The rapid academic and industrial development of nanotechnology has led to its implementation in laboratory teaching for undergraduate-level chemistry and engineering students. This laboratory experiment introduces the galvanic replacement reaction for synthesis of hollow metal nanoparticles and investigates the optical properties of these nanoparticles. Changes of localized surface plasmon resonance from solid to hollow nanoparticles are monitored by UV-vis spectroscopy, while corresponding morphological changes are validated by transmission electron microscopy. The optical properties are further investigated by the use of a laser pointer, laser irradiation, and surface-enhanced Raman spectroscopy. By performing these experiments, students gain practical knowledge for the synthesis of hollow metal nanoparticles and the underlying structure-dependent optical properties.