Haldia Institute of Technology

Engineering Chemistry Laboratory (CH 191 &CH 291)

Name of the experiments:
1. Conductometric titration for determination of the strength of a given HCl solution by titration against a
standard NaOH solution.
2. pH- metric titration for determination of strength of a given HCl solution against a standard NaOH
solution.
3. Determination of dissolved oxygen present in a given water sample.
4. To determine chloride ion in a given water sample by Argentometric method (using chromate indicator
solution)
5. Determination of surface tension and viscosity
6. Thin layer chromatography
7. Ion exchange column for removal of hardness of water
8. Determination of the rate constant of a reaction
9. Determination of cell constant and conductance of solutions
10. Potentiometry - determination of redox potentials and emfs
11. Saponification/acid value of oil
12. Chemical analysis of a salt
13. Determination of the partition coefficient of a substance between two immiscible liquids
14. Adsorption of acetic acid by charcoal
15. Use of the capillary viscosimeters to the demonstrate of the isoelectric point as the pH of minimum
viscosity for gelatin sols and/or coagulation of the white part of egg.

Experiment No: 1
Name: Conductometric titration for determination of the strength of a given HCl
 solution by titration against a standard NaOH solution.

Theory:
The monobasic acid HCl being a strong electrolyte undergoes complete ionization and
produces a large number of cations and anions in solution. Moreover ionic conductance of H +
ions being highest (I0 H+ = 350). Thus the initial conductance of a solution will be very high.

When this acid is gradually titrated against a base NaOH, being added from burette, the
following reaction will occur.

H+ + Cl- + Na+ + OH- → Na+ + Cl- + H2O

The salt, a strong electrolyte remains in the solution in completely ionized form, while water
being a very weak electrolyte (   10
9
and in presence of H+ ions its ionization is still smaller)
remains partially ionized.

Thereby H+ ions are gradually replaced by equivalent amount of Na + ions which have relatively
much lower ionic conductance than that of H+ ions. Thus the conductance of resulting solution
will decrease steeply.

This trend will continue until all the H+ ions are replaced by Na+ ions i.e. equivalent point is
reached. At equivalent point only NaCl is present.

Beyond equivalent point when further amount of alkali is added Na + and OH- of excess alkali
remain in the solution unutilized. Consequently the conductance of the solution increases due to
the presence of newly added Na+ and OH- ions (Io OH- = 200).

The point of intersection of curve representing the variation of conductance with the volume of
alkali added, corresponding to the minimum conductance and consequently equivalence point.

The volume of alkali added corresponding to the equivalent point represents the volume of alkali
required for neutralization of acid.
Instruments and apparatus:

 Conductivity meter

 Conductivity cell

 Beaker

 Burette

 Pipette

 Volumetric flask

 Conical flask

 Funnel

Materials:

N
 
 Standard oxalic acid  10 
N
 
 2 NaOH solution
N
 
 HCl solution
 10 

 Phenolphthalein indicator

Procedure:

N
 
1. Prepare 100 ml of standard oxalic acid order  10  .

N
 
2. Prepare 250 ml of an approximately  2  NaOH solution and standardize it against oxalic acid
solution using phenolphthalein as indicator.

N
 
3. Prepare 250 ml of an approximately  10  HCl solution.

4. Rinse the conductivity cell with de-ionized water.

5. Pipette out 25 ml of HCl solution into the conductivity cell and add water if necessary, so that both the
electrodes are completely immersed within the solution. Join the cell with the conductive bridge and
measure the conductivity very carefully.

6. Add NaOH solution from a burette dropwise.

7. Measure the conductance of the solution after addition of 10 drops of NaOH and mildly shaking the
beaker. Repeat the process until you have at least six points beyond the end points.

8. Draw a curve by plotting the conductance against the drops of alkali added, find the end point and
calculate the strength of the HCl solution.

Results:

Table 1: Weighing of oxalic acid

Initial Final weight(gm) Weight Weight to be Strength

weight(gm) taken(gm) taken(gm)

w
W1 W2 W1-W2 = w 1.575 1.575 (N/10)

Table2: Standardization of NaOH solution by standard oxalic acid

No. of Volume of Burette reading of NaOH Volume of Strength of Strength of

observation oxalic acid NaOH (ml) oxalic acid NaOH
(ml)
Initial(ml) Final(ml)

Table 3: Conductometric Titration of HCl solution against NaOH solution.

