Abstract
A new generation isothermal multichannel microcalorimetry system based on an earlier reported system which has been commercialised under the name “Thermal Activity Monitor” (TAM) is described and evaluated. The system has a modular design constituting a thermostat that accommodates up to four calorimetric units. The temperature stability of the thermostat has been improved 100-fold compared to the original TAM mainly due to novel technology for absolute temperature measurements consisting of a platinum resistance sensor combined with a high-resolution thermoelectric (TE) module housed in an aluminium body for temperature fluctuation measurements. In combination with the continuous liquid overflow design similar to that of the original TAM with an inbuilt Peltier cooling/heating system forming part of a single feedback regulation system, temperature drifts/fluctuations over 24 h better than ±10 µK have been achieved. Besides the isothermal mode, the thermostat can be controlled to perform temperature ramps with rates from close to 0 up to 2 K h−1. Two basic designs of twin heat flow calorimeters are described. One is similar to those originally reported having the sample and reference sides mirrored horizontally, and with a solid heat sink time constant of 6000 s. The other has the sample and reference mirrored on the vertical axis with a solid heat sink time constant of 500 s making it considerably smaller. Both calorimeters are equipped with insertion ampoule holders that can hold 4 mL reaction volume. The lowest observed long-term signal stability among a population of data from the two calorimeters was ±17 nW/24 h for the calorimeter with the larger heat sink and ±50 nW/24 h for the calorimeter with the smaller heat sink. Test experiments indicated the absence of significant systematic errors for the former calorimeter type while a maximum of 2–3% error was observed for the latter type. This difference between the two calorimeter types was attributed to different positioning of the TE sensors relative to the calibration heater.
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Acknowledgement
The authors wish to thank Bo Lundberg for the electronics design, Eugen Schwarts for contributions to the mechanical design and Andreas Suurkuusk and Niclas Thisell for the development of the TAM Assistant software.
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Suurkuusk, J., Suurkuusk, M. & Vikegard, P. A multichannel microcalorimetric system. J Therm Anal Calorim 131, 1949–1966 (2018). https://doi.org/10.1007/s10973-017-6684-7
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DOI: https://doi.org/10.1007/s10973-017-6684-7