CHEMICAL ENGINEERING DEPARTMENT, 

 G.P BARAUNI
CHEMICAL ENGINEERING DEPARTMENT,  G.P BARAUNI
 EXPERIMENT No:-1
Aim:- To determine the iodine value of oils

Requirements:- Iodine Monochloride Reagent, Potassium Iodide,

Standardized 0.1 N Sodium thiosulphate, 1% Starch indicator solution, Reagent bottle,
Chloroform, Fat sample in chloroform, Iodination flask, Burette and burette stand with
magnetic stirrer, Glass pipette, Measuring cylinder, Distilled water.

Theory- Fats and oils are a  mixture of triglycerids. Triglycerides are made up of three fatty
acids linked to glycerol by fatty acyl esters. Fatty acids are long chain hydrocarbons with
carboxyl groups (COOH groups). These fatty acids can be classified into saturated or
unsaturated based on the number of double bonds present in the fatty acid. Saturated fatty
acids contain only single bond between the carbon atoms and are tend to be solids at room
temperature. Unsaturated fatty acids contain double bonds between the carbon atom in
addition to the single bonds present in the fatty acid chain. They are likely to exists as liquids
at room temperature. The double bonds present in the
naturally occurring unsaturated fats are in the Cis form.
Trans fatty acids are associated with health problems and
cardiovascular diseases.
 
Unsaturated fatty acids can be converted into saturated by the process of hydrogenation.
Depending upon the degree of unsaturation, the fatty acids can combine with oxygen or
halogens to form saturated fatty acids. So it is important to know the extend to which a fatty
acid is unsaturated.  There are  different methods for checking the unsaturation level in fatty
acids, one among them is by determining the iodine value of fats. Iodine value or number is
the number of grams of iodine consumed by 100g of fat. A higher iodine value indicates a
higher degree of unsaturation.

Procedure-

1. Arrange all the reagent solutions prepared and the requirements on the table.
2. Pipette out 10ml of fat sample dissolved in chloroform to an iodination flask labeled as
“TEST".
3. Add 20ml of Iodine Monochloride reagent in to the flask. Mix the contents in the flask
thoroughly.
4. Then the flask is allowed to stand for a  half an hour incubation in dark.
5. Set up a BLANK in another iodination flask by adding 10ml Chloroform to the flask.
6. Add  to the BLANK, 20ml of Iodine Monochloride reagent and mix the contents in the flask
thoroughly.
7. Incubate the BLANK in dark for 30 minutes.
8. Mean while, Take out the TEST from incubation after 30 minutes and add 10 ml of
potassium iodide solution into the flask.
9. Rinse the stopper and the sides of the flask using 50 ml distilled water.
10. Titrate the “TEST” against standardized sodium thiosulphate solution until a pale straw
colour is observed.
11. Add about 1ml starch indicator into the contents in the flask, a purple colour is observed.
12. Continue the titration until  the color of the solution in the flask turns colourless.
13. The disappearance of the blue colour is recorded as the end point of the titration.
14. Similarly,  the procedure is repeated for the flask labeled ‘Blank'.
15. Record the endpoint values of the BLANK .
16. Calculate the iodine number using the equation below:
 
 
Observation-
Volume of Sodium thiosulphate used  =  [Blank- Test] ml

Calculations-

 
        
 
                                     

Result:-
Equivalent Weight of Iodine = 127
Normality of sodium thiosulphate ( Na2S203) = 0.1
 EXPERIMENT No:-2
AIM – To determine the Saponification value of given oil sample.

APPARATUS REQUIRED – Beaker, stirrer, conical flask, glass, pipette, burette, standard flask,
water bath.

CHEMICALS REQUIRED – Given sample of oil, ethanol, 0.5N KOH, 0.5N HCl,
Phenolphthalein indicator.

THEORY – The saponification number is the number of milligrams of potassium hydroxide

required to neutralize the fatty acids resulting from the complete hydrolysis of 1gm of fat. It
gives information concerning the character of the fatty acids of the fat- the longer the
carbon chain the less acid is liberated per gram of fat hydrolysed. It is also considered as a
measure of the average molecular weight (or chain length) of all the fatty acids present. The
long chain fatty acids found in fats have low saponification value because they have a
relatively fewer number of carboxylic functional groups per unit mass of the fat and
therefore high molecular weight.

PROCEDUERE –
1) Weigh 5 gm of fat in a tared beaker and dissolve in about 25 ml of the fat solvent
[ ethanol /ether mixture].
2) Add 25 ml of 0.5N alcoholic KOH and mix well, attach this to a reflux condenser.
3) Set up another reflux condenser as the blank with all the other reagents present
except the fat.
4) Place both the flasks in a boiling water bath for 30 minutes.
5) Cool the flasks to room temperature.
6) Now add phenolphthalein indicator to both the flasks and titrate with 0.5N HCl.
7) Note down the end point of blank and test.
8) The difference between the blank and test reading gives the number of millilitres of
0.5N KOH required to saponify 5 gm of fat.

