A novel pre-treatment process for the liberation of metals from waste printed circuit boards(PCBs) by layer separation has been developed. The invention particularly relates to the liberation of metallic constituents by the separation of the layers of metallic and non-metallic components from the PCBs. The novelty of the process is the liberation of metal from the PCBs using organic, which is effective, economical and energy saving. In present study, the pieces of PCBs are tested for the separation of the layers of epoxy resins and other non-metallic constituents from the thin metallic plates and wires. The process is compatible in comparison to existing mechanical pre-treatment process. The separated thin metal plates and wire could be effectively processed for the hydrometallurgical extraction, in comparison to the metallic fraction coated or encapsulated with plastic and ceramic material. The mixture of liberated resins and metals from the PCBs were filtered, then dried to remove all liquid. The mixture of liberated thin layers of metals and epoxy resins are finally separated and analysed by using corona electrostatic separator. The recovery of metal was found 99.99%.