A preconcentration method for antimony in waters involving adsorption on a Tantalum Wire, followed by electrothermal atomic absorption spectrometry with a tungsten tube atomizer is described. The best pH for the adsorption of antimony was 2. The optimal immersing time was 120 s. Under the optimal conditions, the detection limit for antimony by the tantalum wire preconcentration method was 50 pg/mL (3S/N) and the relative standard deviation was 9.4%. The effects of large amounts of concomitants on the preconcentration of antimony were evaluated. Even though 103–104 fold excess of matrix elements existed in water, the antimony response was not significantly affected by the matrix elements. The method with preconcentration on a tantalum wire was applied to the determination of antimony in waters and proved to be sensitive, simple, and convenient. This adsorption method can be utilized in in-situ sampling of ultra-trace antimony in environmental samples (water). Furthermore, after sampling it is easy to carry and store the tantalum wire without contamination for a long time. The technique developed was shown to be useful for the determination of Sb in waste waters at the 1–5 µg/L level.