Oil analysis:

Oil analysis refers to the analysis of oil or fats to determine the properties of
oil, which are important in different purposes. These values are important in
different circumstances. We have to know the number of instaurations or double
or triple bonds in an oil or fat while using in chemical reactions or industrial
purposes. Iodine value indicates the number of double/triple bonds. On the other
hand, if we want to produce soap, for best production we have to select suitable
oil, which will produce more soap & is easy to collect. For this purpose we have
to know the saponification values of different oils. We must know the acidity or
alkalinity of oil while using it in chemical reactions, even in hair care. So we will
use some experimental way of determining the properties of oil. These
experiments are DETERMINATION OF IODINE VALUE (IV) OF OILS
DETERMINATION OF SAPONIFICATION VALUE (SV) OF OILS
DETERMINATION OF ACID VALUE & BASE VALUE OF OILS.

Name of the Experiment:

Determination of Iodine Value (IV) of sample oils.

Objective:

The objective of this experiment is to determine the number of instaurations

present in sample oil. The measurement of this property of oil is the iodine value.
Iodine value indicates the number of double or triple bonds in an oil molecule. In
this experiment we have to use non-polar solvents to dissolve the oil in iodine.
This introduces us using non-polar solvents in titration.

Theory of this Experiment:

Iodine Value- Iodine value can be defined as the amount of iodine in grams
reacted with 100 grams of a oil or fat under saturated condition, and is measure
of the instaurations present. Iodine value (IV) is a measure of the total number of
double bonds present in fats and oils. It is generally expressed in terms of
"number of grams of iodine that will react with the double bonds in 100 grams of
fats or oils".
Oils have double bonds & iodine replaces the pai () bonds and produce iodides.

C C

+ I2

I
I

CC

I
I

This amount of iodine reacted with oil sample is the iodine value. Higher the
iodine value indicates the higher instauration. So in case of edible oils with high
iodine value are usually less stable and more susceptible to oxidation and a
better quality of oil but in case of coconut hair oil this means rather different.

Henus Solution- Henus solution is a special type of reagent used in this

experiment. The reagent is prepared by dissolving 10gm iodine monobromide in
500 c.c. Glacial acetic acid, purified and free from alcohol, in a glass stopper
bottle preferably made of yellow glass. It is used as the source of iodine. Here
Iodine is present as Iodide of bromine (IBr). The reagent is free from alcohols.
This solution reacts with KI & produces I2.

Indicator: In fact this experiment is bases on iodometric titration. At the last

step of the experiment we used to standardize remaining I 2 in the solution with
Na2S2O3 solution. As it is a redox titration, starch was used as indicator in the
reaction. Starch adsorbs the remaining I 2 and produce tri-iodide inclusion
complex which is colored deep blue. When the reaction ends the blue color
disappears.

Method of the experiment- A definite amount of Henus solution is added with

1 g of given the sample of oil. Before this the oil should be dissolved is a nonpolar solvent such as CHCl 3. Some KI solution is also added. Some iodine will be
produced and a amount from it will reacted with oils unsaturated asters and
some will remain. The reaction is complete after approximately 30 min, at which
time potassium iodide is added. This remaining iodine can be titrated by standard
Na2S2O3 solution using a starch solution as the indicator. We have to do a
titration of blank (without oil or fats) in which Henus solution added is same for
above titration. The difference of these two values will give the volume of
Na2S2O3 solution as well the amount of iodine required to react with the oil &
eliminate the instauration.
Here IBr from henus solution react with the oils and liberate bromine.

C C

+ IBr

I
I

CC

I
I

Br2

The liberated bromine reacts with added KI and liberates I 2

2KI

Br2

I2

KBr

Then this remaining Iodine is titrated with standard Na 2S2O3 solution. This
titration is a iodometric titration. There is still excess iodide in the sample, and it combines
with the iodine to form tri-iodide ( I-3):
I2(aq)

I-(aq)

I-3 (aq)

Finally, the tri-iodide is reacted in yet another oxidation-reduction step back to iodide, in the
presence of thiosulphate ion (S2O3-2), with the formation of tetrathionate ion (S 4O6-2):
I-3(aq)

S2O3-2(aq)

3I-(aq)

S4O6-2(aq)

Useful Chemicals:

Sample oil (Parachute Coconut Oil)

Carbon tetrachloride (CCl4)
Iodine reagent (Henus solution)
Sodium thiosulphate solution 0.1N
Starch solution
Chloroform (CHCl3)
12% Potassium Iodide solution (KI)

Experimental Data:
Table 1: Standardization of Sodium thiosulphate (Na 2S2O3) solution with
standard potassium dichromate (K2Cr2O7) solution:
No. of
Volume of
Burette reading
Volume of
Average
Obs.
K2Cr2O7 (ml) Initial (ml) Final (ml)
Na2S2O3
volume of
(ml)
Na2S2O3 (ml)
1
10
0.2
15.1
14.9
14.933
2
10
15.1
30.0
14.9
3
10
30.0
45.0
15.0
Sample (Parachute Coconut Oil) Oil taken, W = 0.728 gram

