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VOLUMETRIC ANALYSIS
Introduction
Volumetric analysis involves the quantitative estimation of a substance in solution by
determining the exact volume of one solution required to react completely with a known volume of
another solution. By knowing the volumes of two solutions and the strength of one solution, we will
be able to calculate the quantity of the substance present in the other solution. The commonly used
apparatus in volumetric analysis includes burette, pipette, standard flask and conical flask.
The following are some of the important terms used in volumetric analysis:
1. Titration: The process of determining the exact volume of a solution required to react
completely with a known volume of another solution is called titration.
2. End point: It is the point in the titration which indicated the just completion of a reaction by a
colour change of the solution either by itself or by an indicator.
3. Indicators: An indicator is a substance added to the reaction mixture to indicate the
completion of reaction by change of colour at the end point.
4. Standard solution: A solution of known concentration is called a standard solution.
In volumetric analysis, the concentrations of solutions are expressed in terms of normality or
molarity. Normality is the number of gram equivalent of solute present per litre of the solution, while
molarity is the number of moles of solute present per litre of the solution.
Important points to be remembered in volumetric analysis

1. All the apparatus used should be perfectly clean.

2. The burette and the pipette should be rinsed with the respective solutions before using them.
Use only small quantity of solution for rinsing.
3. Never rinse the conical flask with the given solutions. It is only to be washed with clean water.
4. The made up solution should be shaken well before using for titration.
5. The nozzle of the burette should also be filled with the solution, without any air bubble in it,
before taking the initial burette reading.
6. Use the forefinger to close the pipette.
7. Hold the pipette vertically while draining the solution from it. When the main flow of liquid
ceases, wait for about fifteen seconds and touch the tip of the pipette at the sides of the
conical flask. Never blow the liquid out of the pipette while pipetting out a solution.
8. While taking burette reading, lower meniscus can be taken for colourless solutions and upper
meniscus for coloured solutions. However while pipetting out or making up of any solution, the
lower meniscus is always taken.
9. Solution should be added drop by drop from the burette towards the end of the titration.
10. All the readings should be taken without any parallax error.

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Acidimetry and Alkalimetry

Estimation of an alkali (base) using standard acid solution is called acidimetry and estimation
of an acid using standard alkali solution is called alkalimetry.
When an acid is reacted with a base, neutralization reaction takes place resulting in the formation of
salt and water.
e.g.: NaOH + HCl NaCl + H2O
Both acid and base are colourless. So, in order to identify the completion of the reaction, a
third substance called indicator is used. It is a substance that changes its colour based on the pH of
the solution.
Acid – Base indicators
The indicators commonly used in acid – base reactions are phenolphthalein and methyl
orange. Phenolphthalein is pink in alkali solution, but colourless in acid solution. When one or two
drops of this indicator is added to a known volume of alkali solution, a pink colour is developed. On
adding acid solution into this from burette, the solution turns from pink to colourless as alkali is
completely neutralized. The point at which the pink solution just turns to colourless is taken as the
end point of the reaction. Phenolphthalein is used as indicator in strong acid – strong base titrations
and in weak acid - strong base titrations.
An aqueous solution of methyl orange is golden yellow in alkali solution and orange red in acid
solution. When one or two drops of methyl orange are added into a known volume of alkali, the
solution turns golden yellow. On adding acid solution into this solution from the burette, the golden
yellow solution turns to pale orange red, as the alkali is completely neutralized. The point at which the
golden yellow solution just turns to orange red is taken as the end point of the reaction. Methyl orange
is used as indicator in strong acid - strong base titrations and in strong acid – weak base titrations.
Care should be taken not to add excess of methyl orange indicator.
In acid-base titrations, acid solution is always taken in the burette and the base is pipette out
into a conical flask.
Some common types of titrations, the indicators used and examples are given in the table:

