VOLUMETRIC ANALYSIS – CLASS XII

EXPERIMENT-1

Aim: To prepare 100 ml. of M/20 Mohr salt solution (FeSO4.(NH4)2SO4.6H2O)

and using this solution to find the strength and molarity of given
KMnO4 solution.

Materials: Conical Flask, funnel, KMnO4 solution, distilled water, Mohr salt,
burette, volumetric flask, wash bottle, pipette, watch glass, burette
stand, test tube, test tube stand, 50% sulphuric acid.

Theory:
 To prepare 100 ml. M/20 Mohr salt solution,
Weight of Mohr salt required for preparing 100 ml M/20 Mohr salt
solution
M weight of Mohr salt required for 100 ml .×1000
=
20 molar mass of Mohr salt ×100
1 x×1000 x×10
∴ = ⇒
20 392×100 392
1 10x
=
20 392
392
= =1.96 gm .
200

 Ionic Equation:

MnO−4 +8 H + +5 e ⃗ Mn 2 + + 4 H 2 O
Fe 2+ ⃗ Fe 3+ +e− ×5
− + 2+ 2+ 3+
Overall reaction: MnO 4 + 8 H +5 Fe ⃗ Mn +5 Fe +4 H 2 O

 Formulae used:
M 1 V 1 ( KMnO 4 ) Stoichoimetric coefficient of KMnO 4
=
M 2 V 2 ( FAS ) Stoichiometric coefficient of FAS

1
 M 1 V 1 ( KMnO 4 ) 1
=
M 2 V 2 ( FAS ) 5

M1 V 1 M 2 V 2
=
1 5

 Strength of KMnO4:
Strength of KMnO4 = Molarity x Molar mass

 Indicator:
KMnO4 self-indicator

 End point:
Colourless to pink

Procedure:
(i) 1.96 gm. Of Mohr salt is transferred into a 100 ml volumetric flask and one test
tube 50% of sulphuric acid is added to this solution to prevent hydrolysis of
salt. It is then made up to 100 ml by adding water.
(ii) The burette is filled with KMnO4 solution.
(iii) 20 ml. of Mohr salt solution is pipetted out into the conical flask.
(Iv) 20 ml. H2SO4 is added into the flask again to make the medium acidic.
(v) The initial reading of the burette is noted down (upper meniscus).
(vi) KMnO4 solution is added drop wise with constant stirring into the flask till the
light pink color is obtained. The final reading of the burette is noted.

Observations:

S.No Volume of FAS Burette reading (ml) Volume of KMnO4

used (ml) used (ml)
Initial Final

1 20 0 20 20

2 20 0 19.5 19.5

3 20 0 19.5 19.5

Concordant value = 19.5

2
Calculation:
Molarity of KMnO4
According to the equation, one mole of KMnO4 reacts with 5 moles of FAS.

M 1 V 1 ( KMnO 4 ) Stoichoimetric coefficient of KMnO 4

=
M 2 V 2 ( FAS ) Stoichiometric coefficient of FAS

M 1 V 1 ( KMnO 4 ) 1
=
M 2 V 2 ( FAS ) 5

M1 V 1 M 2 V 2 1 0.05 ×20 0.5

= M 1=x M 2= =0.05 V 1=19.5 ml . V 2=20 ml . x × 19.5= x= =0.01 M
1 5 20 5 19.5

Strength of KMnO4
Strength of KMnO4 = Molarity x Molar mass
= 0.01 mol/L× 158 g / mol = 1.58 g/L

Result:
Molarity of KMnO4 = 0.01M
Strength of KMnO4 = 1.58 g/L

Precautions (For both titrations)

Learn any 4 precautions and it should be experiment specific
 Handle the apparatus and chemicals carefully.
 Rinse the pipette and burette first with distilled water then with the
corresponding solutions.
 Close the pipette with the index finger.
 Always keep the lower end of the pipette in the liquid when sucking it.
 Do not blow out the last drop of the solution from the jet end of the pipette.
 KMnO4 solution is always taken in the burette.
 Do not allow any air bubbles to remain inside the burette.
 Read the upper meniscus while taking burette reading with KMnO4 solution.
 Let no drops of solution be at the tip of the burette at the end point.

