In this paper, we discuss the use of dispersive liquid‐liquid microextraction (DLLME) combined with organic/water interface electrochemistry (OWIE) by using ferrocene as a model‐molecule. A mixture of 150 μL of ethanol (disperser solvent) and 50 μL of 1‐undecanol (extractant solvent) was injected into 9 mL of a ferrocene aqueous solution prepared in 1.0×10−3 mol L−1 H2SO4. Afterward, a drop of the organic phase containing ferrocene was directly inserted on a screen‐printed carbon electrode and the analytical curve was obtained, point‐to‐point, with a good linearity. Besides that, a boron‐doped diamond (BDD) electrode was used to promote the partition coefficient calculation, and it was possible to calculate the final concentrations of ferrocene in the aqueous and organic phases as being equal to 4.2×10−4 mol L−1 and 1.0×10−1 mol L−1, respectively. By using these values, the partition coefficient (log P) was calculated as 2.5±0.1 (n=3), a similar result to that obtained using other methodologies.

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