Two new macrocyclic Schiff bases, (5) and (7), containing nitrogen-sulfur donor atoms were designed and synthesized by reaction of a,a' bis(o-aminophenylthio)-1,2-xylene with glyoxal and phthaldialdehyde, respectively. The liquid-liquid extraction of metal picrates such as Ag+ , Hg2+ , Cd2+ , Zn2+ , Cu2+ , Ni2+ , Mn2+ , K+ , and Na+ from aqueous phase to the organic phase was carried out using the novel ligands. The effect of chloroform and dichloromethane as organic solvents over the metal picrate extractions was investigated at 250.1 degrees C by using UV-visible spectrometry. The extractability and selectivity of the tested metal picrates were evaluated. The values of the extraction constants (log K-ex) were determined for the extracted complexes.