Colour change at
Type of Titration Indicator(s) used Examples
the end point
Strong Acid (SA) vs Phenolphthalein Pink to colourless. HCl vs NaOH (KOH)
Strong Base (SB) or, H2SO4 vs NaOH (KOH)
Methyl Orange Golden yellow to HNO3 vs NaOH (KOH)
orange red.
HCl vs Na2CO3 (K2CO3 or NH4OH)
Strong Acid (SA) vs Golden yellow to
Methyl Orange H2SO4 vs Na2CO3 (K2CO3 or NH4OH)
Weak Base (WB) orange red.
HNO3 vs Na2CO3 (K2CO3 or NH4OH)
Weak Acid (WA) vs Phenolphthalein Pink to colourless. H2C2O4 vs NaOH (KOH)
Strong Base (SB) CH3-COOH vs NaOH (KOH)

Memorise - SAW Me - for remembering the indictor used and type of reaction [SA – Strong
Acid, W – Weak Base, Me – Methyl Orange], In all other cases, use Phenolphthalein indicator.

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Important points to be remembered for calculation of the normality and mass of unknown solution:
In volumetric analysis, the concentration of the solution is mainly expressed in Normality.
It is the number of gram equivalents of solute present per litre of the solution.
Number of gram eauivalents of solute
i.e. Normality (N) =
Volume of solution in litre
Given mass in gram
Number of gram equivalents =
Equivalent weight
Mass per litre
So, Normality (N) =
Equialent weight
From this equation, mass per litre of acid or base can be calculated by the equation,
mass per litre of acid (base) = Normality x Equivalent weight
We are making up 100 mL of the solution. So, from the mass per litre, we can calculate mass of the
Mass per litre x 100 Mass per litre
acid (base) in the whole of the given solution (i.e. 100 mL) = =
1000 10
Molar mass
Equivalent weight of an acid =
Basicity
For monobasic acids like HCl, HNO3, CH3-COOH etc. basicity = 1.
So, for them, equivalent weight = Molar mass.
For dibasic acids like H2SO4, H2C2O4 (oxalic acid) etc. basicity = 2.
Molar mass
So, for these acids, equivalent weight =
2
Molar mass
Equivalent weight of a base =
Acidity
For monoacidic bases like NaOH, KOH, NH4OH etc., acidity = 1.
So, for them, equivalent weight = Molar mass.
For diacidic bases like Ca(OH)2 and for basic salts like Na2CO3, K2CO3 etc., acidity = 2.
Molar mass
So, for them, equivalent weight =
2
For calculating the unknown normality of a solution, we can use the equation, N1V1 = N2V2
For simplicity, acid is taken as 1 and base is taken as 2 in all acidimetry-alkalimetry titrations.
Equivalent weight of some acids and bases
Acid/Base Equivalent weight
Hydrochloric acid (HCl) 36.5
Sulphuric acid (H2SO4) 49
Nitric acid (HNO3) 63
Oxalic acid dihydrate (H2C2O4.2H2O) 63
Sodium hydroxide (NaOH) 40
Potassium hydroxide (KOH) 56
Sodium carbonate (Na2CO3) 53
Potassium carbonate (K2CO3) 69

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Experiment No. 1
Estimation of Sodium hydroxide using std. HCl
Aim
Estimate the mass of sodium hydroxide in the whole of the given solution. You are supplied
with a standard solution of hydrochloric acid containing 3.7 g/L.
Principle
The estimation is based on the reaction between sodium hydroxide and hydrochloric acid.
NaOH + HCl NaCl + H2O
Since HCl is monobasic, its Equivalent weight is same as its molecular mass. i.e. 36.5. As per
the equation, one equivalent of HCl reacts with 1 mol of NaOH solution. Therefore, the Equivalent
weight of NaOH is equal to its molecular mass (40). By determining the volume of HCl reacting with
given volume of the made up solution, mass of NaOH in the whole of the given solution can be
calculated.
Procedure
A clean burette is rinsed with the given HCl solution and is filled with HCl upto the zero mark.
The given NaOH solution is made upto 100 mL in a clean standard flask. It is shaken well to get
uniform concentration. A clean pipette is rinsed with the made up solution. 20 mL of the made up
solution (NaOH) is pipetted out into a clean conical flask. Add one or two drops phenolphthalein
indicator and titrated against HCl from the burette. At the end point, the pink colour changes to
colourless. The final burette reading is noted. The experiment is repeated to get concordant values.
From the volume of the acid, we can find out the mass of NaOH.
Observations
NaOH vs HCl
Sl. Volume of Burette Reading Volume of HCl
No. NaOH (in mL)
Initial Final (in mL)
1. 20 0
2. 20 0
3. 20 0
Concordant value =
Calculations
Mass per litre of HCl = 3.7 g/L
Equivalent weight of HCl = 36.5
Mass per litre 3.7
Normality of HCl, N1 = = = 0.1014 N
Equialent weight 36.5

