Flow-injection atomic spectrometry with sorbent extraction preconcentration is applied to the simultaneous determination of iron(II) and iron(III). Upon injection of a sample containing iron in both oxidation states, iron(In) is directly carried to the flame atomic absorption spectrometer whereas the iron(II)-ferrozine complex formed in-line is temporarily retained on a C-18-modified silica column placed between the injection valve and spectrometer and is subsequently eluted with methanol.