VOLUMETRIC ANALYSIS

Exp No: 1 Estimation of Ferrous Sulphate

Exp No: 2 Estimation of FAS
Exp No: 3 Estimation of Oxalic acid
Exp No: 4 Estimation of Sodium hydroxide
Exp No: 5 Estimation of Oxalic acid
Ex No:1 Estimation of Ferrous Sulphate
Date:
Aim:
To estimate the amount of ferrous sulphate dissolved in 750 ml of the given
unknown solution volumetrically. You are provided with a standard solution
of ferrous ammonium sulphate (FAS) of normality 0.1102 N and potassium
permanganate solution as link solution.

S.No Content Titration-I Titration-II

1 Burette solution KMnO4 solution KMnO4 solution

20 ml of standard 20 ml of unknown
2 Pipette solution
FAS solution FeSO4 solution
3 Acid to be added 20ml of 2N H2SO4 20ml of 2N H2SO4

4 Temperature Lab temperature Lab temperature

Self-indicator Self-indicator
5 Indicator
(KMnO4) (KMnO4)

Appearance of Appearance of
6 End point permanent pale permanent pale
pink colour pink colour

7 Equivalent weight of FeSO4 = 278

Normality of standard ferrous ammonium sulphate solution = 0.1102N

TITRATION –I
Standard FAS solution Vs Link KMnO4 solution

Burette Readings Volume of

Volume of Concordant
(ml) KMnO4
S.No. FAS solution value
solution
(ml) Initial Final (ml)
(ml)
1 20 0 19.5 19.5
19.5
2 20 0 19.5 19.5

Volume of Std FAS solution (V1) = 20 ml

Normality of Std FAS solution (N1) = 0.1102N
Volume of link KMnO4 solution (V2) = 19.5 ml
Normality of link KMnO4 solution (N2) = x N
V1 N1 = V2 N2
V1 N1
N2 =
V2
20 x 0.1102
=
19.5

= 0.1130
Normality of standardised KMnO4 solution (N2) = 0.1130 N
TITRATION –II
Standardised KMnO4 solution Vs Unknown FeSO4 solution

Volume of Burette Readings Volume of

FeSO4 (ml) KMnO4 Concordant
S.No.
solution solution Value (ml)
Initial Final
(ml) (ml)
1 20 0 23.7 23.7
23.7
2 20 0 23.7 23.7

Volume of standardised KMnO4 solution (V1) = 23.7ml

Normality of standardised KMnO4 solution (N1) = 0.1130 N
Volume of unknown FeSO4 solution (V2) =20ml
Normality of unknown FeSO4 solution (N2) = x N
V1 N1= V2 N2
V1 N1
N2 =
V2
23.7 x 0.1130
=
20

= 0.1339𝑁
Normality of standardised FeSO4 solution (N2) = 𝟎. 𝟏𝟑𝟑𝟗 N
WEIGHT CALCULATION:
The amount of FeSO4 dissolved
in 1 lit of the solution = (Normality) x (equivalent weight)

The amount of FeSO4 dissolved

Normality x equivalent weight x 750
in 750 ml of the solution =
1000

0.1339 x 278 x 750

=
1000

0.1339 x 278 x 3
=
4

= 27.91 g
The amount of FeSO4 dissolved in 750 ml of the solution = 27.91 g

RESULT:
1. Normality of standardised KMnO4 solution (N2) = 0.1130 N

2. Normality of standardised FeSO4 solution (N2) = 0.1339 N

3. The amount of FeSO4 dissolved in 750 ml of the solution = 27.91 g

Ex No:2 Estimation of Ferrous Ammonium Sulphate (FAS)
Date:
Aim:
To estimate the amount of ferrous ammonium sulphate (FAS) dissolved in
1500 ml of the given unknown solution volumetrically. You are provided with
a standard solution of ferrous sulphate (FeSO4) of normality 0.1024 N and
potassium permanganate solution as link solution.

