Characteristics of surface runoff from a 0.14-km2 urban catchment with separated sewer in Macau was investigated. Water quality measurements of surface runoff were carried out on five rainfall events during the period of August to November, 2005. Water quality parameters such as pH, turbidity, TSS, COD, TN, Zn, Pb, and Cu were analyzed. The results show that TN and COD are the major pollutants from surface runoff with mean concentration of 8.5 and 201.4 mg/L, both over 4-fold higher compared to the Class V surface water quality standard developed by China SEPA. Event mean concentration (EMC) for major pollutants showed considerable variations between rainfall events. The largest rainfall event with the longest length of antecedent dry weather period (ADWP) produced the highest EMC of TN, TSS and COD. From the pollutographs analysis, the peak concentration of TN precedes the peak runoff flow rate for all three rainfall events. The tendency of the concentration of TSS, turbidity and COD changing with runoff flow varies between rainfall events. The relationship between TSS and other parameters were analyzed to evaluate the efficiency of the physical treatment process to control the surface runoff in the urban catchment. Based on the correlation of parameters with TSS, high treatment efficiency of TSS, TN and COD was expected. The most significant event in term of first flush is the one with the strongest rainfall intensity and longest length of ADWP. TN always showed first flush phenomenon in all three rainfall events, which suggested that the surface runoff in the early stage of surface runoff should be dealt with for controlling TN losses during rainfall events. © 2007 The Research Centre for Eco-Environmental Sciences, Chinese Academy of Sciences.