Volume of HCl (V1) = ………….. mL

Volume of NaOH solution pipetted out, V2 = 20 mL
Normality of NaOH (N2) = ?
From normality equation, N1V1 = N2V2,
N1 V1 0.1014 𝑥………..
N2 = = = …………. N
V2 …………..

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Equivalent weight of NaOH = 40

Mass per litre of NaOH solution = Normality x Equivalent weight = ………… x 40 = ………………. g/L
Mass per litre …………
The mass of NaOH in the whole of the given solution = = = …….. g
10 10
Result
The mass of NaOH in the whole of the given solution = ………………… g
---------------------------------------------------------------------------------------------------------------------------------------

Estimation of NaOH: Calculation – Demonstration

Suppose the concordant value of the titration is 19.5
Observations
NaOH vs HCl
Sl. Volume of Burette Reading Volume of HCl
No. NaOH (in mL)
Initial Final (in mL)
1. 20 0 19.8 19.8
2. 20 0 19.5 19.5
3. 20 0 19.5 19.5
Concordant value = 19.5
Calculations
Mass per litre of HCl = 3.7 g/L
Equivalent weight of HCl = 36.5
Mass per litre 3.7
Normality of HCl, N1 = = = 0.1014 N
Equialent weight 36.5

Volume of HCl (V1) = 19.5 mL

Volume of NaOH solution pipetted out, V2 = 20 mL
Normality of NaOH (N2) = ?
From normality equation, N1V1 = N2V2,
N1 V1 0.1014 𝑥 19.5
N2 = = = 0.0989 N
V2 20
Equivalent weight of NaOH = 40
Mass per litre of NaOH solution = Normality x Equivalent weight = 0.0989 x 40 = 3.956 g/L
Mass per litre 3.956
The mass of NaOH in the whole of the given solution = = = 0.3956 g
10 10
Result
The mass of NaOH in the whole of the given solution = 0.3956 g
&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&

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Experiment No. 2
Estimation of Sodium carbonate using std. H2SO4
Aim
Estimate the mass of sodium carbonate (Na2CO3)in the whole of the given solution. You are
supplied with a standard solution of sulphuric acid containing 4.85 g/L.
Principle
The estimation is based on the reaction between sodium carbonate and sulphuric acid.
Na2CO3 + H2SO4 Na2SO4 + CO2 + H2O
Since H2SO4 is dibasic, its Equivalent weight is the half of the molecular mass. i.e. 49. As per
the equation, one equivalent of H2SO4 reacts with 1 equivalent of Na2CO3 solution. Therefore, the
Equivalent weight of Na2CO3 is equal to half of its molecular mass (53). By determining the volume of
H2SO4 reacting with given volume of the made up solution, mass of Na2CO3 in the whole of the given
solution can be calculated.
Procedure
A clean burette is rinsed with the given H2SO4 and is filled with H2SO4 upto the zero mark. The
given Na2CO3 solution is made upto 100mL in a clean standard flask. It is shaken well to get uniform
concentration. A clean pipette is rinsed with the made up solution. 20 mL of the made up solution
(Na2CO3) is pipetted out into a clean conical flask. One or two drops methyl orange indicator is added
and titrated against H2SO4 from the burette till the golden yellow colour changes to orange red. The
final burette reading is noted. The experiment is repeated to get concordant values. From the volume
of the acid, we can find out the mass of Na2CO3.
Observations
Na2CO3 vs H2SO4
Sl. Volume of Burette Reading Volume of
No. Na2CO3 (in
Initial Final H2SO4 (in mL)
mL)
1. 20 0
2. 20 0
3. 20 0
Concordant value =
Calculations
Mass per litre of H2SO4 = 4.85 g/L
Equivalent weight of H2SO4 = 49
Mass per litre 4.85
Normality of H2SO4, N1 = = = 0.0989 N
Equialent weight 49
Volume of H2SO4 (V1) = ………….. mL
Volume of Na2CO3 solution pipetted out, V2 = 20 mL
Normality of Na2CO3 (N2) = ?
From normality equation, N1V1 = N2V2,
N1 V1 0.0989 𝑥………
N2 = = = …………. N
V2 20