No of observation Volume of HCl taken (ml) Drops of NaOH added Conductance

1 25 0

2 10

3 20

4 30

5 40

6 50
7 60

8 70

9 80

10 90

11 100

12 110

13 120

14 130

15 140

16 150

Calculations:

Let the number of drops of alkali required to neutralized 25 ml of HCl solution = x

x
Therefore, 20 drops = 1 ml then x drops = 20 ml

V1S1 = V2S 2

where, V1 = Volume of HCl S1 = Strength of HCl

V2 = Volume of NaOH S2 = Strength of NaOH

V2S2
S1 
Then, V1

Precautions:

 Conductivity cell must be thoroughly washed with de-ionized water.

 Ensure that there are no air bubbles in the burette.

 During titration, the beaker should be constantly swirled.

 For each titration, use same number of drops of NaOH solution.

 Experiment No.: 02
Name: pH-metric titration for determination of strength of a given HCl
solution against a standard NaOH solution

Theory:
All pH meters have provision for standardizing the glass electrode in a buffer solution of known
pH.This is necessary because different electrodes have different asymmetry potentials. Once the
adjustment has been made so that the meter Registers correctly known the pH of the buffer solution, the
instrument gives the pH other solution without any calculation.

Measurements of pH are also employed to monitor the course of acid-base titrations. The pH values of the
solution at different stages of acid-base neutralization are determined and are plotted against volume of
1
pHlog 
acid/alkali added. On adding abase to an acid, the pH rises slowly in the initial stages H (pH
range is used for only dilute solution, not for concentrated solution) and then it changes rapidly at the end
point. Then it flattens out. The end point of the titration can be detected where the pH changes most
rapidly. However the shape of the inflexion point (i.e. where the pH changes abruptly) and symmetry of
the curve on its two sides depends upon the ionisability of the acid and the base used and on the basicity
of the acid and the acidity of the base.

Apparatus:

 pH meter with glass electrode and standard calomel electrode.

 Beaker

 Burette

 Pipette

Materials:

 Buffer solution of pH 4 and 9

N
 
 Standard oxalic acid  10 
 HCl solution
 NaOH solution
 Phenolphthalein indicator

Procedure:

1. Wash the electrodes with distilled water and standardize the pH meter by using buffer solution of pH
=4 and pH=9, now the selector switch is put to a pH range of 7-14.

N
 
2. Prepare 100 ml of standard oxalic acid order  10  .

3. Prepare 250 ml of an approximately NaOH solution and standardize it against oxalic acid solution
using phenolphthalein as indicator.
 N
 
4. Prepare 250 ml of an approximately  10  HCl solution.

5. Clean the electrodes by distilled water and wipe them with tissue paper.

6. Take 25 ml HCl solution in a 100 ml beaker and immerse the electrodes.

7. Add NaOH solution from the burette dropwise. Note the corresponding value from the meter. Near the
end point add very small amount of NaOH as possible because change in pH will be very much
appreciable because when the acid is neutralized, further addition of such a small amount raises the pH to
about 9 or 10.

8. Put back the selector to zero position after pH measurement and before removing the electrodes from
solution

9. Plot a graph between pH and drops of NaOH added. From this graph, determine the volume of NaOH
required for the complete neutralization of HCl.

Experimental Data:

Table 1: Weighing of oxalic acid

Initial Weight Weight to be

Final weight(gm) Strength
weight(gm) taken(gm) taken(gm)

w
W1 W2 W1-W2 = w 1.575
1.575 (N/10)

Table2: Standardization of NaOH solution by standard oxalic acid

Volume Burette reading 0f NaOH

No. of Volume of Strength of Strength of
of oxalic
observation NaOH (ml) oxalic acid NaOH
acid (ml) Initial (ml) Final(ml)

Table 3: pH-metric titration of HCl solution against NaOH solution.

