A simple dispersive liquid–liquid microextraction based on solidification of floating organic droplets coupled with spectrophotometric detection was developed for the determination of nitrite in Chabahar Bay seawater. In the preparation procedure, 2,3-diaminonaphthalene as derivatization reagent reacts with nitrite in acidic medium to form a photometric center of 1-[H]-naphthotriazole (NAT). Product material (NAT) was extracted by dispersive liquid–liquid microextraction with 1-dodecanol as extraction solvent and after centrifugation, the floated droplet was solidified in an ice bath and was easily removed for analysis at λmax = 358 nm. Several important factors affecting the microextraction efficiency were optimized in artificial seawater as a best simulation media. Under the optimum conditions, the absorbance of NAT was linear with nitrite concentrations ranging from 0.1 to 11 μg/mL in seawater. Figures of merit of method such as enrichment factor (52), limit of detection (0.094 μg/mL), and repeatability (N = 6, %RSD = % 5) were evaluated as appropriate. Determination of nitrite in Chabahar coastal zone showed that nitrite concentration varied in the range of 0.77–1.76 μg/mL with an increase of concentration from South to the North of Bay.

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