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Equivalent weight of Na2CO3 = 53

Mass per litre of Na2CO3 solution = Normality x Equivalent weight = ………… x 53 = ………………. g/L
Mass per litre …………
The mass of Na2CO3 in the whole of the given solution = = = …….. g
10 10
Result
Mass of Na2CO3 in the whole of the given solution = ………………… g

---------------------------------------------------------------------------------------------------------------------------------------

Estimation of Sodium carbonate: Calculation – Demonstration

Suppose the concordant value of the titration is 21.2
Observations
Na2CO3 vs H2SO4
Sl. Volume of Burette Reading Volume of
No. Na2CO3 (in
Initial Final H2SO4 (in mL)
mL)
1. 20 0 21.5 21.5
2. 20 0 21.2 21.2
3. 20 0 21.2 21.2
Concordant value = 21.2
Calculations
Mass per litre of H2SO4 = 4.85 g/L
Equivalent weight of H2SO4 = 49
Mass per litre 4.85
Normality of H2SO4, N1 = = = 0.0989 N
Equialent weight 49
Volume of H2SO4 (V1) = 21.2 mL
Volume of Na2CO3 solution pipetted out, V2 = 20 mL
Normality of Na2CO3 (N2) = ?
From normality equation, N1V1 = N2V2,
N1 V1 0.0989 𝑥 21.2
N2 = = = 0.1048 N
V2 20
Equivalent weight of Na2CO3 = 53
Mass per litre of Na2CO3 solution = Normality x Equivalent weight = 0.1048 x 53 = 5.554 g/L
Mass per litre 5.554
The mass of Na2CO3 in the whole of the given solution = = = 0.5554 g
10 10
Result
Mass of Na2CO3 in the whole of the given solution = 0.5554 g

)))))))))))))))))))))))))))))))))))))))))))))))))))))))))))))))))))))))))))))))))))))))))))))))))))))))))))))))))))))))))))))))))))))))))

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Experiment No. 3
Estimation of Oxalic acid using std. KOH
Aim
Estimate the mass of oxalic acid in the whole of the given solution. You are supplied with a
standard solution of potassium hydroxide containing 5.5 g/L.
Principle
The estimation is based on the reaction between potassium hydroxide and oxalic acid.
2KOH + H2C2O4 K2C2O4 + 2H2O
Since oxalic acid (H2C2O4) is dibasic, the Equivalent weight of crystalline oxalic acid is half of
the molecular mass. i.e. 63. As per the equation, it is clear that 2 moles of KOH will react with 1 mole
(i.e. 2 equivalents) of oxalic acid. So 1 mole of KOH will react with 1 equivalent of oxalic acid. Hence
the Equivalent weight of KOH is the same as its molecular mass (i.e. 56). By determining the volume of
oxalic acid reacting with given volume of KOH, mass of oxalic acid in the whole of the given solution
can be calculated.
Procedure
The given oxalic acid solution is made upto 100 mL in a clean standard flask. It is shaken well
to get uniform concentration. A clean burette is rinsed with the made up oxalic acid solution upto the
zero mark. A clean pipette is rinsed with the given KOH solution. 20 mL of the KOH solution is
pipetted out into a clean conical flask. One or two drops phenolphthalein indicator is added and
titrated against oxalic acid from the burette till the pink colour changes to colourless. The final burette
reading is noted. The experiment is repeated to get concordant values. From the volume of the acid,
we can find out its mass.
Observations
H2C2O4 vs KOH
Sl. Volume of Burette Reading Volume of
No. KOH (in mL)
Initial Final H2C2O4 (in mL)
1. 20 0
2. 20 0
3. 20 0
Concordant value =
Calculations
Mass per litre of KOH = 5.5 g/L
Equivalent weight of KOH = 56
Mass per litre 5.5
Normality of KOH, N2 = = = 0.0982 N
Equialent weight 56
Volume of KOH solution pipetted out, V2 = 20 mL
Volume of oxalic acid [H2C2O4] (V1) = ………….. mL
Normality of H2C2O4 (N1) = ?
From normality equation, N1V1 = N2V2,