Volume of HCl taken

No of observation Drops of NaOH added pH
(ml)

25

Calculation:
Let the number of drops of alkali required to neutralized 25 ml of HCl solution = x

x
Therefore, 20 drops = 1 ml then , x drops = 20 ml

V1S1 = V2S 2

where, V1 = Volume of HCl S1 = Strength of HCl

V2 = Volume of NaOH S2 = Strength of NaOH

V2S2
S1 
Then, V1

Precautions:

 Electrodes must be immersed properly in the solution and sufficient time to be allowed
for the electrodes to assume the temperature of the solution.

 For pH-metric titration, solution should be stirred mechanically from time to time’

 Leave the selector in zero position when not in use.

Experiment No.: 03
Name: Determination of dissolved oxygen present in a given water sample
Theory:
Dissolved oxygen (DO) determination measures the amount of dissolved (or free) oxygen
present in water or wastewater. Aerobic bacteria and aquatic life such as fish need dissolved
oxygen to survive. If the amount of free or DO present in the wastewater process is too low, the
aerobic bacteria that normally treat the sewage will die. DO is determined by the titrimetric
method developed by Winkler.
1. Dissolved molecular oxygen in water is not capable of reacting with KI, therefore an oxygen carrier such as
manganese hydroxide is used. Mn(OH)2 is produced by the action of KOH on MnSO4.
2. Mn(OH)2 so obtained reacts with dissolved molecular oxygen to form a brown precipitate of basic
manganic oxide, MnO(OH)2.
3. MnO(OH)2 then reacts with concentrated sulphuric acid to liberate nascent oxygen.
4. Nascent oxygen results in oxidation of KI to I2.
5. This liberated iodine is then titrated against standard sodium thiosulphate solution using starch as an
indicator.
6. Thiosulphate reduces iodine to iodide ions and itself gets oxidized to tetrathionate ion. (Refer the reactions
below).
 Iron and nitrite interfere with this procedure. The interference of nitrite can be eliminated by
adding sodium azide. If ferric ion is present, H 3PO4 is used instead of H2SO4
 2NaOH + MnSO4 → Mn(OH)2 + K2SO4
2Mn(OH)2 + O2 → 2MnO(OH)2
MnO(OH)2 + H2SO4 → MnSO4 + 2H2O + [O]
2KI + H2SO4 + [O] → K2SO4 + H2O + I2
I2 + I ‫־‬ → I3 ‫־‬

2S2O3 2─ + I3‫־‬ → 3I— + S4O6 2─

Apparatus Required:

 Burette
 Pipette
 Conical flask
 Beaker
 Measuring cylinder
 Volumetric flask
 Wash bottle
 Glass stoppered bottle

Chemicals required:

 Sodium thiosulfate
 Potassium dichromate
 Potassium iodide
 Sulfuric acid
 Manganese (II) sulfate
 Sodium azide
 Sodium hydroxide
 Ortho phosphoric acid
 Starch

Procedure

1. Preparation of 250 ml 0.01(M) sodium thiosulphate solution (Na2S2O3, 5H2O)

Weigh out approximately 0.0620 gm of sodium thiosulphate in a clean 250 ml volumetric flask and
dissolve in small amount of distilled water. Then make up to the volume of the flask with distilled water.

2. Preparation of 100 ml standard 0.01(M) potassium dichromate solution (K2Cr2O7)

Weigh out exact 0.2942 gm of A.R potassium dichromate and transfer it in a 100 ml volumetric flask and
add 50 ml distilled water to it. Dissolve the solid completely in distilled water and then fill the mark with
distilled water.
 W
0. 2949 M
=( ) ×( 100 )

Table 1: Weighing of potassium dichromate

Initial weight(gm) Final weight(gm) Weight taken(gm) Weight to be Strength

taken(gm)
W1 W2 W1-W2 =W 0.2942 -

Therefore, strength of potassium dichromate =

3. Preparation of 100 ml 4(N) H2SO4 solution:

Pour 11 ml of concentrated sulfuric acid in a50 ml of distilled water in a100 ml volumetric flask and then
dilute the solution to 100 ml with distilled water and mix properly.

4. Preparation of 100 ml 20% potassium iodide solution

Dissolve 20 gm of potassium iodide in 100 ml distilled water.

5. Preparation of starch solution

Take 0.1 gm of starch and make a paste with little amount of water. Then pour the paste with

constant stirring to 100 ml of water and boil for 1 minute. Allow the solution to cool at room temperature.

