A direct method has been developed for the spectrophotometeric determination of Ni(II), Co(II) and Cu(II) using 7-(14-nitrophenylazo)-8-hydroxyquinoline-5-sulfonic acid (p-NIAZOXS) as a complexing reagent in the micellar media. Beer’s law was obeyed over the range from 0.24- 1.46μg/mL for Ni (II), 0.29-1.3 μg/mL for Co(II) and 0.22-1.36μg/mL for Cu(II). Sandell’s sensitivity and Molar absorptivity have been found to be 0.0037μg/cm2 and 2x104 Lmol-1cm-1 for Ni(II), 0.0024μg/cm2 and 2.54x104 Lmol-1cm-1 for Co(II), and 0.0034μg/cm2 and 2.2 x104 Lmol- 1cm-1for Cu(II). Each metal complex was stable for more than 24 hrs under optimized conditions. The effect of various diverse ions have been studied and above method has been applied for the determination of Ni(II), Co(II) and Cu(II) in environmental, food samples and water samples. The developed method has been found to be quite simple, rapid, sensitive and reproducible results were obtained. The precision (RSD<1.5%) and the accuracy obtained were satisfactory.