Abstract: In the design, the linear sweep voltammetry (LSV) is carried to investigate the catalytic performance of Co/N/C in acid system using rotating disk electrode (RDE). The electron transfer number is calculated and the catalytic mechanism of catalysts is evaluated. Though this experiment, students will learn the preparation method of Co/N/C oxygen reduction reaction (ORR) catalysts and comprehend the catalytic mechanism and principle of RED. This experiment is suitable for undergraduate experimental teaching of comprehensive or instrumental analysis experiment for applied chemistry specialty.