Experiment -1

M
Object- A solution of ferrous ammonium sulphate (Mohr‵s salt) is provided. Using this
20
solution, find out the Molarity and strength of given KMnO4 solution.

Solution-

Materials Required:

1. Mohr’s salt (ferrous ammonium sulfate)

2. Potassium permanganate solution
3. Dilute sulfuric acid
4. Chemical balance
5. Burette
6. Burette stand
7. Pipette
8. Conical flask
9. Funnel
10. Measuring flask
11. Weighing bottle
Chemical equations-

 Molecular equations –
2KMnO4 + 3H2SO4 → K2SO4 + 2MnSO4 + 3H2O + 5[O]
[2FeSO4.(NH4)2SO4.6H2O + H2SO4 + [O] → Fe2(SO4)3 + 13H2O + 2(NH4)2SO4] × 5
2KMnO4 + 8H2SO4 + 10FeSO4.(NH4)2SO4.6H2O → K2SO4 + 2MnSO4 + 5Fe2(SO4)3 +
10(NH4)2SO4 + 68H2O
 Ionic equations-
MnO4- + 8H+ + 5e- → Mn2+ +4H2O
5Fe2+ → 5Fe3+ + 5e-
--------- ---------------------------------------------------
MnO4- + 8H+ + 5Fe2+ → 5Fe3+ + Mn2+ + 4H2O
Indicator- KMnO4 is a self indicator.
End point- Colourless to permanent pink colour (KMnO4 in burette).
Procedure-

A. Preparation of M/20 FAS solution-

Let volume of solution (V) = 250 ml
1
V= L
4
Molar mass of FeSO4.(NH4)2SO4.6H2O = 56 + 32 + 16×4 + (14+1×4)×2 + 32 + 16×4 +
6×(1×2+16)
m = 392 g/mol

1
Molarity of solution = mass of solute (FAS) (in g) / molar mass of solute × volume of solution (in L)
w
M=
m×V
w=M×m×V
1 1
w= × 392 ×
20 4
w = 4.9 g
Therefore,
1
Required mass of FeSO4.(NH4)2SO4.6H2O to make L solution = 4.9 g
4

Now, dissolve 4.9 g FAS in distilled water till ¼ L solution.

Now,
M/20 FAS solution is ready for further use.

B. Titration of FAS solution against KMnO4 solution-

1) Rinse burette by KMnO4 solution and fill the burette with the given KMnO4 solution.
2) Rinse the pipette with the M/20 F.A.S. solution and pipette out 20 ml of FAS in a washed titration
flask.
3) Add approx 20 ml dil H2SO4 to the solution in titration flask
4) Note the initial reading of the burette.
5) Now add KMnO4 from solution from the burette in small amount in the titration flask and shake it
after each addition till a permanent light pink colour is imparted to the solution in the titration
flask.
6) Note the final reading of the burette.
7) Repeat the above steps 4-5 times to get a set of three concordant readings.

2
Observations and calculations-

M
Molarity of FAS solution =
20
Volume of FAS solution taken for each titration = 20 ml.

S.N. Initial reading of Final reading Volume of KMnO4 Average volume of

the burette (in ml) of the burette solution used (in ml) KMnO4 solution used
1 50 36.5 13.5
2 50 36.4 13.6 13.5 ml
3 50 36.5 13.5
4 50 36.5 13.5

I. To calculate Molarity of the KMnO4 solution:

From the overall balanced chemical equation, it is clear that 2 moles of KMnO 4 reacts with 10
moles of FAS.

