The distribution equilibrium of Zn (II) between synergistic mixture of N-n-octylaniline and trioctylamine in xylene and aqueous acidic thiocyanate media has been investigated as the function of concentration of extractant in organic phase and concentration of hydrogen ion and Zn (II) ions in aqueous phase. The stoichiometry of the extracted species was determined on the basis of slope analysis. Zn (II) is extracted by the anion exchange mechanism as [(RR'NH 2 ) 2 + Zn(SCN) 4 2-] org or [(R 3

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... 2 + Zn(SCN) 4 2- ] org . The extraction process is favored due to synergism. It was found that a large number of cations and anions have a high tolerance limit. The selectivity of the extraction is increased by the use of suitable masking agents. The method is extended for the extraction of Zn (II) from synthetic mixture and pharmaceutical sample.