Utilizing an automated laboratory reaction calorimeter, an energetic reaction was investigated to determine feasible pilot plant operating conditions. The calorimetric data led to kinetic parameters and a predictive heat flow model which allowed simulations of the required pilot plant jacket temperature profiles. On the basis of these profiles, several feasible and safe operating conditions were determined. This study demonstrates the power of calorimetry as it relates to process design and scale-up of batch and semibatch processes.