In this thesis, hollow fiber based liquid-liquid-liquid microextraction (HF-LLLME) followed by flow injection and spectrophotometric detection was applied as a simple method for extraction and determination of iodide in milk and river water. For determination of iodate in edible salt, the iodate was converted to iodide. The extraction of iodide was carried out using a cationic surfactant (Aliquat 336) which dissolved in hexyl acetate as organic phase for filling the porous of the hollow fiber wall and 0.1 M ClO 4 - solution as acceptor phase in the lumen of the fiber. Iodide was oxidized to iodine in a a photochemical reaction coil. A mercury lamp was used as a UV source for the reaction. The iodine showed a maximum absorption at 445 nm. The factors affecting the HF-LLLME and determination include type of organic solvent, concentration of surfactant, type of acceptor phase, concentration of acceptor phase, ionic strength, volume of donor, stirring rate and extraction time were optimized. Tube length of reaction coil and carrier flow rate were also optimized. Analytical parameters include: intra-and inter-day relative standard deviation (4.5%, 11%), linear dynamic range (5-1000) and enrichment factor (350) were calculated.