S.No Content Titration-I Titration-II

1 Burette solution KMnO4 solution KMnO4 solution

20 ml of standard 20 ml of unknown
2 Pipette solution
FeSO4 solution FAS solution
3 Acid to be added 20ml of 2N H2SO4 20ml of 2N H2SO4

4 Temperature Lab temperature Lab temperature

Self-indicator Self-indicator
5 Indicator
(KMnO4) (KMnO4)
Appearance of
Appearance of
permanent pale
6 End point permanent pale
pink colour
pink colour
7 Equivalent weight of FAS = 392

Normality of standard ferrous sulphate solution = 0.1024 N

TITRATION –I
Standard FeSO4 solution Vs Link KMnO4 solution
Volume of Burette Readings Volume of
Concordant
FeSO4 (ml) KMnO4
S.No. Value
solution solution
Initial Final (ml)
(ml) (ml)
1 20 0 16.2 16.2
16.2
2 20 0 16.2 16.2

Volume of Std FeSO4 solution (V1) = 20 ml

Normality of Std FeSO4 solution (N1) = 0.1024N
Volume of link KMnO4 solution (V2) = 16.2 ml
Normality of link KMnO4 solution (N2) = x N
V1 N1 = V2 N2
V1 N1
N2 =
V2
20 x 0.1102
=
16.2

=0.1360
Normality of standardised KMnO4 solution (N2) = 0.1360 N
TITRATION –II
Standardised KMnO4 solution Vs Unknown FAS solution

Volume of Burette Readings Volume of

FAS (ml) KMnO4 Concordant
S.No.
solution solution Value (ml)
Initial Final
(ml) (ml)
1 20 0 21.4 21.4
21.4
2 20 0 21.4 21.4
TITRATION –II
Volume of standardised KMnO4 solution (V1) = 21.4ml
Normality of standardised KMnO4 solution (N1) = 0.1360 N
Volume of unknown FAS solution (V2) = 20ml
Normality of unknown FAS solution (N2) = x N
V1 N1= V2 N2
V1 N1
N2 =
V2
21.4 x 0.1360
=
20

= 0.1455N
Normality of standardised FAS solution (N2) = 0.1455 N
WEIGHT CALCULATION:
The amount of FAS dissolved
in 1 lit of the solution = (Normality) x (equivalent weight)

The amount of FAS dissolved

Normality x equivalent weight x 1500
in 1500 ml of the solution =
1000

0.1455 x 392 x 1500

=
1000

0.1455 x 392 x 3
=
2

= 85.55 g
The amount of FAS dissolved in 1500 ml of the solution = 85.55 g

RESULT:
1. Normality of standardised KMnO4 solution (N2) = 0.1360 N

2. Normality of standardised FAS solution (N2) = 0.1455 N

3. The amount of FAS dissolved in 1500 ml of the solution = 85.55 g

Ex No:3 Estimation of Oxalic acid
Date:
Aim:
To estimate the amount of oxalic acid dissolved in 500 ml of the given
solution volumetrically. You are provided with a standard solution of
ferrous ammonium sulphate (FAS) of normality 0.1N and potassium
permanganate solution as link solution.

S.No Content Titration-I Titration-II

1 Burette solution KMnO4 solution KMnO4 solution

20 ml of standard 20 ml of unknown
2 Pipette solution
FAS solution Oxalic acid
3 Acid to be added 20ml of 2N H2SO4 20ml of 2N H2SO4

4 Temperature Lab temperature 60 to 700C

Self-indicator Self-indicator
5 Indicator
(KMnO4) (KMnO4)
Appearance of
Appearance of
permanent pale
6 End point permanent pale
pink colour
pink colour
7 Equivalent weight of Oxalic acid = 63

Normality of standard FAS solution = 0.1 N

TITRATION –I
Standard FAS solution Vs Link KMnO4 solution

Volume of Burette Readings Volume of

Concordant
FAS (ml) KMnO4
S.No. Value
solution solution
Initial Final (ml)
(ml) (ml)
1 20 0 20.4 20.4
20.4
2 20 0 20.4 20.4

