A fuel heat of vaporization (Delta H-vap) is a fundamental thermodynamic property and an important parameter for internal combustion engine design. The Delta H-vap value is measured with a newly developed vacuum thermogravimetric analysis (VTGA) method. The technique is applicable to jet and diesel range fuels. The measured values for the selected components in the fuels agree with the literature values within a range of +/-5%. VTGA is a quick, cost-effective, and accurate method to measure the Delta H-vap of renewable fuels. The Delta H-vap values for binary mixtures of fuels can be simply estimated from the Delta H-vap values and mix ratio of the parents.