Evaluating phase separation, which encompasses separation time, emulsion formation, and phase split quality, is typically a dynamic process requiring visual comparison over a timescale. As such, imaging tools have been employed to classify liquidliquid biphasic separation. Some researchers have determined the phase separation by monitoring the position of a colored float. However, this approach may be prone to issues related to chemical incompatibility of the float with particular solvent combinations, or variations in float buoyancy over a wide range of solution concentrations. Non-invasive edge detection has been used to determine biphasic separation but can fail when the solutions become colored or turbid. Recently, robust high throughput image analysis algorithms have been developed to specifically automate LLE workflow. Our CV model's multiparameter approach can be used to extract quantitative and qualitative features from multiple layers in a LLE system, distinguishing between homogeneous and heterogeneous regions, and accurately measuring the volume of each layer over time, as shown in Figure . This provides critical process information such as separation time, agitation effectiveness for phase mixing, and phase split quality. 1 -3 A well-agitated mixture of immiscible liquids comprising a specific volume of water (20 mL), brine (5 mL), and DCM (35 mL) containing citric acid, was automatically monitored to observe changes in the volume of each phase as agitation was halted, as shown in Figure . The effect of a 1000 rpm stir rate on the time required for the mixture to reach full separation was investigated. The separation time of 0.18 min was primarily determined based on the volume parameter of each phase, which was further supported by other secondary parameters, including color and turbidity (refer to the SI for detailed information). In comparison to mechanical or densitybased colored sensors commonly used for image analysis in LLE, our non-invasive approach can accommodate various chemical compositions. A more challenging example was realized by applying our liquid ̶ liquid extraction protocol to monitor a salt break and purification of enantiopure tetrabenazine (TBZ) as its aminefree base. This workflow is a critical intermediate step in the synthesis of Valbenazine drug , and follows a crystallizationinduced asymmetric transformation (CIAT) to convert racemic TBZ to the desired enantiomer, which is isolated as the pure (-)TBZ(-)CSA salt. Advancing the synthesis requires charging a reactor with isolated crystals, suspension in a mixture of DCM and water while charging sodium hydroxide to neutralize the acid, then recovery of the free amine from the organic layer, as shown in Figure . However, this seemingly simple procedure raises several challenges. To optimize the process mass intensity (PMI) of the overall route a minimum volume of working solvents is desired, forcing the extraction to operate at a very high concentration. The amphiphilic nature of both camphorsulfonic acid and TBZ increases the micelle forming potential of the solvents and promotes emulsion. Reducing the agitation can partially mitigate this effect but compromises efficient mass transfer leading to very long processing times. Thus, we need to identify the highest possible agitation rate that still allows facile phase separation without creating an emulsion and effectively neutralize the acid.