For the thermal desorption of low-volatility compounds, rapid heating followed by instant cooling is desirable to suppress thermal decomposition. In this work, a new thermal desorption method, heat pulse desorption (HPD), was developed. A heated N2 gas pulse (350 °C, 50 ms) was directed to the solid sample surface, and desorbed analytes were ionized by DC corona discharge and mass analyzed by an Orbitrap mass spectrometer. Because heat transfer from the heated N2 gas to the solid surface is not very efficient, desorption of the solid sample occurs at a certain temperature before reaching 350 °C. In short, there is a self-controlling desorption depending on the volatility of each analyte. Because the exit of the copper tube for gas blowing is separated from the sample surface, no carryover occurs, enabling the repetitive analysis of samples. HPD was applied to various compounds such as narcotics, pharmaceutical tablets, and explosives. Because analysis is completed within a few seconds per sample, this method is highly useful for quick and consecutive analysis of real samples, having potential utility in food quality control, counterfeit drugs analysis, and the detection of explosives for safety and security.