6. Standardization of sodium thiosulfate solution

Pipette out 25 ml of standard potassium dichromate solution in a conical flask. Add 25 ml of 4(N) H 2SO4
and 10 ml of 20% KI solution to it. Cover the conical flask with a watch glass and keep it in dark for 3
minutes. Then dilute the solution with 200 ml of distilled water. Titrate the solution with the sodium
thiosulfate solution running from burette. When the colour of the solution becomes pale yellow, add 2 ml
of the starch solution. The solution will turn blue. Continue the titration until the color changes from blue
to colorless.

Table 2: Standardisation of sodium thiosulfate solution against standard potassium

dichromate solution

No. of Volume of Burette reading of sodium difference Average

observations standard thiosulfate solution(ml)
potassium
dichromate
(ml)
Initial Final
reading(ml) reading(ml)
1
 2
3
4
5

Now, calculate normality of sodium thiosulfate solution;

N1V1 =N2V2

N1= Normality of standard potassium dichromate solution(s)

V1=volume of standard potassium dichromate solution (25 ml)

N2= Normality of sodium thiosulfate solution

V2= volume of sodium thiosulfate solution required

7. Preparation of 100 ml of 50% Manganese (II) sulphate solution

Dissolve 50 gm of manganese (II) sulphate solution in small amount of distilled water and mix well.
Then make up the volume to 100 ml.

8. Preparation of 50 ml Alkaline iodide azide solution

Weigh 2.5 gm of NaOH and dissolve in 50 ml of distilled water. Then dissolve 0.675 gm of KI and 0.5 gm
of sodium azide to the solution and mix well.

9. Determination of dissolved oxygen content by iodometric method

Take 300 ml water sample in a glass stoppered bottle. The bottle always well stoppered to prevent any
sample exposure to air. Now, add 1 ml of 50% manganese (II) sulphate (MnSO 4) to water sample.
Similarly, add 1 ml of alkaline iodide azide solution. Shake well to mix uniformly. A brown precipitate
will be formed. If precipitate not form then add 2 ml of 2 (N) NaOH solution to the water sample and
allowed to settle down for 15 minutes. Then add 2 ml of concentrated phosphoric acid to dissolve the
precipitation. After the complete dissolution of brown precipitate, iodine is released in the solution. Now
pipette out 100 ml of the solution in a conical flask and titrate the liberated iodine with sodium thiosulfate
solution running from the burette. When the colour of the solution becomes pale yellow, add 2 ml of the
starch solution. The solution will turn blue. Continue the titration until the color changes from blue to
colorless.

Table 3: Determination of dissolve oxygen content

No. of Volume of Burette reading of difference Average(V)

observations water sodium thiosulfate solution(ml)
sample(ml)
Initial Final
 reading(ml) reading(ml)
1
2

Calculation:

1000 mL of 1N Na2S2O3 = 8 g oxygen

V mL of y (N) Na2S2O3 = V× y × 8/ 1000 g oxygen = V× y×8 mg oxygen

V1 mL water sample = V× y×8 mg oxygen

V × y × 8 ×1000
1000 mL water sample = mg dissolved oxygen.
V1

Precautions:

 Any sample contact with air should be avoided as per as possible. Exposure of air will lead to higher
results.
 Exclude air bubbles carefully while replacing the stopper.
 Use freshly prepared starch solution for the titration.
 Add starch solution while approaching the end point. If the starch solution is added in highly concentrated
iodine solution, some iodine is absorbed since starch gives water insoluble complex with iodine.
 Experiment No.: 04

Name: To determine chloride ion in a given water sample by Argentometric method (using
chromate indicator solution

Theory:

Chlorides are present in water usually as NaCl, MgCl 2 and CaCl2. Although chlorides are not harmful as
such, their concentrations over 250 pomp impart a peculiar taste to the water thus rendering the water
unacceptable for drinking purposes.

By argentometric method, chloride ions in a water sample (neutral or slightly alkaline) can be determined
by titrating it against standard silver nitrate (AgNO 3) solution using potassium chromate (K 2CrO4) as an
indicator. The pH should be in between 7-8. At higher pH, silver ions are precipitated as silver hydroxide.
At lower pH, potassium chromate indicator is converted to potassium dichromate (K 2Cr2O7).

