The paper presents the experimental study of a novel unsteady-statemembrane gas separation approach for recovery of a slow-permeant component in the membrane module with periodical retentate withdrawals. The case study consisted in the separation of binary test mixtures based on the fast-permeant main component (N2O, C2H2) and the slow-permeant impurity (1%vol. of N2) using a radial countercurrent membrane module. The novel semi-batch withdrawal technique was shown to intensify the separation process and provide up to 40% increase in separation efficiency compared to a steady-state operation of the same productivity.