Waste generation and management is a priority issue for most of the EU countries and policies are being developed to overcome existing obstacles. Of these, plastic wastes have an immense impact on the environment because of their non-biodegradability in the long terms; therefore, recycling is mandatory for their management Segregation of different types of plastics is an important process in waste recycling. There is no significant specific gravity difference between plastics making separation gravity methods inapplicable. On the other hand, methods evaluating the changes in surface chemistry features provide effective and cost beneficent solutions for separation of PET and PVC. Of these, flotation method comes into prominence to separate these materials having similar hydrophobic properties by changing physicochemical properties for either PET or PVC to hydrophilic by using plasticiser reagents for selective flotation of PET and PVC. In this research, lab and pilot scale flotation columns were used in order to determine the best flotation parameters for selective separation of PET and PVC. In evaluation of optimum conditions, it is found that PET can be floated with 95.6% purity and 92.3% recovery and the product remaining in the flotation cell (PVC particles) can be discarded as another product with 99.4% purity.