A new rapid and accurate method for the spectrophotometric microdetermination of nic- kel and copper ions using p-nitro-(Ia), p-methoxy-(Ib) and p-ethoxy phenylazo-Schaffer acid (Ic) is given. The optimum conditions favouring the formation of the complexes are extensively investigated. The molecular structure of complexes and their obeyence to Beer’s law as well as their stabilities are also studied, a spectrophotometric titration method for Ni and Cu with EDTA using la, Ib or Ic as indicators is also given