1.

Titration
Titration of KMnO4 solution vs M/20 FAS solution.

Aim
To determine the concentration/molarity of KMnO 4 solution by
titrating it against standard solution of ferrous ammonium
sulphate.
Theory
Ferrous ammonium sulphate also acts as a reducing agent in
the titration against potassium permanganate.
The reaction which takes place is given below:

The oxidation number of iron in Mohr’s salt is +2. Iron is

oxidised during the reaction and its oxidation number changes
from +2 to +3. In this titration heating of ferrous ammonium
sulphate solution is not required because reaction rate is very
high even at room temperature. Also, at high temperatures,
ferrous ions may be oxidised to ferric ions by oxygen of air and
error may be introduced in the experiment.

Material Required
• Measuring flask (250 mL)
• Burette (50 mL)
• Burette stand
• Pipette
• Conical flask
• Glazed tile (white)
• Funnel
• Weighing bottle
• Potassium permanganate solution
• Dilute sulphuric acid
• Ferrous ammonium sulphate

Procedure

A. Preparation of M/20 standard solution of ferrous

ammonium sulphate
(Molar mass of FeSO4(NH4)2SO4 .6H2O = 392 g mol–1).

(i) Weigh 1.96 g of ferrous ammonium sulphate and transfer it

into a 100 mL measuring flask through a funnel.

(ii) Transfer the solid sticking to the funnel with the help of
distilled water into the flask and add dilute H 2SO4 into the flask
drop wise to get the clear solution.

(iii) Shake the flask till the substance dissolves and make the
solution upto the mark.

B. Titration of ferrous ammonium sulphate against

potassium permanganate solution

(i) Rinse and fill the clean burette with potassium

permanganate solution. Remove air bubbles if any, from the
burette tip by releasing some solution through it.

(ii) Take 10 mL of M/20 ferrous ammonium sulphate solution in

a conical flask and add half a test tube (10 mL) full of 2M H 2SO4
to it.

(iii) Titrate the above solution with potassium permanganate

solution till the colour of the solution changes to permanent
pink. Swirl the content of the flask during the titration.

(iv) Repeat the titration, until three concordant readings are

obtained.
(v) Record the readings as shown in the observation Table and
calculate the strength of potassium permanganate solution in
mols/litre.

Titration of potassium permanganate solution against

standard ferrous ammonium sulphate solution

OBSERVATION TABLE
S.N Volume of Initial Final Volume of
o FAS used Reading Reading KMnO4 used
1. 20 ml 0.0 ml 10.1 ml 10.1 ml
2. 20 ml 10.1 ml 20.1 ml 10 ml
3. 20 ml 20.1 ml 30.1 ml 10 ml
4. 20ml 30.1 ml 40.1 ml 10 ml

Calculations
The strength of unknown solution in terms of molarity may be
determined by the following equation :

n1M1V1 = n2M2V2

Where
M1 = molarity of ferrous ammonium sulphate
M2 = molarity potassium permanganate solution
V1 = Volume of ferrous ammonium sulphate solution.
V2 = Volume potassium permanganate solution.
n1 = 1, (the number of electrons lost per formula unit of ferrous
ammonium sulphate in the half cell reaction)

n2 = 5, (the number of electrons gained per formula unit of

potassium permanganate in a half cell reaction)

Strength can be calculated by the formula given below :

Strength = Molarity x Molar mass

Calculation:
n1M1V1 = n2M2V2

2 × 1/20 × 10 = 10 × M2 × 10

M2 = 2× 1× 10
10× 20× 10

M2 = 2
200

M2 = 1/100
M2 = 0.01 M

Result
The strength of the given potassium permanganate solution is
1.58 g/L

Precautions
(a) Always use a fresh sample of ferrous ammonium sulphate to
prepare its standard solution.
(b) Always rinse the burette and the pipette with the solutions
to be taken in them.
(c) Never rinse the conical flask with the experimental
solutions.
(d) Remove the air gaps, if any, from the burette.
(e) Never forget to remove the funnel from the burette before
noting the initial reading of the burette.
(f) No drop of the liquid should hang at the tip of the burette at
the end point and while noting reading.
(g) Always read the upper meniscus for recording the burette
reading in the case of all coloured solutions.
(h) Never use pipette and burette with a broken nozzle.
(i) The lower end of the pipette should always remain dipped in
the liquid while sucking the liquid.
(j) Do not blow out the last drop of the solution from the jet end
of the pipette.
(k) The strength of the solution must be calculated up to the
fourth decimal place.
2. Titration

Titration of KMnO4 solution vs M/50 Oxalic acid

Aim
To determine the concentration/molarity of KMnO 4 solution by
titrating it against a M/50 standard solution of oxalic acid.

Theory
In the present experiment, potassium permanganate acts as a
powerful oxidising agent. Although KMnO4 acts as an oxidising
agent in alkaline medium also, for quantitative analysis mostly
acidic medium is used. The oxidising action of KMnO 4 in the
acidic medium can be represented by the following equation:

.
The acid used in this titration is dilute sulphuric acid. Nitric acid
is not used as it is itself an oxidising agent and hydrochloric
acid is usually avoided because it reacts with KMnO 4 according
to the equation given below to produce chlorine and chlorine
which is also an oxidising agent in the aqueous solution.

