Iodine was determined in foodstuffs consumed in Libya employing two modes of NAA. The first mode was instrumental using short-time irradiation with epithermal neutrons behind a Cd shield (EINAA). The other mode utilized short-time irradiation with the reactor-pile neutrons followed by radiochemical separation (RNAA). The radiochemical separation procedure was based on the alkaline-oxidative fusion of samples and extraction of elemental iodine into chloroform. Separation yield determined using the radiotracer 131I was within the range of 90 to 95%. For quality control purposes, standard reference materials were analyzed in both modes employed. Using RNAA, a detection limit of ∼1 ng g−1 could be obtained indicating superiority of the method in measuring ultra-trace levels of iodine. On the other hand, more than one order of magnitude higher detection limit did not allow sufficiently accurate determination of iodine in Libyan foodstuffs using EINAA.