[en] Simple and highly sensible nuclear-physical methods were developed for Ni and Co analysis in ferrous laterites with previous chemical treatment of samples. Concentrated fluorhydric acid was used for sample treatment. Separation of Ni and Co from Fe and other elements was made using cationic exchange resins in 1N HF. Further separation of Ni from Co was made with anionic exchano.e resins in 9N HCl. For exciting x-ray fluorescence of the elements ₇₁Ce and ₁₀₉Cd sources were used; and for the samples activation photo-neutrons and bremsstrahlung from a microtron were used. Sensitivity limits were obtained of approximately 0.0001% for Ni and Co by x-ray fluorescence method; approximately 0.00005% for Co by neutronic activation analysis; and approximately 0.0015% for Ni by gamma activation analysis. The measurement time was 20 min