CALCULATIONS –
Weight of the oil Sample = W gm

Saponification value or number of fat = mg of KOH consumed by 1 gm of fat

Weight of KOH = Normality (N) of KOH * Equivalent weight * Volume of KOH in ml

Volume of KOH consumed by W gm fat = [Blank (B) – Test (T)] ml

SAPONIFICATION VALUE = [56 *(B - T)*N]/W

RESULT – The saponification value of an oil sample is found to be ______________

 EXPERIMENT No:-3
AIM- To determine the Acid Value of given oil sample

APPARATUS- Beaker,Stirrer,conical flask,glass,pipette,burette,standard flask,water bath

CHEMICALS REQUIRED- given sample of soap,methyl alcohol,phenolpthalene

indicator,.5N KOH solution

THEORY- Acid value denotes the ratio of free fatty acid found in an fat or oil and could be
referred to as the quantity of milligrams of caustic potash needed to counteract the acid in
one gram of the sample.The regular acid of majority of samples lies within 0.5.In the event
that any titratable acid besides fatty acid is found in the sample,it is going to be an error.An
high acid value implies stale oil or fat has been stored in unsuitable conditions.

PROCEDURE-
1)About 5gm of oil sample is taken in a conical flask.

2)Dissolved in 50ml methyl alcohol by gentle warming

3)It is then titrated against 0.5N KOH using phenolpthalene indicator until a slight pink
colour appears

4)For this titre value,the acid value is calculated by the following equation

CALCULATION-
VxNx56
Acid value A= W

Where

1)volume of alkali added in mL

2)N is the normality of KOH

3)w is the weight of oil sample taken in grams

4)56 is the equivalent mass of KOH

RESULTS-

The acid value of the oil sample is found out to be -------------------

 EXPERIMENT No:-4
Aim—To determine the moisture content in given soap sample.

Requirements—China dish, oven, weighing machine and soap scraps.

Theory—Soap is a salt of fatty acid. Soap is produced by process saponification , where

fats(from plants and animals) is first hydrolyzed into free fatty acids, which then combine
with alkali to form crude soap and glycerol often called glycerin is liberated and is either left
or washed out & recovered. Fats of plants and animals also contain some water content.
Water is used to dilute lye crystals &act as a carrier for the lye. The less water in the recipe,
the faster would be the saponification. Soap with high water content will take longer time to
unmold and longer to dry presence of water also prevents cracking and absence of water also
causes the recipe to become too thick to flow.

Procedure--
1.Weigh accurately 5 grams of soap scraps and put them into china dish.

2. This china dish is now put into oven maintaining at temperature around 70 to 80 degrees
Celsius

3. After 45 minutes of heating, the china dish was taken out and measures the weight of soap
scraps again.

4. Note this reading.

5. Then again put these scraps back into oven for at least 15 minutes.

6. After that again measure the weight.

Observations--
 Initial weight of soap scraps=5.002gm
 Weight of china dish=40.5gm

After ½ hour—

Final weight of soap scraps =_______gm

Calculation—
%moisture content= {initial weight-final weight}*100/initial weight

=_________*100
=

Result—Moisture content present in given soap scrap is =____%

 EXPERIMENT No:-5
Aim: To determine the aniline point of given oil sample.
Apparatus: Aniline point apparatus, Thermometer, Electric heating device, pipette etc.

Chemicals Required: Given sample of oil.

Theory: - It is the lowest temp. at which the sample is completely miscible with equal vol. of
aniline.The minimum equilibrium soln. temp. of a mixture of two volume of aniline, 1vol. of
sample and 1vol. of n- heptane of specific purity. Aniline point of a oil gives the indication of
possible detoration of a rubber sealing, packaging etc. in contact with oil. The aromatic
hydrocarbon has a tendency to dissolve certain type of rubber, so low aromatic content is
desired for the oil. Lighter the paraffin content, higher is the aniline point and cetane number
at the same time minimum is the knocking in the diesel fuel.

Procedure:
1. Clean and dry the ‘U’ tube and arrange the apparatus desired. Now add 20ml. of
distilled aniline and 20ml. of given sample in the ‘U’ tube, it will form two layers.
2. Arrange the apparatus with stirrers in such way that liquid in ‘U’ tube and the paraffin
of the beaker are stirred simultaneously.
3. Switch on the heater to heat the paraffin at a controlled rate, so there is no much
difference in temp. of paraffin bath and ‘U’ tube.
4. The minimum temp. at which two layers give a single phase is noted as aniline point.
5. Now stirring of ‘U’ tube mixture is stopped, and mixture is allowed to cool. Temp. at
which two layers are formed is also considered as aniline point.

Observations--
(1) Vol. of Aniline taken = -------------
(2) Vol. of Kerosene/ Diesel taken = ---------
(3) Cloud formation temp. = -----------
(4) One phase temp.(Aniline point) = ---------
(5) Two phase formation temp. = -----------

Results:
 Aniline point of the given sample = --------------