Argentometric method is based on the precipitation titration in which silver nitrate solution is released
from the burette to the water sample which contains chloride ions and indicator. The silver ions (from
silver nitrate solution) react with chloride ions (from water sample) and chromate ions (from indicator) to
form white precipitate of silver chloride and red precipitate of silver chromate.

Ag+ + Cl- → AgCl (White Precipitate)

2Ag+ + CrO42- → Ag2CrO4 (Red Precipitate)

Red colour formed because of formation of silver chromate disappears initially as the solution contains
high concentration of chloride ions.

Ag2CrO4 + 2Cl- → 2AgCl + CrO42-

When the concentration of chloride ions has decreased, the red colour starts disappearing slowly and
slowly on shaking and a stage is reached when all the chloride ions have formed silver chloride. One extra
drop of silver nitrate at this point reacts with potassium chromate and reddish coloured silver chromate is
formed.
 2AgNO3 + K2CrO4 → Ag2CrO4 + 2KNO3

Apparatus Required:
 Burette
 Pipette
 Conical flask
 Beaker
 Measuring cylinder
 Volumetric flask
 Wash bottle

Chemicals Required:

 Silver nitrate
 Sodium chloride
 Potassium chromate

Procedure:

1.Preparation of potassium chromate indicator

5gm of potassium chromate is dissolved in about 5ml of distilled water. Few drops of silver nitrate are
added until a definite red precipitate forms. It I allowed to stand for 12 hours, filtered and diluted to 100
ml with distilled water.

2. Preparation of 1000 ml
(50M ) standard sodium chloride (NaCl) solution

Weigh out about 1.17 gm of NaCl and transfer in a1000 ml volumetric flask and add small amount of
distilled water to it. Dissolve completely the solid in distilled water and fill the mark with distilled water
and mix thoroughly.

Table 1: Preparation of
(50M ) standard sodium chloride (NaCl) solution

Initial weight(gm) Final weight(gm) Weight taken(gm) Weight to Strength

be taken(gm)
W1 W2 W1-W2 = W 1.17 -

Therefore, the strength of standard sodium chloride solution is =

3. Preparation of silver nitrate solution

Weigh about 3.4 gm of silver nitrate and dissolve in 50 ml of distilled water and then dilute to 1000 ml in
a dark bottle.

4. Standardization of silver nitrate solution

Pipette out 10 ml of standard sodium chloride solution in a conical flask. Add 5 drops of potassium
chromate indicator to it and titrate the solution with silver nitrate solution running from the burette. A red
color of silver chromate appears and again redissolves. Continue the titration until a pinkish or reddish
tinge persists in the yellow solution with constant swirling of the liquid in the conical flask throughout the
titration procedure.

Table 2: Standardization of silver nitrate solution against standard sodium chloride solution

No. of Volume of Burette reading of silver nitrate difference Average(x)

observations standard solution(ml)
sodium
chloride(ml) Initial Final
reading(ml) reading(ml)

Now, calculate molarity of silver nitrate solution;

M1V1 = M2V2

M1= Strength of standard sodium chloride solution(s) in molarity

V1= volume of standard sodium chloride solution (25 ml)

M2= Strength of silver nitrate solution in molarity

V2= volume of silver nitrate solution required (x)

5. Determination of the amount of chloride ion in the given water sample

Pipette out 25 ml of the water sample in a conical flask. Add 5 drops of potassium chromate indicator to
it and titrate the solution with silver nitrate solution running from the burette. A red color of silver
chromate appears and again redissolves. Continue the titration until a pinkish or reddish tinge persists in
the yellow solution with constant swirling of the liquid in the conical flask throughout the titration
procedure.

Table 3. Determination of the amount of chloride ion in the given water sample

No. of Volume of Burette reading of difference Average(y)

observations water silver nitrate solution(ml)
sample(ml)
Initial Final
reading(ml) reading(ml)
Calculation:

Suppose y ml of the silver nitrate solution is required for the titration of the given water sample.

