Instrumental and preconcentration methods of neutron activation analysis (NAA) have been standardized for the determination of concentration of iodine in grass and cow milk samples, respectively. To study the transfer of iodine from grass to milk, known quantity of grass spiked with potassium iodide solution was fed to a cow. The spiked grass samples and milk samples, obtained from the cow after the ingestion of spiked grass, were collected. Iodine was separated from the milk samples chemically using Dowex 1X8 anion exchange resin. Spiked grass and ion exchange resin samples were neutron irradiated and radioactive assay was carried out using a 45 % relative efficiency HPGe detector coupled to an 8k channel analyzer. Iodine concentrations in spiked grass samples were found to be in the range of 1,487–2,002 mg kg^-1. Concentration of iodine in milk after 12 h of feeding the cow with spiked grass was 871 ± 56 μg L^-1 which was reduced to 334 ± 32 μg L^-1 after 48 h.