EXPERIMENT 14

ANALYSIS OF OILS AND FATS:

Structure

14.1 Introduction
Objective
14.2 Determination of Saponification Value
Principle
Requirements
Procedure
Observations
Calculations and Result
14.3 Determination of Iodine Value
Requirements
Reagent
Procedure
Observations
Calculations and Result
14.4 Determination of Acid Value
Principle
Requirements
Procedure
Observations
Calculations and Result

14.1 INTRODUCTION
Oils and fats are triglycerides with three long chains of fatty acid group randomly
esterified with glycerol. The difference between oils and fats is that, oil are liquid
whereas fats are solid at ordinary temperature. .

Fats and oils mainly come from plant seed. In animals they are present under the
skin, in tissues and muscles. Some of the fatty acids like linoleic, linolenic and
arachidonic acids are very essential for our body. Fats and oils are widely distributed
in food and are of great nutritional value. They are also used in manufacture of
soaps, detergents, glycerine, candles, printing ink etc.

The industrial value of a particular oil or fat depends upon its physical and chemical
characteristics, e.g. melting point, specific gravity, refracting index, viscosity,
saponification value, iodine value, acid value, acetyl value, etc. In this experiment we
will determine some of these parameters, such as saponification value, iodine value
and acid value.

Objectives

After studying and performing this experiment you should be able to

define the term saponification value, iodine value and acid value, and
determine sap&ification value, iodine value and acid value.

14.2 DETERMINATION OF SAPONIFICATION VALUE

Esters are hydrolyzed either by aqueous base or by aqueous acid to yield component
acid and alcohol fragments. Hydrolysis of an ester in alkaline medium is called
saponification.
 RCOOK
I I
CHOOCR' + 3 KOH 4 CHOH + R f C o o ~
I I
Saponification number or saponification value is an arbitrary unit that is defined as
"number of mg of potassium hydroxide required to saponify lgm of oil o r fat" i.e. to
neutralise completely the fatty acids resulting from complete hydrolysis of lgm fat or
oil.

The saponification value gives an idea about the molecular weight of fat or oil. The
smaller the saponification value, the higher the molecular weight. As the average
molecular weight of oil or fat depends on the average length of carbon chain of the
fatty acid components, the saponification value also gives an indication of the
average length of the carbon chain in the oils or fats. The saponification value for
each oil has its own characteristic value.

14.2.1 Principle
Boiling of'the sample under reflux condenser with ethanolic KOH solution, and .
titration of excess potassium hydroxide with standard HC1 in presence of an indicator.

Apparatus Chemicals
Conical f-1.sk - 250 cm3 Standard HC1 (ME)
Reflux condenser Alcohol
Pipette Potassium hydroxide
Burette - 50 cm3 Phenolphthalein
Water bath

Solution Provided

2.5 M KOH Solution: It can be prepared by dissolving 24.2g KOH in 100 cm3 water.

Procedure
1. Weigh accurately about l g of oil in 250 cm3 conical flask,
2. Dissolve the ester in 25 cm3 alcohol and then add 25 cm3 of 2.5M KOH
solution with the help of a pipette,
3. A t t a ~ ha reflux water condenser to the flask and add some boiling chips,
4. Heat the flask in water bath for about 1 hour with-occasional shaking,
5. After 1hour, stop heating. Add to the hot solution 0.5 to 1.0 cm3 of
phenolphthalein,
6. Titrate the excess alkali with standard MI2 HCI until the colour of the
indicator changes. Record the volume of HCI used in Observation Table-11.
7. Carry out determination with the same prepared sample again to get at least
two concordant readings.
8. Carry out a blank test upon the same quantity of KOH solution a t the same
time under the same conditions. Record the volume of HCI used in
Observation Table-I.

143.3 Observations
Mass of the weighing bottle, ml=
Mass of the bottle + oil, m2=
Mass of the bottle, m3 =
(after transferring the oil)
I Mass of oil transferred, m2-m3 = m=
Analysis of oils and Fats:

Observation Table-I
(Blank ~ x ~ e i i m e n t )
KOH Solution vs. HCI
I
I
SI. Volume of KOH Burette Reading Volume of HCI
No. Solution in cm3 Initial Final solution used in cm3
(Final-Initial)

Observation Table-I1
(Original Experiment)
+
Oil Sample KOH Solution vs. HCI

S1. Volume of oil Sample Burette Reading Volume of HCI

No. + KOH Solution in cm3 Initial Flnal solution used in cm3
(Final-Initlal)
1.
2.
3.