Table 2: Data for titration of sample oil with Na2S2O3:

No. of
Obs.
1

Burette reading of Na2S2O3 (ml)

Initial
Final
0.20
18.40

Table 2: Data for blank titration:

No. of Obs.
Burette reading of Na2S2O3 (ml)
Initial
Final
1
0.10
33.60

Calculations:
Weight of the sample Lily Coconut Oil, W = 0.728 gm
Strength of Na2S2O3, N =

0.1 10
N
14.933

= 0.0676 N
Volume of Na2S2O3 in blank titration, B = 32.7 ml
Volume of Na2S2O3 in sample titration, A = 11.5 ml
12.7 B A N
Iodine Value, IV =
W
12.7 33.5 18.20 0.0676
=
0.728
= 18.043

Result:
The Iodine Value (IV) Of Sample Lily Coconut Oil = 18.043

Volume of
Na2S2O3 (ml)
18.20
Volume of
Na2S2O3 (ml)
33.50

Discussion:
Here while determining iodine value Iodine was not added directly. It was added
as Ian iodine reagent henus solution where iodine is present as IBr. If we use
iodine directly the reaction would not be done easily as the reaction mechanism
does not support iodine to directly with the bonds. I 2is not a polar molecule, but
the bonds reacts easily with polar molecules. On the other hand the IBr
molecule is polar which reacts easily with unsaturated oils & fats.
The measure of such instauration is more important in case of edible
oils. So in case of edible oil high iodine value is more favorable than
that of a lower one.
To perform the experiment more accurately we must have to shake the
reagents mixture for about an hour otherwise the saturation may not
be occurred. And some disappearances have to be observed from the
standard value.

NAME OF THE EXPERIMENT:

DETERMINATION OF SAPONIFICATION VALUE (S.V.)

Objective:
The objective of this experiment is to determine the saponification value of oils
or fats. The saponification value is usually used, where in analytical work the
saponification equivalent is more useful.

Theory of the Experiment:

To determine the saponification value of oil we have to reflux the oil with a
specific amount of alcoholic KOH for half an hour. After completing the
saponification reaction we have to determine the amount of KOH used to
naturalize total oil through titremetric analysis.
Saponification value (or "saponification number") represent the number of
milligrams of potassium hydroxide or sodium hydroxide(NaOH) required to
saponify 1g of fat under the conditions specified. It is a measure of the average
molecular weight (or chain length) of all the fatty acids present. As most of the
mass of a fat/triester is in the 3 fatty acids, it allows for comparison of the
average fatty acid chain length. If there are more moles of potassium hydroxide
(KOH) used for 1 gram of fat then there are more moles in the fat. Therefore the
chain lengths are smaller, due to the equation: Number of moles = mass of
oil/relative atomic mass. The relative atomic mass would be smaller with smaller
fatty acid chains, meaning more moles. The higher the saponification value the
smaller the chain lengths.
The reaction responsible for production of soap is defined as saponification
reaction. It is actually the hydrolysis reaction of esters. Oils and fats usually are
the esters of long chain fatty acids. the typical reaction of saponification isLong chain aster of fatty acids+ water = free fatty acid + glycerin
Free fatty acid

KOH =

soap

water

Total reaction:
CH2OCOC17H35
|
CHOCOC17H35
|
CH2OCOC17H35
Stearin
potassium stearate

+ 3KOH

CH2OH
|
CHOH
|
CH2OH

3C17H35COOK

glycerol

To estimate the saponification of a sample of oil or a fat at first we have to

hydrolyze the sample properly by alcoholic KOH then we can easily calculate the
excess KOH (A) by titration with standard HCl solution. Then we have to do a
blank titration (without oil or fats). The difference of theses two measurements

will give the value of HCl solution required to neutralize the KOH, which was
involved to saponify the oil if in both case the amount of solution of KOH is same.
Indicator- In the neutralization titration of excess KOH with standard HCl
we used phenolphthalein indicator. This indicator changes its color in
neutralization reactions in pH range 8.3 to 10.