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N2 V2 0.0982 𝑥 20
N1 = = = …………. N
V1 ………
Equivalent weight of oxalic acid = 63
Mass per litre of oxalic acid solution = Normality x Equivalent weight = ………… x 63 = ………………. g/L
Mass per litre …………
The mass of oxalic acid in the whole of the given solution = = = …….. g
10 10

Result
Mass of oxalic acid in the whole of the given solution = ………………… g

Estimation of Oxalic acid: Calculation – Demonstration

Suppose the concordant value of the titration is 18.7
Observations
H2C2O4 vs KOH
Sl. Volume of Burette Reading Volume of
No. KOH (in mL)
Initial Final H2C2O4 (in mL)
1. 20 0 19.0 19.0
2. 20 0 18.7 18.7
3. 20 0 18.7 18.7
Concordant value = 18.7
Calculations
Mass per litre of KOH = 5.5 g/L
Equivalent weight of KOH = 56
Mass per litre 5.5
Normality of KOH, N2 = = = 0.0982 N
Equialent weight 56
Volume of KOH solution pipetted out, V2 = 20 mL
Volume of oxalic acid [H2C2O4] (V1) = 18.7 mL
Normality of H2C2O4 (N1) = ?
From normality equation, N1V1 = N2V2,
N2 V2 0.0982 𝑥 20
N1 = = = 0.1050 N
V1 18.7
Equivalent weight of oxalic acid = 63
Mass per litre of oxalic acid solution = Normality x Equivalent weight = 0.1050 x 63 = 6.615 g/L
Mass per litre 6.615
The mass of oxalic acid in the whole of the given solution = = = 0.6615 g
10 10
Result
Mass of oxalic acid in the whole of the given solution = 0.6615 g

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Experiment No. 4
Estimation of Nitric Acid using std. K2CO3
Aim
Estimate the mass of nitric acid (HNO3)in the whole of the given solution. You are supplied
with a standard solution of potassium carbonate (K2CO3) containing 6.82 g/L.
Principle
The estimation is based on the reaction between potassium carbonate and nitric acid.
K2CO3 + 2 HNO3 2 KNO3 + CO2 + H2O
Since HNO3 is monobasic, its Equivalent weight is equal to the molecular mass. i.e. 63. As per
the equation, one equivalent of HNO3 reacts with half equivalent of K2CO3 solution. Therefore, the
Equivalent weight of K2CO3 is equal to half of its molecular mass (69). By determining the volume of
HNO3 reacting with given volume of the K2CO3 solution, mass of HNO3 in the whole of the given
solution can be calculated.
Procedure
The given HNO3 solution is made upto 100 mL in a clean standard flask. It is shaken well to get
uniform concentration. A clean burette is rinsed with the made up solution and is filled upto the zero
mark. A clean pipette is rinsed with the given K2CO3 solution. 20 mL of this solution is pipetted out
into a clean conical flask. One or two drops of methyl orange indicator is added and titrated against
HNO3 solution from the burette till the golden yellow colour changes to orange red. The final burette
reading is noted. The experiment is repeated to get concordant values. From the volume of the acid,
we can find out its mass.
Observations
HNO3 vs K2CO3
Sl. Volume of Burette Reading Volume of
No. K2CO3 (in mL)
Initial Final HNO3 (in mL)
1. 20 0
2. 20 0
3. 20 0
Concordant value =
Calculations
Mass per litre of K2CO3 = 6.82 g/L
Equivalent weight of K2CO3 = 69
Mass per litre 6.82
Normality of K2CO3, N2 = = = 0.0988 N
Equialent weight 69
Volume of K2CO3 solution pipetted out, V2 = 20 mL
Volume of nitric acid [HNO3] (V1) = ………….. mL
Normality of HNO3 (N1) = ?
From normality equation, N1V1 = N2V2,
𝑁2 𝑉2 0.0988 𝑥 20
N1 = = = …………. N
𝑉1 ………