14.3.4 Calalation and

Result

The saponification value (S.V.) is given by the formula:

56.1 xMm x (Vo- Vl)

S.V. =
m
where: Vo = Volume of HCl used in the blank titration cm3
Vl = Volume of HC1 used in the original titration cm3
M,,,= Molarity of HCl
m = mass of the oil in g.

14.3 DETERMINATION OF IODINE VALUE

Iodine value or iodine number of fats or oil is a measure of its degree of unsaturation
and gives an idea of its drying character. Iodine value depends on the number of
double bond present in the molecule. Low iodine value means that the carbon chain
of triglyceride contains very few carbon-carbon double bond, while a higher iodine
number indicates a large number of double bonds present in the molevle. If the
triglyceride do not contain any double bond then the iodine value will be zero.
Iodine value can be defined as "the number of grams of halogen absorbed by 100
grams of the oils fat, and expressedas the weight of iodine.

14.3.1 Principle
A know weight of oil is treated with ICI solution in CC14 or CHC13 and the amount
of IC1 absorbed is determined. Iodine number is thus determined. In this process
following reaction occurs:

>c = c( + CI>-I c-c<

I I
I C1
Chemical LabV After the completion of the reaction K1 solution is added which is oxidised to I2 by
unreacted ICl
IC1 + K
l
- I2 + KC1
(unused)
. .
The liberated iodine is titrated with standard NaS203 solution using starch solution
as indicator. .

I, + 2Na2S,03 -2NaI + Na2S206

143.2 Requirements
Apparatus

The apparatus must be clean and perfectly dry.

1. Conical flask (250 cm3)

2. Burette (50 cm3)
3. Pipette (25 cm3)

Chemicals
1. Glacial acetic acid
2. Carbon tetrachloride
3. Iodine trichloride
4. Iodine, pure, resublimed
5. Potassium iodide,
6. Sodium thiosulphate,
7. Starch solution

Solution Provided

Alternatively Wijs solution

Sodium Thiosulphate (Mf10):It can be prepared by dissolving 24.8g Na25203in water
may be prepared by dissolving in a ldm3 volumetric flask.
separately 7.9g of iodine
tri-cloride and 8.7g of pure Potassium iodide: It can be prepared by dissolving 100 g potassium iodide in 1 dm3
i o d ~ n ein glacial acetic acid, water.
rm ixing the two solution and
dilu. ting them to one dm3with
Wijs Solution (ICI): This can be prepared by dissolving 9 m of iodine trichloride in
glacial acetic acid. 3
a mixture of 700 cm3 glacial acetic acid (pure) and 300 cm carbon tetrachloride.

143.3 P-rocedure
The amount of oil to be taken varies according to its expected iodine value and is
given in the following table:
- --

Iodine Value Weight to be taken

expected (g)
0-5 3.0
5-20 1.O
21-50 0.40
51-100 0.20
101-150 0-15
151-200 0.10
1. Dissolve the appropriate quantity of oil, in a Analysis of oils and Fats:

250 cm3 conicalflask in 15 cm3carbontetrachloride.

2. Add 25 cm3 of Wijs solution, from the burette, to the mixture. If 15cm3is insufficient to
dissolve the oil, large amount of
3. Close the flask, shake gently and allow it to stand in dark at about 20'~. oil may be added. This should
be mentioned in the report of
4. For oils having iodine value below 150, leave the flask in dark for 1 hour; for the analysis.
those with iodine value above 150 leave.the flask for 2 hours.
5. After that add 25'cm3 of potassium iodide solution and 150 cm3 of water.
6. Titrate the liberated iodine with standard W 1 0 sodium thiosulphate solution,
using starch solution as indicator, continue the titration until the blue colour
just disappears. Record the value of Na2S203 used in Observation Table-IV
7. Carry out experiment again to get at least two correspondent readings.
8. Carry out a blank test with out oil under the same conditions. Record the
volume of Na2S203 used in Observation Table-I11

