[en] Antimony is an element found in low concentrations in the environment. However, its determination has attracted great interest due to the knowledge of its toxicity and increasing application in industry. The determination of antimony has been a challenge for researchers since this element is found in low concentrations which make its analysis a difficult task. Therefore, although neutron activation analysis (NAA) is an appropriate method for the determination of various elements in different types of matrix, in the case of Sb its analysis presents some difficulties, mainly due to spectral interferences. The objective of this research was to validate the NAA method for Sb determination in environmental samples. To establish appropriate conditions for Sb determinations, preliminary assays were carried out for further analysis of certified reference materials (CRM). The experimental procedure was to irradiate samples with a synthetic Sb standard for a period of 8 or 16 hours in the IEA-R1 nuclear research reactor, followed by gamma ray spectrometry. The quantification of Sb was performed by measuring the radioactive isotopes of ¹²²Sb and '1²⁴Sb. The results of preliminary assays indicated the presence of Sb in Whatman no 40 filter paper used in the preparation of the synthetic standard, but at very low concentrations, which could be considered negligible. In the case of the plastic material used in bags for the sample irradiation, it should be chosen carefully, because depending on the thickness, they may contain Sb. The analyses of the stability of the diluted Sb standard solution showed no change in the Sb concentration within eight months after its preparation. Results obtained in the analysis of certified reference materials indicated the interference of ⁷⁶As and also of ¹³⁴Cs and ¹⁵²Eu in the Sb determinations by measuring '1²²Sb, due to the proximity of the gamma ray energies. The high activity of '2⁴Na can also mask the peak of ¹²²Sb hindering its detection. The analysis of CRM indicated that the accuracy and precision of the results depend on the type of matrix analyzed, its concentration in the sample, radioisotope measured and of the decay time used for the measurements. The analysis of the components that contribute to the uncertainty of the Sb concentration indicated that the largest uncertainty contribution is given by statistical counting of the sample. The findings also showed that the value of combined standard uncertainty depends on the radioisotopes of Sb measured and the decay time used for counting. This study showed that NAA is a very adequate method for Sb determinations in environmental samples furnishing results with low uncertainty values. (author)