Volume of Std FAS solution(V1) = 20 ml

Normality of Std FAS solution (N1) = 0.1N
Volume of link KMnO4 solution(V2) = 20.4 ml
Normality of link KMnO4 solution (N2) = x N
V1 N1 = V2 N2
V1 N1
N2 =
V2
20 x 0.1
=
20.4

= 0.0980 N
Normality of standardised KMnO4 solution (N2) = 0.0980 N
TITRATION –II
Standardised KMnO4 solution Vs Unknown Oxalic acid

Burette Readings Volume of

Volume of Concordant
(ml) KMnO4
S.No. Oxalic acid Value
solution
(ml) Initial Final (ml)
(ml)
1 20 0 24.5 24.5
24.5
2 20 0 24.5 24.5

Volume of standardised KMnO4 solution (V1) = 24.5ml

Normality of standardised KMnO4 solution (N1) = 0.0980 N
Volume of unknown oxalic acid solution (V2) = 20ml
Normality of unknown oxalic acid solution (N2) =x N
V1 N1= V2 N2
V1 N1
N2 =
V2
24.5 x 0.0980
=
20

= 0.1200 N
Normality of standardised oxalic acid (N2) =0.1200 N
WEIGHT CALCULATION:
The amount of oxalic acid dissolved
in 1 lit of the solution = (Normality) x (equivalent weight)

The amount of oxalic acid dissolved

Normality x equivalent weight x 500
in 500 ml of the solution =
1000

0.1200 x 63 x 500
=
1000

0.1200 x 63 x 1
=
2

= 3.78 g
The amount of oxalic acid dissolved in 500 ml of the solution = 3.78 g

RESULT:
1. Normality of standardised KMnO4 solution (N2) = 0.0980 N

2. Normality of standardised oxalic acid (N2) = 0.1200 N

3. The amount of oxalic acid dissolved in 500 ml of the solution= 3.78 g

Ex No:4 Estimation of sodium hydroxide
Date:
Aim:
To estimate the amount of sodium hydroxide dissolved in 250 ml of the given
unknown solution volumetrically. You are provided with a standard solution
of sodium carbonate solution of normality 0.0948 N and hydrochloric acid
solution as link solution.

S.No Content Titration-I Titration-II

1 Burette solution HCl solution HCl solution

20 ml of standard 20 ml of unknown
2 Pipette solution
Na2CO3 solution NaOH solution
3 Temperature Lab temperature Lab temperature

4 Indicator Methyl orange Phenolphthalein

Colour change Disappearance of
from straw pink colour
5 End point
yellow to pale
pink
6 Equivalent weight of Sodium hydroxide = 40

Normality of standard Na2CO3 solution = 0.0948 N

TITRATION –I
Standard Na2CO3 solution Vs Link HCl solution
Volume of Burette Readings Volume of
Concordant
Na2CO3 (ml) HCl
S.No. Value
solution solution
Initial Final (ml)
(ml) (ml)
1 20 0 18.4 18.4
18.4
2 20 0 18.4 18.4

Volume of Std Na2CO3 solution (V1) = 20 ml

Normality of Std Na2CO3solution (N1) = 0.0948N
Volume of link HCl solution(V2) = 18.4 ml
Normality of link HCl solution(N2) = x N
V1 N1 = V2 N2
V1 N1
N2 =
V2
20 x 0.0948
=
18.4

= 0.1030 N
Normality of standardised HCl solution(N2) = 0.1030N
TITRATION –II
Standardised HCl solution Vs Unknown NaOH solution

Volume of Burette Readings Volume of

Concordant
NaOH (ml) HCl
S.No. Value
solution solution
Initial Final (ml)
(ml) (ml)
1 20 0 22.2 22.2
22.2
2 20 0 22.2 22.2

