Investigation techniques for fire prevention in low-temperature warehouses were studied using energy dispersive X-ray fluorescence (ED-XRF). In the first experiment, a sample (galvanized steel sheet plus urethane foam plus sandwich panel) was burned with 500 mL of a flammable liquid (gasoline, thinner, kerosene, and light oil)/ Then, the component change of the sample was measured. In the combustion experiment, there was a difference in the heat of combustion depending on the type of flammable liquid; however, as a result of measuring the component change of the sample with ED-XRF after combustion, the largest component change was measured in the combustion experiment with gasoline. The change was in the order of thinner, kerosene, and diesel. Using ED-XRF, it was possible to distinguish the flammable liquid used in the experiment by measuring the component change of the sample resulting from the difference in the combustion heat of the flammable liquid. A second experiment was conducted under the same conditions as the first experiment, assuming a fire brigade fire suppression condition, and the combustion time of the flammable liquid was limited to 600 s. A combustion characteristic of flammable liquids is that the temperature and heat flux reach the maximum value within 300 s after the start of combustion regardless of the type of liquid. Because the change of composition was confirmed in the order of light oil, it was possible to distinguish the flammable liquid used at the fire site using the ED-XRF measurement result.