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Equivalent weight of nitric acid = 63

Mass per litre of HNO3 = Normality x Equivalent weight = ………… x 63 = ………………. g/L
Mass per litre …………
The mass of HNO3 in the whole of the given solution = = = …….. g
10 10

Result
Mass of HNO3 in the whole of the given solution = ………………… g
……………………………………………………………………………………………………………………………………………………………

Estimation of Nitric acid: Calculation – Demonstration

Suppose the concordant value of the titration is 22.5
Observations
HNO3 vs K2CO3
Sl. Volume of Burette Reading Volume of
No. K2CO3 (in mL)
Initial Final HNO3 (in mL)
1. 20 0 22.5 22.5
2. 20 0 22.5 22.5
Concordant value = 22.5
Calculations
Mass per litre of K2CO3 = 6.82 g/L
Equivalent weight of K2CO3 = 69
Mass per litre 6.82
Normality of K2CO3, N2 = = = 0.0988 N
Equialent weight 69
Volume of K2CO3 solution pipetted out, V2 = 20 mL
Volume of nitric acid (V1) = 22.5 mL
Normality of HNO3 (N1) = ?
From normality equation, N1V1 = N2V2,
𝑁2 𝑉2 0.0988 𝑥 20
N1 = = = 0.0878 N
𝑉1 22.5
Equivalent weight of nitric acid = 63
Mass per litre of HNO3= Normality x Equivalent weight = 0.0878 x 63 = 5.5314 g/L
Mass per litre 5.5314
The mass of HNO3 in the whole of the given solution = = = 0.5531 g
10 10
Result
Mass of HNO3 in the whole of the given solution = 0.5531 g
***********************************************************************************

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PERMANGANOMETRY
Permanganometric titrations involve redox reactions in which potassium permanganate is the
oxidising agent. It is a good oxidising agent in the acidic medium.
2KMnO4 + 3 H2SO4 K2SO4 + 2 MnSO4 + 3 H2O+ 5[O]
Or, MnO4– + 8 H+ + 5e– Mn2+ + 4 H2O
Thus, acidified permanganate is largely used in the estimation of reducing agents such as
ferrous salts, oxalic acid etc. Only dilute sulphuric acid is used for making the reaction medium acidic.
HCl cannot be used as it reacts with KMnO4 to evolve chlorine gas. Nitric acid also cannot be used as it
is an oxidising agent by itself.
Potassium permanganate is purple in colour. During redox reaction, the purple colour is
discharged because KMnO4 gets reduced to colourless potassium sulphate and manganous sulphate.
Thus KMnO4 acts as a self-indicator.
In all permanganometric titrations, KMnO4 solution is taken in the burette and burette readings are
taken at the upper meniscus.

Points to be remembered in Permanganometric titrations:

❖ In Permanganometric titrations, KMnO4 is always taken in the burette.

❖ While filling the burette and taking the measurements, upper meniscus is taken (since KMnO 4
is a coloured solution).
❖ In order to make the solution acidic, always add one test tube full of dil. H 2SO4 (about 15 mL)
to the pipetted solution.
❖ No indicators are needed for the titration, since KMnO4 itself is coloured.
❖ At the end point, permanent pink colour appears.
❖ When oxalic acid is used, after pipetting the solution and adding the acid, it is heated to about
600C.
❖ Titrations using KMnO4 is an example for redox titrations.
❖ Equivalent weights to be memorized in Permanganometric titrations are:

Compound Equivalent
weight
KMnO4 31.6
Mohr’s salt [FeSO4.(NH4)SO4.6H2O] 392
Hydrated oxalic acid [H2C2O4.2H2O] 63

