To examine the effect of extraction solvent volume on the extraction efficiency xtures containing various volumes of 1-decanol and 1undecanol as extraction solvent with a fixed volume of ethanol as dispersive solvent were applied using the same DLLME-SFO procedure. In general, the extraction efficiency increases with increasing volume of extraction solvent and then decreases due to the dilution effect. Although the use of a lower volume of extraction solvent might lead to a better analytical response, it is not easy to handle, and it is difficult to remove the solidified drop from the surface of the aqueous phase in the amount necessary for the absorbance measurement. So 55 μL was preferred as the extraction solvent volume. Since the results obtained are close for both extraction solvents, 1-undecanol was selected for subsequent experiments due to the higher melting point.