This paper proposed a comprehensive analysis chemical experiment. The experiment contents including preparation of fluorescent copper nanoclusters, fluorescent spectroscopic characterization, and hydrogen peroxide detection based on fluorometry. This experiment can not only make students understand the fluorescent metal nanoclusters and monitoring methods of hydrogen peroxide, but also allow students to learn operation methods and fundamental principles of magnetic stirring, darkbox type ultraviolet analyzer, lab-dancer and fluorescence spectrophotometer. Moreover, this experiment will make students establish an academic idea of optimizing experimental conditions and comprehensively analyzing problems, which is helpful for cultivating students' comprehensive innovation capability.