1000 ml 1(M) silver nitrate solution ¿ 35.5 gm of Cl

= 35.5 gm of Cl

35 .5
¿
1 ml 1(M) silver nitrate solution 1000 gm of Cl

35 .5× y×S2
y ml of S2 (M) silver nitrate solution = 1000 gm of Cl

= (35.5×y×S2) mg of Cl

Therefore,

25 ml sample water contains (35.3×y×S2) mg of Cl

35 .5× y×S2×1000
1000 ml sample water contains 25 mg of Cl

= A mg/L

Therefore, the concentration of the chloride in the given water sample is A mg/L

Precautions:

 Each apparatus should be washed with distilled water which is free of chlorine.
 Carefully handle silver nitrate and avoid any skin contact since silver nitrate is corrosive and leave black
spots.
 Add same amount of potassium chromate indicator each time.
 Perform the titration with constant swirling of the liquid in the conical flask.
 Experiment No. –
Name: Determination of percentage composition of sugar solution from
viscosity

Theory:
When a fluid passes through one another, due to internal friction, it experiences a resistance to its
flow which is known as viscosity. The coefficient of viscosity is a measure of the resistance and defined
as the tangential force per unit area required to maintain unit difference of velocity between two layers
unit distance apart. Its unit in CGS system is dyne.sec/cm 2.

When a homogeneous fluid of volume ‘v’ flows through a capillary tube of length ‘l’, radius ‘r’, in time
‘t’, under a driving force ‘p’, the co-efficient of viscosity is given according to Poisseuille’s formula by

 Pr4 t

8lv

The experimental determination of viscosity is rather different. If

1 and 2 are the viscosity of two
 
different liquids of density 1 and 2 respectively which are successively allowed to fall through the
same length h of capillary e.g. between the marks of an Ostwald viscometer, the pressures are given by h
1 g and h  2 g and thus 1 and 2 are given by

1 = and  2 =

P = Pressure difference between two ends.


1 
t
11

,o
r 

1t
1

 

2 
t
22
1 2

1t
2
where x is the unknown concentration of supplied sugar solution.

Apparatus:

 Viscometer (Ostwald)

 Stop watch

 Stand with clamp

 Pipettes

 Beakers

 Specific gravity bottle

Materials:

 Supplied sugar solution

 Distilled water

Procedure:

The weight of dry specific gravity bottle, filled with water and with supplied solution was
taken. At first 5%, 10%, 15% and unknown sugar solution were prepared by proper dilution. The
density of the solution was determined. The viscometer was cleaned thoroughly a clamped
vertically. Then a fixed amount of sugar solution was taken in it by sucking up and allowed to
fall freely between the two marks and time was noted and repeated for three times. For 5%, 10%,
15% and unknown solution the same was repeated.
Experimental Data:

1. Measurement of relative density of a solution

Room temperature= --------------------------0C

Density of water at that temperature = --------------------------- gm/ cc

Viscosity of water at that temperature = -------------------------- Poise

Wt. of dry and Wt. of sp. Gravity Wt. of sp. Gravity

Wt. of solutions
clean sp. Gravity bottle with water Wt. of water (gm) bottle with
(gm)
bottle (gm) (gm) solutions (gm)

W1 W2 W 2- W 1= W w W3 W3-W1= Ws

2. Density of sugar solution at different concentrations

Concentration 5% 10% 15% Unknown solution

Density (gm/cc)

3. Calculation of relative density:

Relative density, or specific gravity, is the ratio of the density (mass of a unit volume) of a
substance to the density of a given reference material. Specific gravity usually means relative
density with respect to water. It is unitless.

m
Density ρ = v , where m = mass of liquid, V = volume of liquid

ms
v
ρs mw
Therefore relative density of solution = ρw = v

where ρs = density of sugar solution, ρw = density of water

 ms = mass or weight of sugar solution
m w = mass or weight of water

v = volume of specific gravity bottle

ms
ρw
As v is same for both liquid, therefore ρs = mw

4. Determination of Viscosity co-efficient

Substance No. of Time Mean time Density Viscosity

observation required (sec) (gm/cc) (Poise)
(sec.)
Pure water 1

5% solution 1

10% solution 1

15% solution 1

Unknown 1
solution
2

5. Calculation of viscosity of sugar solution:

 ηs ρs t s
ηw = ρw t w

ρs t s
Therefore, ηs = ρw t w ηw where ηs = viscosity of sugar solution

ηw = viscosity of water

ρs = density of sugar solution

ρw = density of water

ts = time required for sugar solution

tw = time required for water

Precautions:

 The viscometer must be cleaned and rinsed.

