To investigate the run-off characteristics of dissolved and particulate substances from a heavily urbanized area (basin area: 95 ha, percentage of impervious surfaces: 60%), sensors for measuring water level, water temperature, DO, pH, electric conductivity (EC), turbidity and ammonium ion were placed in the channel connecting storm sewers and natural river, together with water sampling for analyzing SS, nutrients and metals. While both turbidity and EC showed apparent "first flush", the peaks of EC were always earlier than those of turbidity. In a similar manner, dissolved nutrients and metals exhibited earlier "first flush" compared with particulate nutrients and acid-extractable metals. Significantly positive correlations between EC and dissolved substances as well as those between turbidity and particulate (acid-extractable minus dissolved) substances were usually observed, and two distinct different regressions were found between the two datasets separated before and after the concentration peaks. Using these relationships, the total loads during the respective rainfall events were calculated on the basis of EC and turbidity changes. The total loads of nitrogen, zinc, etc. were nearly proportional to the lengths of non-rainfall periods before the events, indicating that these loads derived from the atmospheric deposition.