Iodine Value of Oil

12.
0 Determination of Iodine Value

12.1 Definition: The iodine value of an oil/fat is the number of grams of iodine absorbed by 100g of
the oil/fat, when determined by using Wijs solution.
The iodine value is a measure of the amount of unsaturation (number of double bonds) in a fat. The
iodine value
(or iodine adsorption value or iodine number or iodine index, commonly abbreviated as IV) in
chemistry is the mass of iodine in grams that is consumed by 100 grams of a chemical substance.
12.2 Principle: The oil/fat sample taken in carbon-tetrachloride is treated with a known excess of
iodine monochloride solution in glacial acetic (Wijs solution). The excess of iodine monochloride is
treated with potassium iodide and the liberated iodine estimated by titration with sodium thiosulfate
solution.
12.3 Analytical importance:
Iodine numbers are often used to determine the amount of unsaturation in fats, oils and waxes.
In fatty acids, unsaturation occurs mainly as double bonds which are very reactive towards halogens,
the iodine in this case.
Thus, the higher the iodine value, the more unsaturations are present in the fat.[1] It can be seen from
the table that coconut oil is very saturated, which means it is good for making soap. On the other
hand, linseed oil is highly unsaturated, which makes it a drying oil, well suited for making oil paints.
R — CH = CH — R ′ + ICl (excess) → R — CH(I)— CH(I) — R ′ + ICl (remaining)

ICl + 2 KI → KCl + KI + I2
I2 + Starch(blue) + 2 Na2S2O3 → 2 NaI + Starch(colorless) + Na2S4O6
12.3.1 Apparatus: 500 ml Erlenmeyer flask.
12.3.2 Reagents:
i) Potassium dichromate AR
ii) Concentrated hydrochloric acid AR
iii) Glacial acetic acid, free from ethanol
iv) Carbon tetrachloride, analytical reagent grade
v) Iodine mono-chloride (ICl)
vi) Potassium iodide (free from potassium iodate) - 10% solution prepared fresh
vii) Starch solution - Mix 5 g of starch and 0.01 g of the mercuric iodide with 30 ml of cold water
and slowly pour it with stirring into one litre of boiling water. Boil for three minutes. Allow to cool
and decant off the supernatant clear liquid.
viii) Wij’s Iodine monochloride solution - Dissolve 10 ml of iodine monochloride in about 1800 ml
of glacial acetic acid and shake vigorously. Pipette 5 ml of Wij's solution, add 10 ml of potassium
iodide solution and titrate with 0.1N standard sodium thiosulphate solution using starch as indicator.
Adjust the volume of the solution till it is approximately 0.2 N or prepare Wij’s iodine solution by
dissolving 13 gm resublimed Iodine in 1 litre acetic acid and pass in dried chlorine (dried through
H2SO4.) until original Sod thiosulphate titre of the solution is not quite doubled (characteristic
colour change at the end point indicates proper amount of Chlorine. Convenient method is to reserve
some amount of original I solution, add slight excess of Cl to bulk of solution and bring to desired
titre by re additions of reserved portion). Store in an amber bottle sealed with paraffin until ready for
use. Wij’s solutions are sensitive to temp, moisture and light. Store in dark at less than 30°C.
Determine I / Cl ratio as follows Iodine Content – Pipette 5 ml Wij Solution into 500 ml Erlenmeyer
flask containing 150 ml saturated Cl – water and some glass beads. Shake, heat to boiling point and
boil briskly 10 minutes. Cool, add 30 ml H 2SO4 ( 1 + 49) and 15 ml 15 % KI solution and titrate
immediately with 0.1 N Na2 S2O3.
Total Halogen content – Pipette 20 ml Wij’s solution into 500 erlenmeyer flask containing 150 ml
recently boiled and cooled water and 15 ml 15 % KI solution. Titrate immediately with 0.1 N
Na2S2O3. I / Cl = 2 X / (3B – 2 X) where X = ml of 0.1 Na 2 S2O3 required for I content and B = ml
required for total halogen content. I / Cl ratio must be 1.10±0.1 ix) Standard sodium thiosulphate
solution (0.1N)- Dissolve approximately 24.8 g of sodium thiosulphate crystals (Na 2S2O3.5H2O) in
distilled water and make up to 1000 ml. Standardise this solution by the following procedure:
Weigh accurately about 5.0 g of finely powdered potassium dichromate which has been previously
dried at 105ºC±2ºC for one hour, dissolve it in distilled water and make up to 1 L. For
standardisation of sodium thiosulphate, pipette 25 ml of this solution into a 250 ml conical flask. Add
5 ml of concentrated hydrochloric acid and 15 ml of a 10 percent potassium iodide solution. Allow to
stand in dark for 5 min and titrate the content with sodium thiosulphate solution using starch as
indicator at the end. End point is change of blue colour to green. N = 25W 49.03 V Where, N =
Normality of the sodium thiosulphate W = Weight in g of the potassium dichromate, and V =
Volume in ml of sodium thiosulphate solution required for titration
12.3.4 Procedure:
Oil / fat may be weighed accurately following the Table given below: Expected Iodine Weight to be
take for Value estimation (g)
Weigh 2.7g (As expected value of coconut oil is between 6 – 11) accurately an appropriate quantity
of the dry oil/fat as indicated in the Table above, into a 500 ml conical flask with glass stopper, to
which 25 ml of carbon tetrachloride have been added. Mix the content well. The weight of the
sample shall be such that there is an excess of 50 to 60 percent of Wij’s solution over that actually
needed. Pipette 25 ml of Wij's solution and replace the glass stopper after wetting with potassium
iodine solution. Swirl for proper mixing and keep the flasks in dark for half an hour for non-drying
and semi-drying oils and one hour for drying oils. Carry out a blank simultaneously. After standing,
add 15 ml of potassium iodide solution, followed by 100 ml of recently boiled and cooled water,
rinsing in the stopper also. Titrate liberated iodine with standardized sodium thiosulphate solution,
using starch as indicator at the end until the blue colour formed disappears after thorough shaking
with the stopper on. Conduct blank determinations in the same manner as test sample but without
oil/fat. Slight variations in temperature appreciably affect titre of I 2 solution as chloroform has a high
coefficient of expansion. It is thus necessary that blanks and determinations are made at the same
time.
12.3.5 Calculation:
Iodine value = [12.69 (B – S) N]/ W
Where, B = volume in ml of standard sodium thiosulphate solution required for the blank.
= Final Burette Reading – Initial Burette Reading = 39.1-2.7
S = volume in ml of standard sodium thiosulphate solution required for the sample

= Final Burette Reading – Initial Burette Reading = 39.2 - 25.6
N = normality of the standard sodium thiosulphate solution = 0.1 N.

W = weight in g of the sample = 2.7g.

Iodine Value of Oil

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12.

0 Determination of Iodine Value

R — CH = CH — R ′ + ICl (excess) → R — CH(I)— CH(I) — R ′ + ICl (remaining)

12.3.1 Apparatus: 500 ml Erlenmeyer flask.

S = volume in ml of standard sodium thiosulphate solution required for the sample

N = normality of the standard sodium thiosulphate solution = 0.1 N.

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