Volumetric Analysis Procedure
Volumetric Analysis Procedure
Volumetric Analysis Procedure
EXPERIMENT-1
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:
1 20 0 20 20
2 20 0 19.5 19.5
3 20 0 19.5 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 ) 1
=
M 2 V 2 ( FAS ) 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
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,
[ 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:
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 ) 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