High-resolution mass spectrometry (HRMS) is an analytical technique that is typically used by mass spectrometry experts. However, with recent advancements, it is becoming more accessible to students in organic chemistry laboratories. Still, a significant knowledge gap exists between these experts and students. A straightforward laboratory experiment in HRMS is crucial to bridging this gap. This experiment outlines key steps for understanding HRMS, including defining the resolution, estimating the molecular formulas using accurate mass, understanding the calibration, selecting the appropriate ionization methods and calibration compounds, and validating the results. Following these steps will enable students to better grasp HRMS and effectively use it in their research.