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Reference material for temperature calibration of differential scanning calorimeters above 1400 °C

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Abstract

Platinum crucible pans are widely used for differential scanning calorimetry (DSC) at temperatures above the aluminum melting point (about 660 °C) due to good signal quality, chemical inertness and easiness of cleaning. However, reference materials commonly used for the calibration of DSC equipment operating with platinum pans exhibit phase transition temperatures no higher than about 1000 °C. In this work, the solid–solid, reversible, \(\alpha ^{\prime }_{\mathrm{H}}\rightarrow \alpha\) phase transition of calcio-olivine, \(\hbox {Ca}_{2}\hbox {SiO}_{4},\) was found to produce a marked DSC peak with an onset temperature of \(1453^{+1}_{-2}\,^{\circ }\hbox {C}\) and a relatively small hysteresis. This compound is compatible with platinum crucibles and fulfills the requirements to be used as reference material for high-temperature calibration of differential scanning calorimeters.

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Acknowledgements

Authors acknowledge financial support from the Brazilian agencies CNPq (Conselho Nacional de Desenvolvimento Científico e Tecnológico), through the “Pesquisador Visitante Especial” initiative—Grant No. 408677/2013-9, as well as research Grant Nos. 304831/2014-0 (CAP) and 304675/2015-6 (JEZ), Inmetro (Instituto Nacional de Metrologia, Qualidade e Tecnologia) and Capes (Coordenação de Aperfeiçoamento de Pessoal de Nível Superior), through the Rede de Laboratórios Associados ao Inmetro para Inovação e Competitividade (RELAI) initiative, and SDECT (Secretaria do Desenvolvimento Econômico, Ciência e Tecnologia do Estado do Rio Grande do Sul). Thanks are due also to Netzsch Gerätebau GmbH, Cynthia M. Gomes (formerly at Bundesanstalt für Materialforschung und prüfung—BAM, Germany), Alessandro Dalponte for his collaboration in the early stages of this work, and the IMC staff, mainly D. Golle for helping us with the many thermal analysis experiments and R. C. D. Cruz for insightful discussions.

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Authors and Affiliations

  1. Instituto de Materiais Cerâmicos, Universidade de Caxias do Sul, Bom Princípio, RS, 95765-000, Brazil

    J. E. Zorzi & C. A. Perottoni

  2. Departamento de Engenharia de Materiais e Cerâmica (CICECO), Universidade de Aveiro, 3810-193, Aveiro, Portugal

    A. M. Segadães

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  1. J. E. Zorzi
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Zorzi, J.E., Segadães, A.M. & Perottoni, C.A. Reference material for temperature calibration of differential scanning calorimeters above 1400 °C. J Therm Anal Calorim 128, 1547–1554 (2017). https://doi.org/10.1007/s10973-016-6048-8

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