A new operation policy-quasi-batch distillation for recovering infinitesimal amounts species existing in a mixture is presented. In quasi-batch distillation operation, feed is introduced with a constant flow rate onto the feed stage of the column, and the flow rate of the distillate is the same as that of the feed, whereas the bottom product is withdrawn periodically. The behavior of quasi-batch distillation is simulated and analyzed through an example on heavy water separation. Comparing with continuous or batch distillation, the new operation policy is more reliable and efficient to achieve higher recovery of dilute component. This is especially suitable for separating small amount of precious species from large amount of raw material.