The synthesis of operating procedures for the transient operation of chemical processes is a formidable and expensive task during the design of a plant. It is time-consuming and error-prone both for the process engineering department to specify the procedures and for the automation department to generate sequence control code from the specifications. A further source of error arises at the interface between the two departments since the boundary is typically ill-defined and engineers of different backgrounds often make assumptions without adequate understanding of the other discipline. In this paper, we describe the application of the CAPS (computer-aided procedure synthesis) system (Crooks et al., 1992a,b,c) to a case study in the nuclear industry - British Nuclear Fuels’ (BNFL) Thermal Oxide Reprocessing Plant (THORP), which will be the largest facility in the world for reprocessing spent reactor fuel pins. The case study considers the "head end" plant of THORP which involves reagent preparation and fuel pin dissolution and is a single product batch and semi-continuous process. The CAPS system successfully generated realistic supervisory procedures and control sequence specifications which were in close agreement with the actual control sequences developed by BNFL engineers. Furthermore, the modelling effort required as input to CAPS was reasonable and all of the information was readily available early in the design life cycle.