Volume of standardised HCl solution (V1) = 22.2ml

Normality of standardised HCl solution (N1) = 0.1030 N
Volume of unknown NaOH solution (V2) = 20 ml
Normality of unknown NaOH solution (N2) =x N
V1 N1= V2 N2
V1 N1
N2 =
V2
22.2 x 0.1030
=
20

= 0.1143 N
Normality of standardised NaOH solution (N2) = 0.1143 N
WEIGHT CALCULATION:
The amount of NaOH dissolved
in 1 lit of the solution = (Normality) x (equivalent weight)

The amount of NaOH dissolved

Normality x equivalent weight x 250
in 250 ml of the solution =
1000

0.1143 x 40 x 250
=
1000

0.1143 x 40 x 1
=
4

= 1.143 g
The amount of NaOH dissolved in 250 ml of the solution = 1.143 g

RESULT:
1. Normality of standardised HCl solution (N2) = 0.1030 N

2. Normality of standardised NaOH solution (N2) = 0.1143 N

3. The amount of NaOH dissolved in 250 ml of the solution= 1.143 g

Ex No:5 Estimation of oxalic acid
Date:
Aim:
To estimate the amount of oxalic acid dissolved in 1250 ml of the given
unknown solution volumetrically. You are provided with a standard solution
of HCl solution of normality 0.1010 N and sodium hydroxide solution as link
solution.

S.No Content Titration-I Titration-II

Unknown oxalic
1 Burette solution Std HCl solution
acid solution
20 ml of NaOH 20 ml of NaOH
2 Pipette solution
solution solution
3 Temperature Lab temperature Lab temperature

4 Indicator Phenolphthalein Phenolphthalein

Disappearance of
Disappearance of
5 End point pink colour
pink colour
6 Equivalent weight of Oxalic acid = 63

Normality of standard HCl solution = 0.1010 N

TITRATION –I
Standard HCl solution Vs link NaOH solution
Volume of Burette Readings Volume of
Concordant
NaOH (ml) HCl
S.No. Value
solution solution
Initial Final (ml)
(ml) (ml)
1 20 0 19.6 19.6
19.6
2 20 0 19.6 19.6

Volume of Std HCl solution (V1) = 20 ml

Normality of Std HCl solution (N1) = 0.1010 N
Volume of link NaOH solution (V2) = 19.6 ml
Normality of link NaOH solution (N2) = x N
V1 N1 = V2 N2
V1 N1
N2 =
V2
20 x 0.1010
=
19.6

= 0.1030 N
Normality of standardised NaOH solution (N2) = 0.1030 N
TITRATION –II
Standardised NaOH solution Vs Unknown Oxalic acid solution
Burette Readings Volume of
Volume of
(ml) Oxalic Concordant
NaOH
S.No. acid Value
solution
Initial Final solution (ml)
(ml)
(ml)
1 20 0 22.8 22.8
22.8
2 20 0 22.8 22.8

Volume of standardised NaOH solution (V1) = 22.8 ml

Normality of standardised NaOH solution (N1) = 0.1030 N
Volume of unknown oxalic acid solution (V2) =20 ml
Normality of unknown oxalic acid solution (N2) =x N
V1 N1= V2 N2
V1 N1
N2 =
V2
22.8 x 0.1030
=
20

= 0.1174 N
Normality of standardised oxalic acid solution (N2) = 0.1174 N
WEIGHT CALCULATION:
The amount of oxalic acid dissolved
in 1 lit of the solution = (Normality) x (equivalent weight)

The amount of oxalic acid dissolved

Normality x equivalent weight x 1250
in 1250 ml of the solution =
1000

0.1174 x 63 x 1250
=
1000

0.1174 x 63 x 5
=
4

= 9.24 g

The amount of oxalic acid dissolved in 1250 ml of the solution = 9.24 g

RESULT:
1. Normality of standardised NaOH solution (N2) = 0.1030 N

2. Normality of standardised oxalic acid solution (N2) = 0.1174 N

3. The amount of oxalic acid dissolved in 1250 ml of the solution= 9.24 g