3
 2
MKMnO4 =
10× 13.5
2
=
135
= 0.0148 mol / L
Therefore,
Molarity of given KMnO4 solution = 0.0148 mol / L

II. To calculate strength of the KMnO4 solution -

Molar mass of KMnO4 = 39 + 55 + 16 × 4
= 39 + 55 + 64
= 158 g/mol
Molar mass of KMnO4 = 39 + 55 + 16 × 4 = 158 g/mol
Strength (in g/L) = Molarity × molar mass
= 0.0148 × 158
= 2.3384 g/L
Now,
Strength of given KMnO4 solution = 2.34 g/L

Results:

1. Molarity of given KMnO4 solution is 0.0148 moles/liter

2. The strength of given potassium permanganate solution is 2.34 g/L

Precautions:

1. Clean all the apparatus with distilled water before starting the experiment and then rinse with the
solution to be taken in them.
2. Rinse the pipette with FAS solution and burette with KMnO4 solution before use.
3. Potassium permanganate is dark, so always read the upper meniscus.
4. Use dilute sulfuric acid for acidifying the potassium permanganate.
5. Take accurate readings once it reaches the end point and doesn’t go with average readings.
6. Do not use a rubber cork burette as it can be attacked by KMnO4.
7. The strength of the unknown solution should be taken up to two decimal places only.

4
 Experiment -2
M
Object- A 10 solution of ferrous ammonium sulphate (Mohr‵s salt) is provided. Using this
solution, find out the Molarity and strength of given KMnO4 solution.

Solution-

Materials Required:

1. Mohr’s salt (ferrous ammonium sulfate)

2. Potassium permanganate solution
3. Dilute sulfuric acid
4. Chemical balance
5. Burette
6. Burette stand
7. Pipette
8. Conical flask
9. Funnel
10. Measuring flask
11. Weighing bottle
Chemical equations-

 Molecular equations –
2KMnO4 + 3H2SO4 → K2SO4 + 2MnSO4 + 3H2O + 5[O]
[2FeSO4.(NH4)2SO4.6H2O + H2SO4 + [O] → Fe2(SO4)3 + 13H2O + 2(NH4)2SO4] × 5
2KMnO4 + 8H2SO4 + 10FeSO4.(NH4)2SO4.6H2O → K2SO4 + 2MnSO4 + 5Fe2(SO4)3 +
10(NH4)2SO4 + 68H2O
 Ionic equations-
MnO4- + 8H+ + 5e- → Mn2+ +4H2O
5Fe2+ → 5Fe3+ + 5e-
--------------------------------------------------------------
MnO4- + 8H+ + 5Fe2+ → 5Fe3+ + Mn2+ + 4H2O
Indicator- KMnO4 is a self indicator.
End point- Colourless to permanent pink colour (KMnO4 in burette).
Procedure-

A. Preparation of M/10 FAS solution-

Let volume of solution (V) = 250 ml
1
V= L
4
Molar mass of FeSO4.(NH4)2SO4.6H2O = 56 + 32 + 16×4 + (14+1×4)×2 + 32 + 16×4 + 6 × (1×2+16)
m = 392 g/mol
Molarity of solution = mass of solute (FAS) (in g) / molar mass of solute × volume of solution (in L)
w
M=
m×V
w=M×m×V

5
 1 1
w= × 392 ×
10 4
w = 9.8 g
Therefore,
1
Required mass of FeSO4.(NH4)2SO4.6H2O to make L solution = 9.8 g
4

Now, dissolve 9.8 g FAS in distilled water till ¼ L solution.

Now,
M/10 FAS solution is ready for further use.

B. Titration of FAS solution against KMnO4 solution-

1. Rinse burette by KMnO4 solution and fill the burette with the given KMnO4 solution.
2. Rinse the pipette with the M /10 F.A.S. solution and pipette out 20 ml of FAS in a washed
titration flask.
3. Add approx 10 ml dil H2SO4 to the solution in titration flask
4. Note the initial reading of the burette.
5. Now add KMnO4 from solution from the burette in small amount in the titration flask and shake it
after each addition till a permanent light pink colour is imparted to the solution in the titration
flask.
6. Note the final reading of the burette.
7. Repeat the above steps 4-5 times to get a set of three concordant readings.

6
Observations and calculations-
Molarity of FAS solution = M /10
Volume of FAS solution taken for each titration = 20 ml.

