At the Delft University of Technology Interfaculty Reactor Institute, a facility has been installed to irradiate cylindrical samples with diameters up to 15 cm and weights up to 50 kg for instrumental neutron activation analysis (INAA) purposes. To be able to do quantitative INAA on voluminous samples, it is necessary to correct for gamma-ray absorption, gamma-ray scattering, neutron absorption, and neutron scattering in the sample. The neutron absorption and the neutron scattering are discussed. An analytical solution is obtained for the diffusion equation in the geometry of the irradiation facility. For samples with known composition, the neutron flux—as a function of position in the sample—can be calculated directly. Those of unknown composition require additional flux measurements on which least-squares fitting must be done to obtain both the thermal neutron diffusion coefficient Ds and the diffusion length Ls of the sample. Experiments are performed to test the theory.