Abstract: In this comprehensive experiment, bandgap structures were determined by cyclic voltammetry and UV-Vis absorption spectroscopy. Firstly, the cyclic voltammetry curves of ferrocene and tris (8-hydroxyquinoline) aluminum were measured using electrochemical workstation. Secondly, the UV-Vis absorption spectrum of tris (8-hydroxyquinoline) aluminum was determined by UV-Vis spectrophotometer. Highest occupied molecular orbital (HOMO), lowest unoccupied molecular orbital (LUMO) and bandgap values of organic molecules were calculated according to cyclic voltammetry curves and UV-Vis absorption spectrum. The results of the former (3.07 eV) were basically in accordance with that of the latter (2.80 eV), and the deviation was in the permissive range. Applying traditional testing methods to the experimental teaching content regarding the energy band structure of organic molecules not only consolidates students’ basic knowledge, but also deepens their understanding of electrochemical redox process and absorption process.