3
 Add about an equal volume of dil.H2SO4 to the solution to be titrated before
adding KMnO4.
 If oxalic acid or some oxalate is to be titrated, add required amount of dil.H 2SO4
and heat the flask to 60°-70°C.
 In case of ferrous salt, no warming is required.
 No external indicator is required for KMnO 4 titration because KMnO4 acts as self-
indicator.

4
EXPERIMEMT-2

Aim: To prepare 100 ml. of M/40 Oxalic acid solution and using this solution
to find the strength and molarity of given KMnO4 solutions.

Materials: Conical Flask, funnel, KMnO4 solution, distilled water, Oxalic acid,
burette, volumetric flask, wash bottle, pipette, watch glass, burette
stand, test tube, test tube stand, 50% sulphuric acid, sprit lamp and
match box.

Theory:
 To prepare 100 ml. M/40 Oxalic acid solution,

M weight of Oxalic acid required for 100 ml .×1000

=
40 molar mass of Oxalic acid ×100
1 x×1000
∴ =
40 126×100
1 10 x
=
40 126
126
x= =0.315 gm .
400
 Ionic Equation:

[ MnO−4 +8 H + +5 e⃗ Mn2++4 H 2 O ] ×2
[ C 2 O2−4 ⃗2 CO 2+2 e− ] ×5
− + 2− 2+
Overall reaction: 2 MnO 4 +16 H +5 C 2 O 4 ⃗ 2 Mn +8 H 2 O+10 CO 2

 Formulae used:
M 1 V 1 ( Oxalic Acid ) Stoichoimetric coefficient of Oxalic Acid
=
M 2 V 2 (KMnO 4 ) Stoichiometric coefficient of KMnO 4

5
 M 1 V 1 ( Oxalic Acid ) 5
=
M 2 V 2 ( K MnO 4 ) 2

 Strength of KMnO4:
Strength of KMnO4 = Molarity x Molar mass

 Indicator:
KMnO4 acts as self-indicator

 End point:
Colourless to pink

Procedure:
(i) 0.315 gm. of Oxalic acid crystals are transferred into a volumetric flask of 100
ml. and water is added to it till its mark.
(ii) The burette is filled with KMnO4 solution.
(iii) 20 ml. of Oxalic acid solution is pipette out into the conical flask.
(iv) 20 ml. H2SO4 is added into the flask to make the medium acidic.
(v)Conical flask is heated till 60°C and then titrated against KMnO4.

Observations:

S.No Volume of oxalic Burette reading (ml) Volume of KMnO4

acid used (ml) used (ml)
Initial Final

1 20 0 20 20

2 20 20 40 20

3 20 0 20 20

Concordant value = 20 ml

6
Calculations:
Molarity of KMnO4
According to the equation, two mole of KMnO4 reacts with 5 moles of oxalic acid

M 1 V 1 ( Oxalic Acid ) Stoichoimetric coefficient of Oxalic Acid

=
M 2 V 2 (KMnO 4 ) Stoichiometric coefficient of KMnO 4

M 1 V 1 ( Oxalic Acid ) 5
=
M 2 V 2 ( K MnO 4 ) 2

Strength of KMnO4
 Strength of KMnO4 = Molarity x Molar mass
= 0.01 mol/L× 158 g / mol = 1.58 g/L

7
Result:
Molarity of KMnO4 = 0.01M
Strength of KMnO4 = 1.58 g/L

Precautions (For both titrations)

Learn any 4 precautions and it should be experiment specific
 Handle the apparatus and chemicals carefully.
 Rinse the pipette and burette first with distilled water then with the
corresponding solutions.
 Close the pipette with the index finger.
 Always keep the lower end of the pipette in the liquid when sucking it.
 Do not blow out the last drop of the solution from the jet end of the pipette.
 KMnO4 solution is always taken in the burette.
 Do not allow any air bubbles to remain inside the burette.
 Read the upper meniscus while taking burette reading with KMnO4 solution.
 Let no drops of solution be at the tip of the burette at the end point.
 Add about an equal volume of dil.H2SO4 to the solution to be titrated before
adding KMnO4.
 If oxalic acid or some oxalate is to be titrated, add required amount of dil.H 2SO4
and heat the flask to 60°-70°C.
 In case of ferrous salt, no warming is required.
 No external indicator is required for KMnO 4 titration because KMnO4 acts as self-
indicator.
 Do not rinse the titration flask with the solution.