen Fällen unterschiedlich. Sie wird aus individuellen DSC Kurven erhalten und beseitigt somit Unsicherheiten der Temperatur des Musters, welche durch Änderungen der Masse, der Geometrie und der Aufheizungsgeschwindigkeit bedingt sind. Die Leistung des Instrumentes kann erhöht werden und die Bestimmung spezifischer Wärmen ist mit einer Genauigkeit von ±1 % möglich.

Резюме

Описана комбинирова нная статическая и динамическая калибр овка температуры. Статическая калибро вка вносит поправку в чтение температуры по шкале прибораДинамическа я калибровка включает приборный и материал ьный компоненты и поэтому изменяется в зависим ости от образца. Она пр оведена на основе индивидуальн ых термических кривых и, следователь но, устраняет колебан ия в температуре образца, обусловленные изменениями массы, ге ометрии и скорости на грева. Инструментальное вы полнение улучшено и удельную т еплоемкость можно оп ределятьс точностью до ±1%.

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Abbreviations

T i,T f :

steady initial and final temperatures, respectively, in a calorimetric experiment

gDT=Tf-Ti; TD :

dial temperature reading;

T :

true temperature corresponding toT D after all corrections have been made

T m :

melting point;

δT s :

correction toT D to giveT under isothermal, ‘static’ conditions;

δT (=δT 0+δT mat):

additional correction toT D, due to thermal lag, to giveT under programmed temperature conditions;

δT 0,δT mat :

contributions to δT originating in the instrument and sample material respectively

δT d (=δT s +δT) :

total correction toT D to giveT under programmed temperature conditions

R :

calorimeter heating rate

H(T i),H(T f):

enthalpy atT i andT f respectively

¯c p :

mean heat capacity over the temperature rangeT i toT f

c p, Tf :

heat capacity atT f

References

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Authors and Affiliations

  1. Division of Materials Applications, National Physical Laboratory, Teddington, Middlesex, UK

    M. J. Richardson & P. Burrington

Authors
  1. M. J. Richardson
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  2. P. Burrington
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Richardson, M.J., Burrington, P. Thermal gradients in differential scanning calorimetry. Journal of Thermal Analysis 6, 345–354 (1974). https://doi.org/10.1007/BF01950065

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  • DOI: https://doi.org/10.1007/BF01950065

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