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The paper presents an investigation of the enhancement of hydrocarbon extraction from calotropis procera. An extraction yield of 8% has been obtained, with toluene as the solvent. An increase in the extraction yield to 11.5% has been achieved by modification of the design of the conventional 'Soxhlet' extractor. A further enhancement in extraction has been achieved by pretreatment of the biomass with alkali or acid. This pretreatment results in an extractive or hydrolytic breakdown of the plant structure and hence exposes the hydrocarbons to solvent attack. As alkali pretreatment of ground biomass resulted in a much higher extraction, it was studied in further detail with more alkalis of varying strength. An enhancement from 8 to 18% has been achieved by pretreatment with 1 N sodium hydroxide. Analytical studies by the use of IR and NMR have been conducted to prove that the enhancement in extraction is due to efficient extraction of hydrocarbons.