Citrus peel wastes were studied for bioethanol production using the H2SO4 pretreatment method and the fermentation of Saccharomyces cerevisiae. This study investigates the potential of acidic pre-treatment for 3 h at 100 °C to remove D-Limonene. The results obtained from FT-IR analysis confirmed that D-limonene was significantly decreased from 0.21% to below 0.01%. The density of the bio-ethanol produced was found to be 0.85 g/cc. The turbidity analysis results showed that there was no haze or turbidity developed. Further, the citrus peel wastes treated with 10% (v/v) of H2SO4 showed an increase in reducing sugar concentration at 42 hrs. An ethanol concentration of 70.94 % was obtained from citrus peel wastes during fermentation for 24 hrs. The results observed from the density, turbidity, and Benedict’s test confirm that a good bioethanol yield was produced by removing D-limonene through the sequential acid hydrolysis and fermentation process.