This document describes the Wijs method test for determining the iodine value of oils and fats. It involves reacting a test portion of the oil or fat with Wijs iodine solution, then titrating the remaining iodine with sodium thiosulfate solution. The iodine value is calculated based on the titration results and is a measure of the degree of unsaturation in the oil or fat. Test portion weights are specified based on the expected iodine value or values in a reference table. The procedure involves multiple steps including addition of reagents, titration, and calculations to determine the iodine absorbed and reported as the iodine number.
This document describes the Wijs method test for determining the iodine value of oils and fats. It involves reacting a test portion of the oil or fat with Wijs iodine solution, then titrating the remaining iodine with sodium thiosulfate solution. The iodine value is calculated based on the titration results and is a measure of the degree of unsaturation in the oil or fat. Test portion weights are specified based on the expected iodine value or values in a reference table. The procedure involves multiple steps including addition of reagents, titration, and calculations to determine the iodine absorbed and reported as the iodine number.
This document describes the Wijs method test for determining the iodine value of oils and fats. It involves reacting a test portion of the oil or fat with Wijs iodine solution, then titrating the remaining iodine with sodium thiosulfate solution. The iodine value is calculated based on the titration results and is a measure of the degree of unsaturation in the oil or fat. Test portion weights are specified based on the expected iodine value or values in a reference table. The procedure involves multiple steps including addition of reagents, titration, and calculations to determine the iodine absorbed and reported as the iodine number.
This document describes the Wijs method test for determining the iodine value of oils and fats. It involves reacting a test portion of the oil or fat with Wijs iodine solution, then titrating the remaining iodine with sodium thiosulfate solution. The iodine value is calculated based on the titration results and is a measure of the degree of unsaturation in the oil or fat. Test portion weights are specified based on the expected iodine value or values in a reference table. The procedure involves multiple steps including addition of reagents, titration, and calculations to determine the iodine absorbed and reported as the iodine number.
AOAC Official Method 920.159 a Iodine value g Test portion Accuracy, mg Iodine Absorption Number of Oils and Fats 3 10.58–8.46 ±0.5 Wijs Method 10 3.17–2.54 0.2 First Action 1920 20 1.59–1.27 0.2 Final Action 40 0.79–0.63 0.2 A. Reagents 80 0.40–0.32 0.2 Wijs iodine solution.—(1) Dissolve 13 g resublimed I2 in 1 L 120 0.26–0.21 0.1 CH3COOH, and pass in dried (through H2SO4) Cl2 until original 160 0.20–0.16 0.1 Na2S2O3 titration of solution is not quite doubled. (Characteristic 200 0.16–0.13 0.1 color change at end point indicates proper amount of Cl2. Convenient a For 100 and 150% excess, respectively. method is to reserve some of original I2 solution, add slight excess of Cl2 to bulk of solution, and bring to desired titer by readditions of reserved portion.) Or: (2) Dissolve 16.5 g ICl in 1 L CH3COOH. few drops starch indicator, (mix ca 1 g soluble starch with enough Store in amber bottle sealed with paraffin until ready for use. Wijs cold water to make thin paste, add 100 mL boiling water, and boil ca solutions are sensitive to temperature, moisture, and light. Store in 1 min while stirring) and continue titration until blue entirely dark at <30°C. Determine I/Cl ratio as follows: disappears. Toward end of reaction, stopper bottle and shake Io dine con tent.—Pipet 5 mL Wijs so lu tion into 500 mL vigorously so that any I2 remaining in solution in CCl4 may be taken Erlenmeyer containing 150 mL saturated Cl2–H2O and some glass up by KI solution. beads. Shake, heat to bp, and boil briskly 10 min. Cool, add 30 mL Conduct 2 determinations on blanks in same manner as test portion, H2SO4 (1 + 49) and 15 mL 15% KI solution, and titrate immediately but without fat. Slight variations in temperature appreciably affect with 0.1M Na2S2O3. titer of I2 solution, as CH3COOH has high coefficient of expansion. It Total halogen content.—Pipet 20 mL Wijs solution into 500 mL is essential, therefore, that blanks and determinations on test portion Erlenmeyer containing 150 mL recently boiled and cooled H2O and be made at same time. Na2S2O3 equivalent of I2 absorbed by test 15 mL 15% KI solution. Titrate immediately with 0.1M Na2S2O3. portion taken = mL standard Na2S2O3 solution required by blank (B) - 2X mL used in determination (S). Calculate % by weight of I2 absorbed as I/Cl = 3B - 2X in 920.158B (see 41.1.13) and report as I2 number, Wijs method. Reference: JAOAC 48, 127(1965). where X = mL 0.1M Na2S2O3 required for I2 content and B = mL required for total halogen content. I/Cl ratio must be 1.10 ± 0.1. B. Determination Use test portion weight calculated as 26/expected Iodine value, or from Table 920.159. Weigh melted and filtered test portion into clean, dry, 500 mL glass-stoppered flask containing 20 mL CCl4. With pipet, add 25 mL I2 solution, draining pipet definite time. Excess of I2 should be 50–60% of amount added, that is, 100–150% of amount absorbed. Swirl, and let bottle stand in dark 30 min at 25° ± 5°C. Let oils with I2 values >150 (linseed and perilla) stand 1 h. Add 20 mL 15% KI solution and 100 mL recently boiled and cooled H2O. Titrate the I2 with 0.1M Na2S2O3, 942.27 (see A.1.13), added gradually, shaking constantly until yellow solution turns almost colorless. (Vigorous magnetic stirring is convenient.) Add