S.N. Initial reading of Final reading Volume of KMnO4 Average volume of

the burette (in ml) of the burette solution used (in ml) KMnO4 solution used
1 50 23.4 26.6
2 50 23.5 26.5 26.5 ml
3 50 23.5 26.5
4 50 23.5 26.5

I. To calculate Molarity of the KMnO4 solution:

From the overall balanced chemical equation, it is clear that 2 moles of KMnO 4 reacts with 10
moles of FAS.

7
 4
MKMnO4 =
10× 26.5
4
=
265
= 0.0151 mol / L
Therefore,
Molarity of given KMnO4 solution = 0.0151 mol / L

II. To calculate strength of the KMnO4 solution -

Molar mass of KMnO4 = 39 + 55 + 16 × 4
= 39 + 55 + 64
= 158 g/mol
Molar mass of KMnO4 = 39 + 55 + 16 × 4 = 158 g/mol
Strength (in g/L) = Molarity × molar mass
= 0.0151 × 158
= 2.3858 g/L
Now,
Strength of given KMnO4 solution = 2.39 g/L

Results :

1. Molarity of given KMnO4 solution is 0.0151 moles/liter

2. The strength of given potassium permanganate solution is 2.39 g/L

Precautions:

1. Clean all the apparatus with distilled water before starting the experiment and then rinse with the
solution to be taken in them.
2. Rinse the pipette with FAS solution and burette with KMnO4 solution before use.
3. Potassium permanganate is dark, so always read the upper meniscus.
4. Use dilute sulfuric acid for acidifying the potassium permanganate.

8
 5. Take accurate readings once it reaches the end point and doesn’t go with average readings.
6. Do not use a rubber cork burette as it can be attacked by KMnO4.
7. The strength of the unknown solution should be taken up to two decimal places only.

Experiment: 3
Object- To determine the concentration / molarity of KMnO4 solution by titrating it against a 0.1
M standard solution of oxalic acid.

Theory /Principle – In the reaction between potassium permanganate and oxalic acid, potassium
permanganate is a strong oxidising agent and oxalic acid is a reducing agent. Thus, the reaction
between them is a redox reaction and the titration of these reagents is called redox titration. The
oxidizing action of KMnO4 in the acidic medium can be represented by the following reaction-

MnO4- + 8H+ + 5e- → Mn2+ + 4H2O

Note-
 The acid used in this titration is dilute sulphuric acid.
 Nitric acid cannot be used because it is an oxidising agent thus, may oxidize oxalic acid.
 Hydrochloric acid cannot be used because it reacts with KMnO4 to produce chlorine
which also acts as an oxidising agent in the aqueous solution and interfere in the titration.
2KMnO4 + 16HCl → 2KCl + 2MnCl2 + 5Cl2 + 8H2O

Chemical equations: The equations involved in the titration of oxalic acid against potassium
permanganate in the acidic medium are as follows-

9
Indicator- In these KMnO4 acts as a self indicator.

End Point- Initially, dark purple colour of KMnO4 is discharged when it is added to oxalic acid
because of reduction of KMnO4 by oxalic acid. At the end point of titration, the light pink colour
persist in the solution because of the presence of a little excess of titration, unreacted KMnO 4.
This is so because at the end point, no oxalic acid is left in the solution to reduce KMnO4, i.e.
oxalate ions are completely consumed. Hence, the light pink colour when persist in the solution
shows the completion of titration.

Material required-

 Measuring flask (250 mL) :1

 Burette (50 mL) :1
 Burette stand :1
 Pipette :1
 Conical flask :1
 Funnel :1
 Weighing bottle :1
 Burner :1
 Chemical balance :1
 Oxalic acid : as per need
 Potassium permanganate solution : as per need
 Sulphuric acid : as per need

Procedure-

A. Preparation of 0.1 M standard solution of Oxalic acid-

10
 Let volume of solution (V) = 250 ml
1
V= L
4
Molar mass of H2C2O4.2H2O = 1× 2 + 12 × 2 + 16 × 4 + 2 × (1 ×2 + 16)
m = 126 g/mol

mass of solute ( oxalic acid ) ∈gram

Molarity of solution =
molar mass of solute ( oxalic acid ) × volume of solution(¿ L)
w
M=
m×V
w=M×m×V
1
w = 0.1 × 126 ×
4
w = 3.150 g
Therefore,
1
Required mass of H2C2O4.2H2O to make L solution = 3.150 g
4

Now, dissolve 3.150 g oxalic acid in distilled water till ¼ L solution.

