Thermochemical characteristics were determined for several National Institute of Standards and Technology standard-reference-material petroleum and biodiesel fuels, using a novel laser-heating calorimetry technique. Measurements focused on the sample thermal behavior, specific heat release rate, and total specific heat release. The experimental apparatus consists of a copper sphere-shaped reactor mounted within a chamber, along with laser-beam-steering optical components, gas-supply manifold, and a computer-controlled data-acquisition system. At the center of the reactor, liquid sample is injected onto a copper pan substrate that rests and is in contact with a fine-wire thermocouple. A second thermocouple is in contact with the inner reactor sphere surface. The reactor is heated from opposing sides by a continuous-wave, near-infrared laser to achieve nearly uniform sample temperature. The change in temperature with time (thermogram) is recorded for both thermocouples, and compared to a baseline thermogram (without liquid in the pan). The thermograms are then processed (using an equation for thermal energy conservation) for the thermochemical information of interest. The results indicated that the energy reaching the pan is dominated by radiative heat transfer processes, while the dominant thermal process for the reactor sphere is the stored (internal) thermal energy within the sphere material. Sufficient laser power is necessary to detect the fuel thermal-related characteristics, and the required power can differ from one fuel to another. With sufficient laser power, one can detect the preferential vaporization of the lighter and heavier fuel fractions. The total specific heat release obtained for the different conventional and biodiesel fuels used in this investigation were similar to the expected values available in the literature.