Iodine value is an important quality parameter for evaluation of the oxidative stability of biodiesel and vegetable oils, but the official methods are time-consuming and demand large amounts of reagents and solvents. The present work describes a novel procedure for determination of iodine value based on the discoloration of a triiodide aqueous solution due to halogenation of the unsaturated compounds in the samples. Iodine is extracted to the organic phase and consumed proportionally to the amount of unsaturated compounds in the samples. Thus, the remaining fraction of I 3 quantified by spectrophotometry in the aqueous phase is inversely proportional to the concentration of unsaturated compounds. For biodiesel samples, responses were linear from 10 to 106 g I 2 per 100 g, with coefficient of variation and limit of detection estimated at 5.0% (n = 8) and 2.5 g I 2 per 100 g, respectively. The corresponding values for vegetable oils were 20 to 140 g I 2 per 100 g, 3.0% (n = 10), and 7 g I 2 per 100 g, respectively. The procedure consumed only 1.2 mL of sample, 365 μg of I 2 , and 42 mg of KI with ca. 2.4 mL of waste generated per determination. The results agreed with those obtained by the official methods at the 95% confidence level.
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