Now,
0.1M Oxalic acid solution is ready for further use.

B. Titration of Oxalic acid against KMnO4 solution-

1) Rinse burette by KMnO4 solution and fill the burette with the given KMnO4 solution.
2) Rinse the pipette with the 0.1M Oxalic acid solution and pipette out 20 ml of Oxalic acid in a
washed titration flask.
3) Add approx 5 ml dil H2SO4 to the solution in titration flask in order to prevent the formation of
any precipitate of MnO2 during the course of the titration.
4) Heat the conical flask containing oxalic acid solution to 50-600C.
5) Note the initial reading of the burette.
6) Now add KMnO4 from solution from the burette in small amount in the titration flask and shake it
after each addition till a permanent light pink colour is imparted to the solution in the titration
flask.
7) Note the final reading of the burette.
8) Repeat the above steps 4-5 times to get a set of three concordant readings.

Observations-
Molarity of oxalic acid solution = 0.1M
Volume of oxalic acid solution taken for each titration = 20 ml.

11
 S.N. Initial reading of Final reading Volume of KMnO4 Average volume of
the burette (in ml) of the burette solution used (in ml) KMnO4 solution used
1 50 33.4 16.6
2 50 33.5 16.5 16.5 ml
3 50 33.5 16.5
4 50 33.5 16.5

Calculation-

The strength of unknown solution of KMnO4 in term of molarity cal be calculated as follows-

n1M1V1 = n2M2V2

 where, n1 is the number of electrons lost per formula unit of oxalic acid in a balanced equation of
half cell reaction. Here, its value is 2.
 n2 is the number of electrons gained per formula unit of KMnO4 in the balanced equation of half
cell reaction. Here, its value is 5.
 M1 and M2 are the molarities of oxalic acid and potassium permanganate solutions used in the
titration respectively.
 V1 and V2 are the volumes used of oxalic acid and KMnO4 solutions respectively.

(2 ×M1V1)oxalic acid = (5 ×M2V2) KMnO4

2 M 1V 1 2× 0.1× 20
M2 = = = 0.0485 M
5V 2 5× 16.5

Molarity of unknown solution of KMnO4 = 0.0485M

Strength of KMnO4 solution = M2 × 158 = 0.0485 ×158 = 7.663 g/ L

Result-

1. Molarity of KMnO4 solution = 0.0485M

2. Strength of KMnO4 solution = 7.663 g/L

Precautions-

1. While preparing standard solution, use dropper to add last few drops of water in the
standard flask.
2. Burette must have glass stopcock but not rubber cork because rubber may get reacted by
permanganate ions.
3. While noting the reading, no drop of the solution should hang at the tip of the burette at
the end point.
4. Do not forget to heat the mixture of oxalic acid and dil H2SO4 solutions between 50-600C.

12
 Experiment: 4
Object- To determine one anion and one cation in a given salt.

Detection of anion

13
S.N. Procedure Observation Inference
1 Take a pinch of the salt in dry Brisk effervescence with the CO32- anions may be
test tube and add 1-2 mL of evolution of colourless and present.
dil. HCl. odourless gas is formed.
2 Mix above gas in lime water. Lime water turns milky. CO32- anions
But on passing the gas for confirmed.
some more time, through lime
water milkiness disappears.

Detection of cation
S.N. Procedure Observation Inference
+
1 The given salt around 0.1 g is heated A pungent smell of NH4 cations may be
with 1-2 mL of conc. NaOH solution. ammonia is present.
obtained.

14
 2 Bring a glass rod dipped in conc. White dense fumes NH4+ cations are
HCl near the mouth of the test tube. are observed. confirmed.

Result-
1. Anion = CO32-

2. Cation = NH4+

15