This work aimed the development of a methodology for the treatment of uncertainty in the k 0 Method for Neutron Activation Analysis (NAA), comprehensively and accurately, by applying the covariance analysis methodology. All parameters involved in determining the concentration of a given element were analyzed with criteria in order to establish the correlations among them. Also established were the possible correlations between the concentrations of different elements for the same sample and for different samples. This procedure generated a large number of correlations that have been rigorously addressed. Data for analysis were obtained experimentally by means of irradiations performed at 24A irradiation position, near the core of the IEA-R1 research reactor, located at IPEN-CNEN/SP. The parameters and f, characterizing the neutron field were determined by applying several methods from the literature. A detailed statistical treatment was applied to each measurement, verifying the various uncertainties and partial correlations. In order to deepen the study, targets of 64 Zn and 68 Zn were chosen, for which the nuclear parameters k 0 and Q 0 showed discrepancies in the literature in order to determine them experimentally. For 64 Zn, the values for these parameters resulted 5.63(8) × 10-3 and 1.69(6), respectively. For 68 Zn they resulted 4.00(6) × 10-4 and 2.34(4), respectively. These values were compared with data from the literature. The Monte Carlo method was applied at various stages of study, to allow accurate determination of some parameters needed for the complete data analysis.