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Due to the rapid development of electronic devices and their shortened lifespans, waste electrical and electronic equipment (WEEE), or E-waste, is regarded as one of the most fast-growing wastes. Among the categories of E-waste, waste printed circuit boards (WPCBs) are considered the most complex waste materials, owing to their various constitutes, such as plastics, capacitors, wiring, and metal plating. To date, a variety of processing technologies have been developed and studied. However, due to the heterogeneous nature of WPCBs, a thorough study on both material characterization and physical separation was needed to provide a better understanding in material handling, as well as to prepare a suitable feedstock prior to the downstream chemical process. In the present study, integrated size and density separations were performed to understand the liberation of contained metals, particularly Cu and Au, from the plastic substrates. The separation performance was evaluated by the elemental concentration, distribution, and enrichment ratio of valuable metals in different size and density fractions. Further, SEM-EDS on the density separation products was carried out to characterize the surface morphology, elemental mapping, and quantified elemental contents. Moreover, thermo-gravimetric properties of waste PCBs were investigated by TGA, in order to understand the effect of temperature on volatile and combustible fractions during the thermal processing.