The development and operation of an automated workstation for performing solution-phase organic synthesis and on-line HPLC analysis is described. A wide scope of applications and chemistries, typically encountered in process development laboratories, are reported. The application of this workstation to process screening and optimisation studies coupled with statistical design of experiments (DOE) is illustrated using three simple case studies. The utility of this approach in accelerating core aspects of process research and development by performing multiple experiments in parallel and generating quality data more efficiently has been explored.