 The viscometer should be clamp in a vertical position and its height must remain
constant each time when it is clamped.

 Exactly same volume of the two liquids should be used.

 The viscometer should not be disturbed during measurement of time of flow.

EXP. NO. – 11

Name of the experiment: Determination of Saponificatioin Value of an oil or

fat.
Objective: The objective of our experiment is to find out the Saponification value of oil or fat, using
either KOH or NaOH.

Theory: Saponification value of oil is defined as the number of milligram of KOH needed to saponify
one gram of oil. Saponification is in fact the alkali hydrolysis of oil and fat. A fat is mixer of various
glycerides, the esters of glycerols with higher fatty acid like steric acid Palmitic acid etc. It reacts with
alkali under goes hydrolytic decomposition and converts into soap and glycerol.

O H O

C17H31 – C – O – C – H 3 C 17H31 – C – O- Na+

O +3 NaOH soap

C17H31 – C – O – C – H HEAT +

O C 3H8O3

C17H31 – C – O – C – H glycerol

fat

So if an excess of alkali is made to react with a known amount of the oil sample, some of the alkali will
be used up for saponification, depending upon the amount of which the saponification value of oil can be
found out by titrating excess alkali against a standard acid solution.

Chemicals required:

1. Standard (N/20) oxalic acid solution

2. Mustard oil
3. (N/2) alcoholic KOH solution
4. (N/2) HCl solution

Procedure:

1. Standardise the aicoholic (N/20) KOH solution against standard (N/20) oxalic acid:

Take an aliquot of 25 ml of the standard (N/20) oxalic acid in a 250 ml conical flask, add 2-3 drops of
phenolphthalein indicator, dilute to 50 ml and titrate with the (N/20) KOH solution up to a red end
point.

Table 1: Standardisation of (N/20) KOH solution

No. of Volume of Burette reading of KOH Difference Mean Strength of

observations oxalic acid solution volume of KOH
solution Initial Final KOH solution
solution

Calculation:
 Strength of standard oxalic acid solution = (0.3/ 0.3152) (N/20)

25 ml of standard (0.3/ 0.3152) (N/20) oxalic acid ¿ V1 ml of (N/20) KOH solution

25×0. 3
Therefore, Exact strength of (N/2) KOH solution = ( V1×0. 3152 ) (N/2)

2. Standardize the HCl solution against KOH solution:

Take an aliquot of 25 ml of the standard (N/20) HCl acid in a 250 ml conical flask, add 2-3 drops of
phenolphthalein indicator, dilute to 50 ml and titrate with the standard (N/20) KOH solution up to a red
end point.

Table 2: Standardization of (N/20) HCl solution

No. of Volume of Burette reading of KOH Difference Mean Strength of

observations HCl acid solution volume of HCl solution
solution Initial Final KOH
solution

Calculation:

Strength of standard KOH solution =

25 ml of standard (N/20) HCl acid ¿ V2 ml of (N/20) KOH solution

V2×0 . 3
Therefore, Exact strength of (N/2) HCl solution = ( 2×V1×0 . 3152 ) (N)

3.Estimation of saponification value:

1 to 2 ml of oil sample is introduced into a 250 ml round bottom flask or a conical flask. 25 ml 1 (N)
alcoholic KOH is added to it. This is fitted with long air condenser and refluxed in boiling water for
an hour to complete the saponification. It is then titrated; at hot condition against a standard (N/2)
HCL using few drops of phenolphthalein indicator till a distinct pink color disappears.

A blank titration is performed without taking oil into flask and required amount acid is noted down.

