Metal-organic framework MIL-53(Al) pellets were tested for the selective adsorption and separation of xylene isomers, in liquid phase and using n-heptane as eluent. The objective of this work is to assess relevant data for a posterior xylene isomers separation process design. In order to complete this study, single and multi-component breakthrough experiments were performed at 313 K, in the presence of n-heptane. MIL-53(Al) presented a preference for o-xylene over m-xylene and p-xylene in all experiments. The selectivities of 2.0 were obtained for o-xylene over m-xylene and over p-xylene. It is concluded that MIL-53(Al) may be used for separating o-xylene from the other xylene isomers, using n-heptane as desorbent. Supplemental materials are available for this article. Go to the publisher's online edition of Separation Science & Technology to view the free supplemental file.