Abstract This paper introduced a comprehensive experiment including preparation, quantitative determination of composition and photochemical properties test of K3[Fe(C2O4)3]·3H2O by reforming traditional experiment. This comprehensive experiment was planned for 12 class hours. In the experimental operation, this experiment involved the preparation of coordination compound, vacuum filtration, crystallization by evaporation condensation, gravimetric analysis, redox titration, ion charge determination by conductivity method, etc. This experiment involved a large number of reaction types, such as precipitation, dissolution, oxidation reduction, coordination and photo induced discoloration. This experiment needed only basic experiment equipment and could be easily applied in practical teaching. Teaching practice showed that the experiment could stimulate students' initiative think, expand students' thinking span and depth, and achieved good teaching results.