Separation of organic-organic liquid mixtures using membranes has been investigated extensively over the past several decades due to its great significance in the chemical industry, Aromatic-alkane, alkane alkene and aromatics removal from gasoline systems among the most studied. These compounds are often present at very low concentrations in the mixtures and their recovery with traditional techniques, such as distillation and partial condensation, are not very simple. Pervaporation (PV) has been considered as one of the most active and promising areas in membrane technologies. In PV, the membrane itself is the key Polyvinyl chloride (PVC)-based mixed matrix membranes were prepared with LDH layered double hydroxide (NiFeCO 3 ) particles, and were studied for the separation of toluene-heptane mixtures. It was found that the PVC transport properties could be significantly modified by the amount of NiFeCO 3 incorporated. NiFeCO 3 /PVC membranes were characterized by IR FT spectroscopy and ATG.