The Nigerian Research Reactor-1 was employed in the analysis of iodine in local food samples at an operating flux of ?ncm?2?s?1. Preconcentration neutron activation analysis (PCNAA) was compared against the most common spectroscopic (Sandell-Kolthoff reaction) technique, giving a concentration range of 0.295 to 2.960?mg/Kg and 0.264 to 2.725?mg/Kg, respectively, with an average percentage deviation of 11.34% and a positive correlation between the methods at 0.89. PCNAA and Sandell-Kolthoff spectroscopy of NIST 1548a reported values of ?mg/Kg and with Student’s t-test score of 1 and 0.95 and percentage standard deviation of 0 and 1.12%, respectively. 1. Introduction Iodine is an essential component of the thyroid hormones: thyroxine (T4) and triiodothyronine (T3), comprising 65 and 59 percent of their respective weights [1]. The thyroid hormones T4 and T3 regulate many key biochemical reactions, particularly protein synthesis and enzymatic activity. Major target organs are the developing brain, muscle, heart, pituitary, and kidney. Without sufficient iodine, the body is unable to synthesize the thyroid hormones, and because they regulate metabolism in every cell of the body and play a role in virtually all physiological functions, iodine deficiency can have a devastating impact on health and well-being summarily termed iodine deficiency disorders (IDD). IDD is a major cause of retardation in children and was one of the contributing factors to high infant mortality [2]. Thyroid hormones, and therefore iodine, are essential for mammalian life. The Nigerian Research Reactor-1 (NIRR-1) is the first in the country and its primary objective is to uplift the socioeconomic life of Nigerian citizen through effective utilization and research activities. It is meant to serve all categories in need of nuclear analytical and other related services. Irradiation and counting regimes for over 30 elements in both biological and geological matrices, including the essential elements Fe, Cr, Co, Cu, Mn, and Zn have been standardized [3]. Recently, standard addition technique was employed to determine Selenium in cereals [4]. Accurate determination of iodine and in particular in biological matrix has always been difficult due to its low concentration and the inherent volatility of molecular iodine through sublimation at room temperature. However, iodine concentrations in biological matrix have been analyzed using a variety of techniques including spectroscopy [5–7], inductively coupled mass spectrometry [8–10], and ENAA [11–13] with the neutron activation analysis and mass
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