Chemicals:

Alkoholic KOH
HCl, 0.5N
Phenolphthalein Indicator

Experimental Data:
Weight of sample: (Soya bin oil) = 1.121 gm
Table 1: Data for blank titration:
No. of
Vol. of alcoholic
Burette Reading
Obs.
KOH (ml)
Initial (ml)
Final (ml)
1
20
0.10
17.6 0

Volume of HCl (ml)

17.5 0

Table 2: Data for titration of excess KOH with HCl for Soya bin oil:
No. of
Vol. of alcoholic
Burette Reading
Volume of HCl (ml)
Obs.
KOH (ml)
Initial (ml)
Final (ml)
1
20
18.10
27.70
9.60

Calculation:
Here,
Weight of the sample Lily coconut oil, W = 1.121 gm
Normality of HCl, N = 0.532 N
Vol. of HCl in ml use in the titration with sample, V =9.60 ml
Vol. of HCl in ml use in the blank titration, V o = 17.50 ml

Saponification Value, SV = 56.1 Vo V N

W
56.1 17.0 6.8 0.532
=
1.216
= 210.33

Result:
The Saponification Value (SV) Of Sample: (Soya bin Oil) = 210.33

Discussion:
The saponification value is inversely proportional to the molecular
weight of the fatty acids obtained from esters.
To do the experiment perfectly we should reflux the reagents
mixture in water bath for about 24h otherwise we may have some
disappearances. There may some disappearances due not to
hydrolyze the fat properly because we spent only half an hour
instead of 24 hour.
The solution of HCl must be standardized properly before titration
carried out.
From the experiment we can know how to measure the purity of
oils or
fats.
This saponification value must vary from source to source of oil and
fat such as the saponification value of edible pure oil, pure fat,
and hair oil must be different.

NAME OF THE EXPERIMENT:

DETERMINATION OF ACID VALUE (A.V.)

Object of the experiment:
The objective of this experiment is to determine the acid value of oils or
fats. The acid number is a measure of the amount of carboxylic acid groups in a
chemical compound such as a fatty acid. n a typical procedure, a known amount
of sample dissolved in organic solvent is titrated with a solution of potassium
hydroxide with known concentration and with phenolphthalein as a color
indicator.

Theory of the Experiment:

Acid value (or "neutralization number" or "acid number" or "acidity") is the
mass of potassium hydroxide (KOH) in milligrams that is required to neutralize
free fatty acid in 1 gram of fat or oil. This value enables the free fatty acid in an oil
or fat to be calculated or mean molecular weight of fatty acids to be determined.
It is used as criterion of edibility and a limit to the value is usually set for
lubricating and pharmaceutical fats.
The functional and nutritional values of different vegetable oils are
dependent on the nature of the different fatty acids which are incorporated like
building blocks into the oil (triacylglycerols). For example, erucic acid makes up
about 50% of the fatty acids of traditional rapeseed oil and is the desired product
for most industrial uses of this oil. Fatty acid composition is mostly effected by
variety and growing environment. It is important to know the effect of
environment on the fatty acid composition of any seeds in order to determine
where seed can be harvested to make oils meeting the specifications for
saturated fatty acids required. Similarly, it is important to know which areas
produce the effective seeds of desirable oil with levels of iodine value suitable for
coating manufacture.
Indicator: Phenolphthalein is a sensitive chemical with the formula
C20H14O4 (often written as "HIn" in shorthand notation). Often used in titrations, it
turns colorless in acidic solutions and pink in basic solutions. If the concentration
of indicator is particularly strong, it can appear purple. In solutions containing a
pH below 0, phenolphthalein turns a bright orange color.

Figure: Phenolphthalein
In a typical procedure, a known amount of sample dissolved in organic
solvent is titrated with a solution of potassium hydroxide with known
concentration and with phenolphthalein as a color indicator.

Chemicals:

KOH solution
Phenolphthalein Indicator

Experimental Data:
No.
Obs.
1

Table 1: Data for titration for sample Parachute coconut oil:

of Vol. of alcohol Burette Reading
Volume of KOH (ml)
(ml)
Initial (ml) Final (ml)
30
0.80
3.60
2.80

Calculation:
Here,
Weight of the sample Lily coconut oil, W = 0.927 gm
Normality of KOH solution, N = 0.01 N
Volume of KOH in ml, V = 2.80 ml

Acid Value (AV) = 56.1 N V

W
= [56.10.012.80]/ 0.927
= 1.694

Result:
The Acid Value (AV) Of Sample Lily Coconut Oil = 1.694

Discussion:

From the experiment we can know how to measure the mean

molecular weight of fatty acid of oils or fats.
From the above experiment we can see that the measure of acidic
properties of oil can be obtained.
The measurement of such acidic properties is more important in
case of edible oils.
So in case of edible oil low AV is more preferable than that of a
higher one.
For the presence of free acid in the solution low concentrated KOH
is used.
To perform the exp., we must have to heat the solution at 40-50 C
for sometime and the titration was done quickly. Otherwise we wont
be able to get exact result.

BIBLIOGRAPY:
VOGELS
TEXTBOOK OF QUANTATIVE CHEMICAL ANALYSIS
-J MENDHAM, R C DENNEY, J D BARNES, M J K THOMAS.
GENERAL CHEMISTRY
-EBBINGS.
ESSENTIALS OF PHYSICAL CHEMISTRY
-B S BHAL, G D TULI, ARUN BHAL.