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Experiment No. 1
Estimation of potassium permanganate using Mohr’s salt
Aim:
Estimate the mass of KMnO4 in the whole of the given solution. You are supplied with a
standard solution of Mohr’s salt containing 40 g per litre.
Principle
The estimation is based on the reaction between Mohr’s salt and potassium permanganate.
2KMnO4 + 10FeSO4.(NH4)2SO4.6H2O + 8H2SO4 K2SO4 + 2MnSO4 + 68H2O + 10(NH4)2SO4 + 5Fe2(SO4)3
2+ -
The ionic equation is: 5Fe + MnO4 + 8H + 5Fe3+ + Mn2+ + 4H2O
Equivalent weight of KMnO4 = 31.6
Equivalent weight of Mohr’s salt = 392
A definite volume of standard solution of Mohr’s salt is titrated against potassium
permanganate solution. At the end point, a permanent pink colour is formed. From the volume of
potassium permanganate solution used, the normality and mass of KMnO 4 in the whole of the
solution can be calculated.
Procedure
The given Mohr’s salt solution is made upto 100 mL in a standard flask. 20 mL of the Mohr’s
salt solution is pipetted out into a clean conical flask, about 10 mL of dil. H2SO4 is added. The solution
is titrated with the potassium permanganate solution taken in the burette. The first few drops of
potassium permanganate take some time for decolourisation. The end point is the appearance of
permanent pink colour. The titration is repeated till concordant values are obtained. From the titre
values, the normality and mass of potassium permanganate in the whole of the given solution can be
calculated.
Observations
KMnO4 vs Mohr’s salt
Sl. Volume of Burette Reading Volume of
No. Mohr’s salt
Initial Final KMnO4 (in mL)
soln. (in mL)
1. 20 0
2. 20 0
3. 20 0
Concordant value =
Calculations
Mass per litre of Mohr’s salt = 40 g/L
Equivalent weight of Mohr’s salt = 392
Mass per litre 40
Normality of Mohr’s salt, N2 = = 392
= 0.1020 N
Equialent weight

Volume of Mohr’s salt solution pipetted out, V2 = 20 mL

Volume of KMnO4 solution (V1) = ………….. mL

Prepared by Anil Kumar K L, APHSS ADICHANALLOOR, KOLLAM 13

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Normality of KMnO4 (N1) = ?

From normality equation, N1V1 = N2V2,
N2 V2 0.1020 𝑥 20
N1 = V1
= ………
= …………. N

Equivalent weight of KMnO4 = 31.6

Mass per litre of KMnO4 = Normality x Equivalent weight = ………… x 31.6 = ………………. g/L
Mass per litre …………
The mass of KMnO4 in the whole of the given solution = 10
= 10
= …….. g

Result
Mass of KMnO4 in the whole of the given solution = ……………… g

Estimation of Potassium permanganate: Calculation – Demonstration

In permanganometric titrations, let’s take all the terms related to KMnO4 be 1.
Suppose the concordant value of the titration is 19.6
Observations
KMnO4 vs Mohr’s salt
Sl. Volume of Burette Reading Volume of
No. Mohr’s salt
Initial Final KMnO4 (in mL)
soln. (in mL)
1. 20 0 20.1 20.1
2. 20 0 19.6 19.6
3. 20 0 19.6 19.6
Concordant value = 19.6
Calculations
Mass per litre of Mohr’s salt = 40 g/L
Equivalent weight of Mohr’s salt = 392
Mass per litre 40
Normality of Mohr’s salt, N2 = = = 0.1020 N
Equialent weight 392

Volume of Mohr’s salt solution pipetted out, V2 = 20 mL

Volume of KMnO4 solution (V1) = 19.6 mL
Normality of KMnO4 (N1) = ?
From normality equation, N1V1 = N2V2,
N2 V2 0.1020 𝑥 20
N1 = = = 0.1041 N
V1 19.6
Equivalent weight of KMnO4 = 31.6
Mass per litre of KMnO4 = Normality x Equivalent weight = 0.1041 x 31.6 = 3.289 g/L
Mass per litre 3.289
The mass of KMnO4 in the whole of the given solution = = = 0.3289 g
10 10
Result
Mass of KMnO4 in the whole of the given solution = 0.3289 g
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Prepared by Anil Kumar K L, APHSS ADICHANALLOOR, KOLLAM 14

