Employing floating static chamber-chromatography method, the N2O diurnal fluxes at the water-air interface of four rivers (Tuanjie River, Jinchuan River, Inner and Outer Qinhuai River) and Jinniu Lake were monitored in Nanjing during summer. The results show that four rivers act as the sources of N2O emission, but Jinniu Lake is characterized by the absorption of N2O. The highest N2O flux from Inner Qinhuai presented at 20:00 because of the changing of hydrodynamic conditions. Both Jinchuan and Tuanjie rivers' minimum N2O fluxes were detected when the content of dissolved oxygen was extremely low. The tendency of N2O from Outer Qinhuai showed a double-peak because of its daytime nitrification and nocturnal denitrification. The flux of N2O from Jinniu Lake had been noted as being generally higher at night than that during light hours due to the effect of wind. For natural rivers, the proper sampling period is from 08:00 to 12:00, but for the river subjected to interference, the sampling period is different.