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A series of calix [4]pyrrole hydroxamic acids have been used for the liquid-liquid extraction, separation, preconcentration and spectrophotometric determination of vanadium(V) ions from aqueous media using ethyl acetate as a solvent. Various significant extraction parameters like pH, effect of solvents, shaking time, concentration of vanadium(V) and concentration of reagent were evaluated. The extracted complex was determined simultaneously by spectrophotometry and inductively coupled plasma atomic emission spectroscopy (ICP-AES). The wavelengths of maximum extraction (λ max ), molar absorptivity (ε), linear concentration range obeying Beers law, effect of diverse ions have been determined. The stoichiometry of complex, the regression analysis equation, relative standard deviation, limit of detection (LOD), limit of quantification (LOQ) were also evaluated. Mechanism of metal-ion transport has been proposed. The validity of proposed method was checked by determining vanadium(V) in environmental and industrial samples as well as some standard reference materials.