Neutron activation analysis has been applied for determination of selenium in environmental and food samples. Food and environmental samples from city, industrial and agricultural zones were collected with utmost care. Samples were activated in the flux 1·1013 n·cm–2·s–1 in the CIRUS reactor of BARC, Bombay, 75-Se was separated from 6.5N HCl solution using ethyl--isonitrosoacetoacetate (HEINA) reagent. The decontamination studies showed the method is very selective. Selenium contents of wheat, rice, vegetables, cereals pulses etc. and of soil, water, and deposits on plants and surface were determined by the procedure developed.