Calorimeter with reflux-condenser

Use of medium-scale heat flow calorimeter for separate measurement of reaction heat removed via reaction vessel walls and via reflux condenser system, under fully realistic processing conditions, with data processing of the results is reported [2], More details are given elsewhere [3], A new computer controlled reaction calorimeter is described which has been developed for the laboratory study of all process aspects on 0.5-2 1 scale. It provides precise data on reaction kinetics, thermochemistry, and heat transfer. Its features are exemplified by a study of the (exothermic) nitration of benzaldehyde [4], A more recent review of reaction safety calorimetry gives some comment on possibly deceptive results. [5],... 

Alternatively the reaction calorimeter can be fitted with a reflux condenser, ora modified Soxhlet assembly can be used. Both of these approaches are described below. It is difficult to obtain accurate calorimetric data with such reflux calorimeters if ... 

A reflux condenser (condenser-kettle embedded in an intermediate thermostat) within a base thermostat is combined via a thermally insulated pipe with the measuring kettle of a calorimeter for a discontinuous reaction (Fig. 2.35). Provided that in the measuring kettle evaporable components are generated by a not-too-fast chemical conversion, between the measuring kettle and the condenser there exists with regard to the evaporable components a quasi-continual equilibrium. ... 

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