Since, oxalic acid acts as a reducing agent, it can be titrated

against potassium permanganate in the acidic medium
according to the following equation:

Reactions of oxalic acid

A. Chemical equations
B. Ionic equation

In these equations, MnO4– is reduced to Mn2+ and C2O4 2– is

oxidised to CO2. The oxidation number of carbon in C2O4 2–
changes from +3 to +4. In these titrations, potassium
permanganate acts as a self indicator. Initially the colour of
potassium permanganate is discharged due to its reduction by
oxalic acid. After complete consumption of oxalate ions, the
end point is indicated by the appearance of a light pink colour
produced by the addition of a little excess of unreacted
potassium permanganate. Further, during the titration of oxalic
acid against potassium permanganate, warming of oxalic acid
solution (50°–60°C) along with dilute H2SO4 is required.
This is essential because the reaction takes place at higher
temperature. During the titration, first manganous sulphate is
formed which acts as a catalyst for the reduction of KMnO 4 by
oxalic acid. Therefore, in the beginning the reaction rate is slow
and as the reaction proceeds, the rate of the reaction
increases.

Material Required
• Measuring flask (250 mL)
• Burette (50 mL)
• Burette stand
• Pipette
• Conical flask
• Funnel
• Weighing bottle
• Glazed tile(white)
• Burner
• Wire gauze
• Chemical balance
• Oxalic acid
• Potassium permanganate solution
• 2 M Sulphuric acid

Procedure
A. Preparation of M/50 standard solution of oxalic
acid
(Molar mass of C2H2O4.2H2O = 126 g mol–1).

(i) Weigh 0.252 g of Oxalic acid and transfer it into a 100 mL

measuring flask through a funnel.
(ii) Transfer the solid sticking to the funnel with the help of
distilled water into the flask and add dilute H 2SO4 into the flask
drop wise to get the clear solution.
(iii) Shake the flask till the substance dissolves and make the
solution upto the mark

[Link] of oxalic acid solution against potassium

permagnate solution

(i) Rinse and fill a clean burette with potassium

permanganate solution. Remove the air bubble, if any, from the
nozzle of the burette by releasing some solution through it. The
burette used in the permanganate titration must have a glass
stop cock as rubber is attacked by permanganate ions.

(ii) Take 10 mL of 0.02 M oxalic acid solution in a conical flask

and add half of the test tube full ( 10 mL) of 2M H 2SO4 to it to
prevent the formation of any precipitate of manganese dioxide
during the course of the titration.

(iii) Heat the oxalic acid solution upto 50°– 60°C before titrating
it with potassium permanganate solution taken in the burette.
To increase the visibility of the colour change, place the conical
flask containing the solution to be titrated over a white glazed
tile kept below the nozzle of the vertically fitted burette.

(iv) Note the initial reading of the volume of permanganate

solution in the burette and add it in small volumes to the hot
oxalic acid solution while swirling the contents of the flask
gently. The violet colour of permanganate solution is
discharged on reaction with oxalic acid. The end point is
indicated by the appearance of permanent light pink colour due
to a slight excess of permanganate solution.

(v) Repeat the titration till three concordant readings are

obtained. Since the solution of KMnO4 is of dark colour, the
upper meniscus should be considered for noting the burette
readings.

(vi) Record the readings as shown in the observation Table and

calculate the strength of potassium permanganate solution in
mols/litre.
Titration of potassium permanganate solution against
standard oxalic acid solution
S.N Volume of Initial Final Volume of
o Oxalic Acid Reading Reading KMnO4 used
used
1. 20 ml 0.0 ml 10.1 ml 10.1 ml
2. 20 ml 10.1 ml 20.1 ml 10 ml
3. 20 ml 20.1 ml 30.1 ml 10 ml
4. 20ml 30.1 ml 40.1 ml 10 ml

Calculations
(i) The strength of the unknown solution in terms of molarity
may be determined by the following equation.
n1M1V1 = n2 M2 V2
For oxalic acid vs potassium permanganate titration:
n1 = 2, (the number of electrons lost per formula unit of oxalic
acid in a balanced equation of half cell reaction)
n2 = 5, (the number of electrons gained per formula unit of
potassium permanganate in the balanced equation of half cell
reaction)
M1 and M2 are the molarities of oxalic acid and potassium
permanganate solutions used in the titration.
V1 and V2 are the volumes of oxalic acid and potassium
permanganate solutions.

On putting the value of n1 and n2 in equation

Calculation:
n1M1V1 = n2M2V2

2 × 1/50 × 10 = 5 × M2 × 10

M2 = 2× 1× 10
5× 50× 10

M2 = 1
125

M2 = 0.008 M

We can calculate the molarity of potassium permanganate

solution by using equation. Strength of the solution is given by
the following equation:
Strength = Molarity × Molar mass

Result
(i) Molarity of KMnO4 solution is 0.008 M.
(ii) Strength of the KMnO4 solution is 1.26g /L.

Precautions
(a) Always rinse the burette and the pipette with the solutions
to be taken in them.
(b) Never rinse the conical flask with the experimental
solutions.
(c) Remove the air gaps if any, from the burette.
(d) Never forget to remove the funnel from the burette before
noting the initial reading of the burette.
(e) No drop of the liquid should hang at the tip of the burette at
the end point and while noting reading.
(f) Always read the upper meniscus for recording the burette
reading in the case of all coloured solutions.
(g) Never use pipette and burette with a broken nozzle.
(h) Lower end of the pipette should always remain dipped in the
liquid while sucking the liquid.
(i) Do not blow out the last drop of the solution from the jet end
of the pipette.
(j) The strength of the solution must be calculated up to the
fourth decimal place.
(k) Do not forget to heat the mixture of oxalic acid and H 2SO4
solutions between 50°–60° C. While titrating it against
potassium permanganate.