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Experiment No. 2
Estimation of Oxalic acid using KMnO4
Aim
Estimate the mass of oxalic acid in the whole of the given solution. You are supplied with a
standard solution of potassium permanganate containing 3.1 g/L
Principle
The estimation is based on the reaction between oxalic acid and potassium permanganate.
2 KMnO4 + 3 H2SO4 + 5H2C2O4.2H2O K2SO4 + 2MnSO4 + 18H2O + 10 CO2
The ionic equation is: 5C2O42- + 2MnO4- + 16H+ 10 CO2 + 2Mn2+ + 8H2O
Equivalent weight of KMnO4 = 31.6
Equivalent weight of oxalic acid = 63
A definite volume of standard solution of oxalic acid is titrated against potassium
permanganate solution. At the end point, a permanent pink colour is formed. From the volume of
potassium permanganate solution used, the normality and mass of oxalic acid in the whole of the
solution can be calculated.
Procedure
The given oxalic acid solution is made upto 100 mL in a standard flask. 20 mL of the made up
solution is pipetted out into a clean conical flask, about 10 mL of dil. H2SO4 is added and the mixture is
heated to 60 to 700C. The solution is then titrated with the potassium permanganate solution taken in
the burette. The first few drops of potassium permanganate take some time for decolourisation. The
end point is the appearance of permanent pink colour. The titration is repeated till concordant values
are obtained. From the titre values, the normality and mass of oxalic acid in the whole of the given
solution can be calculated.
Observations
KMnO4 vs Oxalic acid
Sl. Volume of Burette Reading Volume of
No. Oxalic acid
Initial Final KMnO4 (in mL)
soln. (in mL)
1. 20 0
2. 20 0
3. 20 0
Concordant value =
Calculations
Mass per litre of KMnO4 = 3.1 g/L
Equivalent weight of KMnO4 = 31.6
Mass per litre 3.1
Normality of KMnO4, N1 = = = 0.0981 N
Equialent weight 31.6
Volume of KMnO4 solution (V1) = ………….. mL
Volume of oxalic acid solution pipetted out, V2 = 20 mL

Prepared by Anil Kumar K L, APHSS ADICHANALLOOR, KOLLAM 15

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Normality of oxalic acid (N2) = ?

From normality equation, N1V1 = N2V2,
𝑁1 𝑉1 0.0981 𝑥……
N2 = = = …………. N
𝑉2 20
Equivalent weight of oxalic acid = 63
Mass per litre of oxalic acid = Normality x Equivalent weight = ………… x 63 = ………………. g/L
Mass per litre …………
The mass of oxalic acid in the whole of the given solution = = 10
= …….. g
10
Result
Mass of oxalic acid in the whole of the given solution = ……………… g

----------------------------------------------------------------------------------------------------------------------------------------
Estimation of Oxalic acid: Calculation – Demonstration
Suppose the concordant value of the titration is 20.5
Observations
KMnO4 vs Oxalic acid
Sl. Volume of Burette Reading Volume of
No. Oxalic acid
Initial Final KMnO4 (in mL)
soln. (in mL)
1. 20 0 20.8 20.8
2. 20 0 20.5 20.5
3. 20 0 20.5 20.5
Concordant value = 20.5
Calculations
Mass per litre of KMnO4 = 3.1 g/L
Equivalent weight of KMnO4 = 31.6
Mass per litre 3.1
Normality of KMnO4, N1 = = = 0.0981 N
Equialent weight 31.6
Volume of KMnO4 solution (V1) = 20.5 mL
Volume of oxalic acid solution pipetted out, V2 = 20 mL
Normality of oxalic acid (N2) = ?
From normality equation, N1V1 = N2V2,
N1 V1 0.0981 𝑥 20.5
N2 = = = 0.1005 N
V2 20
Equivalent weight of oxalic acid = 63
Mass per litre of oxalic acid = Normality x Equivalent weight = 0.1005 x 63 = 6.3315 g/L
Mass per litre 6.3315
The mass of oxalic acid in the whole of the given solution = = = 0.63315 g
10 10
Result
Mass of oxalic acid in the whole of the given solution = 0.63315 g

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Prepared by Anil Kumar K L, APHSS ADICHANALLOOR, KOLLAM 16