The aim of this study is to investigate the extraction of oil from scum obtained from a municipal wastewater treatment plant. Various parameters such as solvent volume, temperature, agitation and moisture content were optimized to maximize the oil extraction efficiency using freeze-dried scum. The oil extraction efficiency was compared for each parameter using hexane and petroleum diesel as a solvent. The optimum physical parameters for oil extraction using freeze-dried scum were 75 g solids/L solvent, temperature 60 C, agitation 300 rpm for 60 min, and maximum oil extraction efficiency of 100 and 94.3% w/w was obtained using hexane and petroleum diesel, respectively. The obtained results using 1 g of scum were further validated using 1 kg of wet scum under optimized conditions, and oil extraction efficiency of 94.1 ± 1.3 and 91.3 ± 4.2% w/w was obtained using hexane and petroleum diesel, respectively. Furthermore, ex situ transesterification was performed, and results showed that scum had a higher neutral lipid. In brief, scum is a potential feedstock for the production of biodiesel, and more work on this must be done in future.