A new azo dye Schiff base ligand, namely 1, 1′-bis(5-(4-nitrophenyl)diazenyl)-2-hydroxybenzylideneamino)ethylenediimine (NDHBDED) has been synthesized and it was impregnated with alumina for extractive determination of metal ions. In this report the sorbent matrix was used for extractive determination of Mn (II) and Cu (II) ions by solid phase spectrophotometric (SPS) method. Both the metal ions were extracted at pH 6.5 and 5.5 respectively. The complexes show maximum absorbance at λ _max 590 nm and 570 nm respectively for Mn (II) and Cu (II) ions.  The Beer's law range was 10-100 µg/ ml for both the metal ions. Job’s method and mole-ratio method showed that metal-ligand ratio in the complexes to be 1:1.  The Molar absorptivity for Mn (II) and Cu (II) were 2.351x10^-4   L mol^-1 cm^-1 and 2.225x10^-4   L mol^-1 cm^-1 respectively. The Sandell’s sensitivity was 0.004 µg/ cm² and 0.008 µg/ cm² for Mn (II) and Cu (II) ions respectively. The proposed method was successfully applied to the determination of each metal ion in real samples and tap water.