The subject of previous work on liquid‐liquid extraction is complemented in this paper through the research activities in micro distillation. After a detailed literature study comparing the performance, strengths, and weaknesses of published micro distillation methods, critical process parameters based on model studies will be discussed. Apparative approaches to micro distillation are presented, where the capillary module used for distillation can provide a successful phase separation of gas‐liquid mixtures up to volume feeds of 10 mL min−1.