A simple and efficient method for iron speciation (Fe2+,Fe3+) using dispersive liquid–liquid microextraction based on solidification of organic drop (DLLME-SFO) technique followed by flame atomic absorption spectrometry was developed. In this method, 1 mL of ethanol (as the disperser solvent) containing 50 µL of 1-undecanol (as the extracting solvent) was injected rapidly into the sample solution containing iron (II), iron (III) species and 1.1 × 10−3mol L−1 oxine (as the complexing agent). The procedure is based on the complexation of Fe3+with 8-hydroxyquinoline (oxine) at pH 3, and extraction of the resulting complex using DLLMESFO. The total Fe was determined after the oxidation of Fe2+to Fe3+with concentrated nitric acid. The concentration of Fe2+ was determined from the difference between the concentration of total Fe and the Fe 3+ . Some parameters such as pH, oxine concentration, ratio of disperser and extractant solvent were investigated. Under the optimum conditions, the calibration graph was linear in the range of 25–250 µg L −1 for Fe 3+ with a limit of detection (LOD) of 4.8 µg L −1 . The relative standard deviation (RSD, %) for 10 replicate determinations of Fe3+ at 50 µg L−1 levels was 3.2%. To validate the developed method, a certified reference material (BRGM R52) was analysed and the determined value was in very good agreement with the certified value. The proposed method was successfully employed for determination of iron species in tap, well and spring water samples

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