We next attempted a more challenging example by coupling distillation with antisolvent crystallization, as illustrated in Figure . This workflow is closely related to solvent exchange distillation and is commonly used to isolate products at the end of a synthetic sequence. Here, the addition of the makeup solvent led to supersaturation, resulting in nucleation and crystallization as the distillation progressed. This posed a more complex visual challenge for the CV system. Once again, our primary parameter (volume) and secondary parameter (temperature) provided the main factors for reactor control and integration. Additionally, solid formation was critical to inform the onset of nucleation.