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We developed a new prototype reaction calorimeter with an integrated infrared−attenuated total reflection (IR−ATR) probe that has a sample volume of 45 mL and uses a metal block as an intermediate thermostat. Isothermal conditions are maintained using the power compensation principle. An additional heat balance using Peltier elements is implemented to compensate for changes of the reactor-sided heat-transfer coefficient and to circumvent corresponding calibration steps. The new calorimeter has been tested using the neutralization of NaOH with H2SO4 and the hydrolysis of acetic anhydride. These experiments showed the precision of the new calorimeter and its capability to deal with fast and highly exo- or endothermic reactions. The kinetic parameters obtained from the IR and calorimetric measurements agree well with each other and with literature values. Even for the investigated simple reaction schemes, the IR−ATR probe provided additional information from what is obtained from the calorimetric signal alone.
Zogg et al. (Wed,) studied this question.
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