143.4 Observation:
Mass of the weighing bottle, =ml
P
- ... g
Mass of the bottle + oil, =m2 - ...g
Mass of the bottle, =m3 - ...g
(after transferring the oil)
Mass of the oil transferred, =m2-m3=m = ... g
Observation Table- 111
(Blank Expeiinient)'
1CI solution vs. MI10 Sodium Thiosulphate Solution

SI.No. Volume of ICI Burette Reading Volume of Sodium thiosulphate

No. solution in cm3 Initial Final solution used in cm3
(Final-initial)

Observation Table-N
(Original Experiment)
Oil Sample + ICI Solution Vs MI10 Sodium Thiosulphate Solution
-

SI.No. Volume of Oil Burette Reading Volume of Sodium

Sample + ICI Initial Final thiosulphate used in cm3
solution in cm3 (FinaCinitial)
1.
2.

143.5 Calculations and Result

The iodine value (I.V.) is given by the formula:

12.69xMx(V0 - VIl
LV. =
m
where: Vo = Volume of sodium thiosulphate used in blank titration
Chemical Lab-V Vl = Volume of sodium thiosulphate used i n original titration
M = Molarity of sodium thiosulphate
m = mass of the oil.

14.4 Determination of Acid Value

\

rancidity: strong Acid value of oils or fats indicates the.amount of free fatty acid present in it. The acid
taste or smel when the oil or fat
is going bad value can give the extent of rancidity in a sample. The acid value can be defined as
"the number of mg of potassium hydroxide required to neutralise the free fatty acid
present in 1 gm of oil or fat.

This standard is applicable to animal and vegetable oils and fats. It is not applicable
to waxes.

14.4.1 Principle
Solution of a known quantity of the fat to be analysed in a mixture of ethanol and
diethylether, followed by titration of the free fatty acids present with an ethanolic
solution of KOH.

14.4.2 Requirements
~pparatus Chemical
1. Conical flask (250 em3) 2 NaOH
2. Burette (25 cm3) 1 Ethanol
3. Pipitte (25 cm3) 1 Phenolphthalein
KOH
Diethyl ether.

Solution Provided

Diethyl ether may be I. Solvent: It can be prepared by mixing equal volume of 95% ethanol and
substituted by toluene diethyl ether, then it is neutralized shortly before use, with 0 . M NaOH in
presence of 0.3cm3 of phenolphthalein solution per 100 cm3 of the mixture.

2. Potassium hydroxide: 0.1M. It can be prepared by dissolving 5.4 g KOH in

water in 1 dm3 volumetric flask. It can be standardized by 0.2 M standard
oxalic acid solution.

3. Phenolphthalein indicator: 1% solution in 95% ethanol.

14.4.3. Procedure
.
The weight of the oil are chosen in accordance with the following table.

Expected k V Approx. amount of oil in g

1 20
1-4 10
4-15 2.5
15-75 0.5

1. Weigh accurately appropriate quantity of oil in a 250 cm3 conical flask.

2. Dissolve the oil in about 150 cm3 of the solvent mixture. (mixture of ethanol
and ether). Shake the mixture t o dissolve the oil.
 Add few drops of phenolphthalein. Analysis of oils and Fats:
3.
4. Titrate the mixture, keep shaking, with the standard solution of KOH until
pink C O ~ O Udisappears.
~ * If the solution becomes
Record the volume of KOH used in Observation Table-V. Repeat the. cloudy during titraction, add
5.
further quantity of solvent
experiment to get at least two correspondent readings. mixture

Note: If the quantity of O.1M KOH solution required exceeds 20 cm3, 0.5M solution
should be used.

14.4.4 Observations
Mass of the weighing bottle, = m1 -
- ...g
Mass of the bottle + oil, = m2 -
- ... g
Mass of the bottle, = m3 - ... g
(after transferring the oil)
Mass of the oil transferred, = m2-m3 = ... g
Observation Table-V
Oil Sample solution vs. standard KOH solution

SI.No. Burette Reading Volume of KOH solution

Initial Final used in cm3
(Final-Initial)
1.
2.
3.

14.4.5 Calculations and

Result
The acid value (A.V.) is given by the formula:

A.V. = 56.1xMx x-
v
Wc

where: V = Volume of the KOH solution used

M = Molarity of the KOH solution
m = mass of the oil.