A simple and rapid analytical method was developed for the determination of the anionic surfactants (AS) in the study of environmental geochemistry of the estuary. The sediments were analysed by the extraction-spectrophotometry with ethyl violet and the indirect atomic absorption methods, the sea-water was analysed by indirect atomic absorption method. In estuary water the AS are less stable and enriched in the particles, but stable in sediments. The average concentration of AS in inner Beitang and Dagu outfalls is 20--150 times more than that in the inshore area. The heighest value is about 2 mg/L. The regional distribution patterns of AS in surficial sea-water and surficial sediments reflect that Dagu and Beitang outfalls are its main contributors. And the pollution in Dagu outfall is stronger than that in Beitang. It also reflects the transport- sedimentary trend of the suspended pollutants. In water, the correlation between concentrations of AS and the salinity, the diversity of phytoplankton is negative, while that between concentrations of AS and COD, BOD, nitrogen, phosphorus, coliform bacteria as well as chlorophyll-a is positive. In sediments, the correlation between the concentrations of AS and organic C, humic acid, sulphide, phosphorus as well as nitrogen is distinctively positive. However, the relation between AS and ignition loss is not clear. Thus, it is possible that the AS can be used as a indicator of organic pollution in estuary and as a tracer of the sewage and suspensate. The daily variation of AS shows that the average concentration is lower and the variation range is less in the farther station and that the concentration of AS in botton water is higher than that in surface water. It suggests that the AS is richer in the particles in water and its transport capability is lower than COD. The vertical distribution of AS in the core samples of sediments reflects the history of pollution, it can be used to estimate the rate of sedimentation.