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High-temperature high-pressure calorimeter for studying gram-scale heterogeneous chemical reactions

  • B. P. MacLeod
  • P. A. Schauer
  • K. Hu
  • B. Lam
  • D. K. Fork
  • C. P. Berlinguette
Reviews of Scientific Instruments, vol. 88 (2017), pp. 084101

Abstract

We present an instrument for measuring pressure changes and heat flows of physical and chemical processes occurring in gram-scale solid samples under high pressures of reactive gases. Operation is demonstrated at 1232 °C under 33 bars of pure hydrogen. Calorimetric heat flow is inferred using a grey-box non-linear lumped-element heat transfer model of the instrument. Using an electrical calibration heater to deliver 900 J/1 W pulses at the sample position, we demonstrate a dynamic calorimetric power resolution of 50 mW when an 80-s moving average is applied to the signal. Integration of the power signal showed that the 900 J pulse energy could be measured with an average accuracy of 6.35% or better over the temperature range 150-1100 °C. This instrument is appropriate for the study of high-temperature metal hydride materials for thermochemical energy storage.

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