Table 3: Estimation of saponification value

No. of Volume of Burette reading of HCl Difference Mean volume of

observations KOH acid solution HCl solution
solution Initial Final

Calculation:

Amount of oil taken x gm. Titre value of KOH with oil = V3

Titre value of blank = V4

Therefore KOH consumed by x gm of oil

≡
(V4- V3) ml of
( 2×0V2×0. 3
. 3152×V1 )
(N )
HCl

¿ (V4- V3) ml of ( 2×0V2×0. 3

. 3152×V1 )
(N )
KOH

( V4−V3 )×V2×0 .3
¿
2×0 .3152×V1 ml of (N)KOH

56 .1×( V4−V3 )×V2×0 . 3

¿
2×0 . 3152×V1 mg of (N)KOH

(Hence 1 ml of (N) KOH ¿ 56 .1 mgofKOH

56 .1×( V4−V3 )×V2×0 . 3

¿
Result : KOH consumed by 1 gm of oil 2×0 . 3152×V1 mg of (N)KOH

= Saponification value of oil

Discussion : Discuss why your sap value might have deviated from the true value of 254 also discuss
about the change in sap value if we use NaOH instead of KOH

QUESTION:

1. What is saponification value?

2. How it is vary with different alkali?

Experiment No:13

Name: Determination of Partition Co-efficient of Acetic Acid between Water

and n-butanol

Theory:
The Nerst distribution law states that at constant temperature, when different quantities of a
solute are allowed to distribute between two immiscible solvents I contact with each other, then at
equilibrium the ratio of the concentration of the solute in two solvent layers is constant.

When a solute is shaken in two immiscible liquids, then the solute is found to be distributed between the
liquids in a definite manner, if the solute is soluble in each of the solvent. According to distribution law,
C1
K
the distribution co-efficient at a particular temperature is given by C2 where C and C represents
1 2
the concentration of solute in solvent 1 and 2 respectively, when in solution phase solute molecules are in
same state of association.

Now, if water and n-butanol are taken as the pair of two immiscible solvents and acetic acid as the solute
then as acetic acid retains its normal molecular weight in both the solvents, so the expression for partition
co-efficient will be

K=

Apparatus:

 Stoppered bottles

 Volumetric flask

 Conical flask

 Burette

 Pipette

Materials Required:

 Standard oxalic acid

 NaOH solution

 Acetic acid

 N-Butanol

 Distilled water

 Phenolphthalein indicator

Procedure:

1. A standard oxalic acid solution of (N/10) was prepared and NaOH solution was
standardized against standard oxalic acid solution using phenolphthalein indicator.

2. In bottle 1, 20 ml acetic acid, 490 ml water and 490 ml n-butanol was added. Similarly
in bottle 2, 40 ml acetic acid , 480 ml water and 480 ml n-butanol was added.

3. Stoppered bottles were shaken for one hour and allowed to stand till the two liquid
layers separated.

4. Definite volume of aqueous layer and organic layer from each of the two bottles were
 taken out and standardized against NaOH solution Using Phenolphthalein as indicator.

Experimental Results:
Table 1: Composition of materials in each bottle

Bottle 1 Bottle 2

20 ml acetic acid 40 ml acetic acid

490 ml water 480 ml water

490 ml n-butanol 480 ml n-butanol

Table 2: Preparation of standard oxalic acid solution

Weight to be
Initial weight(gm) Final weight(gm) Weight taken(gm) Strength
taken(gm)

w
W1 W2 W1-W2 = w 1.575
1.575 (N/10)

Table 3: Standardization of NaOH solution by standard oxalic acid solution

Burette reading
Volume of Strength of
No. of Volume of Strength of
oxalic acid NaOH
observation Initial(ml) Final(ml) NaOH (ml) oxalic acid
(ml) solution

Table 4: Standardization acetic acid in aqueous layer and n-butanol layer by NaOH
solution

Burette reading of NaOH Volume of

Strength of
Volume of required
Bottle No Layer taken acetic acid in
layer(ml) Initial(ml) Final(ml) NaOH
layer
solution(ml)
 5
Organic layer
5
1
5
Aqueous layer
5

5
Organic layer
5
2
5
Aqueous layer
5

Table 5: Determination of partition co-efficient

Bottle No partition co-efficient Mean

Partition co-efficient of acetic acid = ----------------------------------

Calculation:

V1S1 = V2S2 where V1 = volume of NaOH

S1 = strength of NaOH V2 = volume of acetic acid in layer

S2 = strength of acetic acid in layer

Therefore, partition co-efficient,

K=

Precaution:

 During withdrawing aliquot one layer must not be contaminated with the other.

 Pipette which is used during the experiment must be cleaned.