Name of the experiment: Determination of Iodine Value (IV) of sample oils.

Theory:
This experiment is bases on iodometric titration. 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 (π) bonds and produce iodides. 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.
In this experiment henus solution is needed. 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.
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 I2 and produce tri-iodide inclusion complex which is
colored deep blue. When the reaction ends the blue color disappears.
Chemistry involved:
1. Required reagents:
a. CCl4
b. Hanus solution
c. Sodium thiosulfate solution(0.1N)
d. Starch solution
2. Chemical reactions:
2KI + Br2 = I2 + KBr
- -
I2(aq) + I (aq) → I (aq)
3

I-3(aq) + S2O3-2(aq) → 3I-(aq) + S4O6-2(aq)

Procedure:
A definite amount of Henus solution is added with 1 g of given sample of oil. Before this
the oil should be dissolved is a non-polar solvent such as CHCl3. Some KI solution is also
added. Some iodine will be produced and a amount from it will reacted with oil’s
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 Na 2S2O3 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. The liberated
bromine react with added KI and liberate I2. Then this remaining Iodine is titrated with
standard Na2S2O3 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). Finally, the
tri-iodide is reacted in yet another oxidation-reduction step back to iodide, in the presence
of thiosulfate ion (S2O3-2), with the formation of tetrathionate ion (S4O6-2).

Data tables:
Table-1:Standardization of Na2S2O3 with standard K2Cr2O7 solution
Volume of Burette reading(ml) Volume of Average Volume of
No. of K2Cr2O7
Na2S2O3 Na2S2O3
Obs. taken Initial Final ml ml
ml
1 0.1 10.4 10.3
2 10 10.4 20.6 10.2 10.2
3 20.9 31.0 10.1

Table-2: Data for titration without sample

Difference (A) of
Hanus solution taken Initial burette Final burette
Na2S2O3 burrtte
in the experiment reading of Na2S2O3 reading of Na2S2O3
reading
ml ml ml
ml
10 31.0 43.9 12.9
Table-3: Data for titration with sample
Difference (A) of
Hanus solution taken Initial burette Final burette
Na2S2O3 burrtte
in the experiment reading of Na2S2O3 reading of Na2S2O3
reading
ml ml ml
ml
10 10 19.5 9.5
Coconut oil taken=0.479g
Calculation:
1. Standardization of Na2S2O3 with standard K2Cr2O7 solution:

Here, Volume of K2Cr2O7, V1 = 10 ml

Volume of Na2S2O3, V2 = 10.2ml
Normality of K2Cr2O7, N1 = 0.1 N
V 1×N 1
Normality of Na2S2O3, N2 =
V2
10× 0.1
=
10.2
=0.098N

2. Iodine value:
 12.7 ( B−A ) N
I.V.=
W
12.7 (12.9−9.5 ) 0.098
=
0.479

=8.834

Result:
The Iodine Value (IV) Of Sample Coconut Oil =8.834

Discussions:
 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.
 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 π bonds. I 2is not a polar molecule, but
the π 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 unsaturation 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.

Name Of The Experiment: Determination Of Saponification Values (SV) Of Sample

Oils.

Theory:
Saponification value may be defined as the amount in milligrams of potassium hydroxide
required to saponify 1 gram of oil or fat.
Oils and fats usually are the esters of long chain fatty acids. So from the saponification
value we can know about the quality of the oil and the mean relative molecular weight of
the glycerides and acid presents. The saponification value is usually used, where in
analytical work the saponification equivalent is more useful, as it gives the immediately
the mean molecular weight and acids presents.
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 is-

Long chain aster of fatty acids+ water = free fatty acid + glycerin
Free fatty acid + KOH = soap + water

Total reaction:

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.

Procedure:
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.
To estimate the saponification of a sample of oil or a fat at first we have to hydrolyze this
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.
Chemistry involved:
1. Required reagents:
a. Alcoholic KOH
b. HCl,0.5N
c. Phenolphthalein indicator
2. Chemical reactions:

CH2—O—CO—C17H35 CH 2OH
| |
CH—O—CO—C17H35 + 3KOH → CHOH + 3C 17H35COOK
| |
CH2—O—CO—C17H35 CH2OH

Stearin glycerol
potassium stearate

Data table:
Table-1: Determination of concentration of HCl with standard Na2CO3
Volume of Burette reading(ml)
No. of Na2CO3 Volume of Average Volume of
Obs. taken Initial Final HCl ml HClml
ml
1 10 0.5 8.7 8.2 8.3
2 8.8 17.2 8.4
 3 17.3 25.6 8.3
Table-2: Standardization of KOH(alc) with sample against HCl
Volume of KOH Burette reading(ml) Volume of
taken
Initial Final HCl ml
ml
20 25.2 32.9 7.7
Table-3: Standardization of KOH(alc) without sample against HCl
Volume of KOH Burette reading(ml) Volume of
taken
Initial Final HCl ml
ml
20 20.4 37.9 17.5
Calculation:
1. Standardization of HCl with standard Na2CO3 solution:

Here, Volume of Na2CO3, V1 = 10 ml

Volume of HCl, V2 = 8.3ml
Normality of Na2CO3, N1 = 0.5 N
V 1×N 1
Normality of HCl, N2 =
V2
10× 0.5
=
8.3
=0.602N

56.1 ( V 0−V ) N
Saponification value, S.V.=
W
56.1 ( 17.5−7.7 ) 0.6
=
1.276
=258.52

Result:

The saponification value (SV) for coconut Oil = 258.52

Discussion:
 In our experiment we analyze a sample of hair oil and we have got a value of
 The saponification value is inversely proportional to the molecular weight of the fatty
acids obtained from esters.
 The solution of HCl must be standardized properly before titration carried out.
 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.
  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.)

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
 Alcohol.

Experimental Data:
Table-1:Data for standardization of KOH with oxalic acid.
Volume of Burette reading(ml) Volume of
No. of oxalic Average Volume of
KOH
Obs. acid taken Initial Final KOH ml
ml
ml
1 14.6 26.2 11.6
2 10 26.2 37.7 11.5 11.6
3 37.7 49.4 11.7

Table-2: Data for titration for sample coconut oil:

Burette Reading Volume of KOH
Oil taken(gm)
Initial (ml) Final (ml) (ml)
1.155 1.4 6.2 4.8

Calculation:
Here,
Weight of the sample coconut oil, W = 1.155gm
10× 0.01
Normality of KOH solution, N =
11.6
=0.0086N
Volume of KOH in ml, V = 4.80 ml
 56.1(N × V )
∴ Acid Value (AV) =
W
=56.1 ¿ ¿
= 2.1

Result:
The Acid Value (AV) of Sample Coconut Oil = 2.1

Discussion:
 The measurement of such acidic properties is more important in case of edible
oils.
 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 won’t be able to get exact
result.
 From the experiment we can know how to measure the mean molecular weight
of fatty acid of oils or fats.
 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.
 From the above experiment we can see that the measure of acidic properties of
oil can be obtained.