We describe the variation of structural and physical properties of mesocarbon microbeads, a potential anode material for rechargeable lithium batteries, as a function of heat-treatment temperature in the range 400–1100 °C. Scanning electron microscopy (SEM) studies indicated changes in the morphology of the mesocarbons with heat treatment. X-ray studies show that average crystallite size varies considerably with heat treatment. The d002 spacing decreases with increasing heat-treatment temperatures. The electronic conductivity of the mesocarbon microbeads also increases substantially with increasing heat-treatment temperature. Based on thermogravimetric analysis (TGA) and other measurements, we find that organic fractions volatilizes out of these carbons in two distinct stages. The observed weight loss correlates with the structural changes observed. We suggest that these observations are consistent with two types of hydrogenated fractions present in the “green” mesocarbons.