Measuring Kinetics in Flow Using Isoperibolic Flow Calorimetry

Abstract

Continuous flow calorimeters are a promising tool in process development and safety engineering, particularly for flow chemistry applications. An isoperibolic flow calorimeter is presented for the characterization of exothermic reactions. The calorimeter is adapted to commercially available plate microreactors made of glass and uses Seebeck elements to quantify the heat of reaction. For automation of calibration procedures and calorimetric measurements, the device is connected to a lab automation system. Reaction enthalpy of exothermic reactions is determined via an energy balance of the entire calorimeter. Characterization of reaction kinetics is carried out via a local balancing of the individual Seebeck elements without changing the experimental setup, while using the previous measurements and additional ones at higher flow rates. The calorimeter and the associated measurement procedures were tested with the oxidation of sodium thiosulfate using hydrogen peroxide. Reaction enthalpy was determined to be 594.3 ± 0.7 kJ mol−1, which is within the range of literature values.

Keywords

• automation
• continuous flow
• compartmental modelling
• flow calorimetry
• kinetics
• microreactors