Two new macrocyclic hydrazone Schiff bases were synthesized by reaction of succindihydrazide and adipdihydrazide with acetylacetone. Hydrazones have been characterized by elemental analyses and IR, mass, (1)H NMR, and (13)C NMR spectral data. Hydrazones have been studied by liquid-liquid extraction towards the s-metal ions (Li(+), Na(+), and K(+)) and d-metal ions (Cu(2+) and Cr(3+)) from aqueous phase to organic phase. The effect of chloroform and dichloromethane as organic solvents over the metal chlorides extraction was investigated at 25 ± 0.1°C by using flame atomic absorption. We found differences between the two solvents in extraction selectivity.