AOC 92.159 Iodine Absorption Number

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41.1.14 Table 920.159.

Test sample weights


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

ã 2005 AOAC INTERNATIONAL

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