AbstractA method for determining antimony in drinking waters is described. In order to prevent a substantial error caused by the different oxidation states of antimony, Sb(V) is reduced to Sb(III) with potassium iodide‐ascorbic acid. Covalent hydride is generated with a home made device by adding NaBH4. The hydride is then atomized in a flame‐heated silica tube and atomic absorption is measured spectrophotometrically. The optimal conditions for this determination are discussed and interference effects are described.Results obtained by determining linearity range (0–200 ng), detection (LOD) and quantitation (LOQ) limits (LOD = 0.347 ng/ml, LOQ = 1.158 ng/ml), precision (instrumental CV 4.08% and method CV 7.74%) and accuracy performed by recovery assays (96.1%) show that the method is useful for antimony determination at the concentration usually present in drinking