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Distillation is a ubiquitous method of separating liquid mixtures based on differences in volatility. Performing such separations in microfluidic systems is difficult because interfacial forces dominate over gravitational forces. We describe distillation in microchemical systems and present an integrated silicon device capable of separating liquid mixtures based on boiling point differences. Microfluidic distillation is realized by establishing vapor–liquid equilibrium during segmented flow. Enriched vapor in equilibrium with liquid is then separated using capillary forces, and thus enabling a single-stage distillation operation. Design criteria for operation of on-chip distillation is set forth, and the working principle demonstrated by separation of binary mixtures of 50 : 50 mol% MeOH–toluene and 50 : 50 mol% DCM–toluene at 70.0 °C. Analysis of vapor condensate and liquid exiting a single-stage device gave MeOH mole fractions of 0.22 ± 0.03 (liquid) and 0.79 ± 0.06 (vapor). Similarly, DCM mole fractions were estimated to be 0.16 ± 0.07 (liquid) and 0.63 ± 0.05 (vapor). These experimental results were consistent with phase equilibrium predictions.
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