The increasing global energy demand, depletion of petroleum reserves, volatile petroleum prices, and growing environmental concerns have accelerated the search for sustainable and clean energy sources. Biodiesel (methyl ester) was produced from scum oil (MESO) and waste vegetable oil (MEWVO) through transesterification using sodium hydroxide and methanol as catalysts and reactants. The composition of the methyl esters in MESO and MEWVO was analyzed using Gas Chromatography-Mass Spectrometry (GC-MS). Various methyl ester blends were prepared by adding pure diesel to MESO and MEWVO, and the best blend was selected for use in compression ignition (CI) engines. The performance, emission, and combustion characteristics of MESO-B20 and MEWVO-B20 blends were studied. Results showed that retarded injection timing (19° before TDC) significantly reduced ignition delay by 15% and improved brake thermal efficiency (BTE) by 6.4% compared to standard injection timing. The increase in injection pressure to 220 bar enhanced fuel atomization, leading to a 10% reduction in brake specific fuel consumption (BSFC) plus 5% reduction in exhaust gas temperature (EGT). These findings demonstrate that MESO-B20 and MEWVO-B20, with optimized injection parameters, are a viable alternative to conventional diesel in CI engines, showing improved combustion efficiency and emission reductions, particularly in CO and unburned hydrocarbons (HC), although there was increase in NOx emissions.. Further research is recommended to address NOx emissions and optimize biodiesel formulations for long-term engine performance.