[en] The objective of this work was the development and establishment of a specific analytical protocol for the determination of the "5"9Ni, "6"3Ni, "5"5Fe, "9"9Tc and "9"4Nb radionuclides in low and intermediate radioactive waste samples of Almirante Alvaro Alberto Nuclear Power Plant, CNAAA, located in the city of Angra dos Reis, RJ. The separation and purification techniques used have taken into account the particularities of each radionuclide studied. Chemical separation methods were used, as well as carriers and radioisotope tracers, and ion-exchange and extraction chromatography involving specific resins. The main techniques used for the analysis and determination of the radionuclides were Liquid Scintillation Counting (LSC) and Gamma Spectrometry. Also used were Atomic Emission Spectroscopy with Inductively Coupled Plasma (ICP-AES) and Neutron Activation Analysis (NAA) for the chemical yield determination. Concerning to the "5"9Ni, "6"3Ni, "5"5Fe radionuclides, the methodology of sequential separation proved to be very appropriate for their separation and determination, as could be observed by the results obtained. Chemical yields in the range from 39 to 100%, and LSC counting efficiencies in the range of 37.8% for "5"5Fe, and 71.5% for "6"3Ni, are in accordance with the results found in the literature. The spectra of LSC showed that the methodology used to separation and purification of these radionuclides was very successful. The results for "5"9Ni have shown that the use of a "5"5Fe certified standard for calibration of the equipment was a viable alternative. In the case of the "9"9Tc radionuclide the use of rhenium as carrier and chemical yield monitor, resulted in high chemical yields. Use of Gamma Spectrometry analysis made it possible to check that the main interfering agents were actually removed with the combined use of anion exchange chromatography and TEVA resin. The chemical yield of "9"4Nb was measured by Gamma Spectrometry analysis of the "9"4mNb nuclide formed by neutron activation of "9"3Nb, and quite satisfactory values close to 70% were obtained. The gamma spectra exhibited the two well-defined peaks characteristic of "9"4Nb and no peaks from possible interfering nuclides, showing that the process of separation and purification was very effective. (author)