LAB MANUAL

ENGINEERING
SCIENCE LAB - I&II
CHEMISTRY (2007)
 ENGINEERING CHEMISTRY

ENGINEERING
CHEMISTRY LAB
SYLLABUS
On completion of the course the student will be able to:

Practical Volumetric Analysis

Single Titration
1. Standardisation of HCl
2. Standardisation of NaOH Double Titrations
3. Estimation of NaOH
4. Estimation of KOH
5. Estimation of Na2 CO3
6. Estimation of K2 CO3
7. Estimation of HCl
8. Estimation of HNO3
9. Estimation of H2 SO4
10. Estimation of Oxalic acid
11. Standardisation of KMnO4
12. Estimation of Oxalic acid
13. Estimation of Fe 2+ ion
14. Estimation of Mohr’s Salt
15. Determination of PH of Solution
16. Estimation of Zinc using EDTA
17. Estimation of Magnesium Using EDTA

REFERENCE:
Prof. A. O. THOMAS – PRACTICAL CHEMISTRY – Eight Edition 2000

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VOLUMETRIC ANALYSIS
It is a method of quantitative chemical analysis. It involves the determination of concentration
of a solution by making use of another suitable solution whose concentration is accurately known.
The reactants in the form of solutions are made to react.

Molarities of a solution: It is the number of gram moles of solute present in one liter of solution.

Normality of a solution: It is the number of gram equivalents of solute present in one liter of
solution.

Standard solution: The solution whose concentration is known is called a standard solution. A
standard solution contains a known weight of a substance in a known volume of the solution.

Titration and end point: It is the process of finding out the exact volume of a solution required to
react completely with a known volume of standard solution. The exact stage at which a reaction is just
complete is called the end point of the titration.

Indicators: These are the substances used in volumetric analysis to point out the end point of a
chemical reaction by change of color. The common indicators used for acid-base titration are methyl
orange and phenolphthalein.

Phenolphthalein: It is a colorless weak acid with pH range 8 — 9.8. This indicator appears as
colorless in acid and pink in alkali solution.

Methyl orange: It is a weak base with pH range of 3.1 — 4.5. This indicator appears golden yellow
color in basic medium and red orange color in acid medium. The choice of indicators of a titration
depends upon the nature of the acid and base. If both acid and base are strong either phenolphthalein
or methyl orange can be used. in titrations of strong base against weak acid only phenolphthalein can
be used and if base is weak and acid is strong, only methyl orange can be used as indicator.

Principles of volumetric analysis: Let V1 and V2 be the volume of solutions reacting. If NI and N2 are
the Normality’s of the two solutions respectively, then by normality formula, N1V1 = N2V2.

Acidimetry and alkalimetry: Estimation of alkali solutions using standard acid solution is called
acidimetry. In reactions between acid and alkali, indicators commonly used are phenolphthalein and
methyl orange. Phenolphthalein is pink in alkali solution but colorless in acid solution. When one or
two drops of the indicator are added to an alkali solution, the whole solution turns pink. But when
acid is carefully added to the pink solution, the solution turns from pink to colorless when alkali is
completely neutralized by the acid. The end point is reached when the color just changes from pink to
colorless.

Permanganometry: Estimation of substances using potassium permanganate is known as

permanganometry. Potassium permanganate KMn04 is a strong oxidizing agent. It is largely used as a
titrant for the estimation of various reducing agents such as oxalic acid, ferrous sulphate, Mohr’s salt
etc. The titration is carried out in acidic medium. The solution is made sufficiently acidic so as to
prevent the formation of manganese dioxide or potassium manganate. The oxidizing action of KMn0 4
is due to the following reaction.
2 KMnO4 + 3 H2SO4 →K2SO4 + 2 MnSO4 + 3 H20 + 5 [0]
This oxygen oxidizes reducing agents such as oxalic acid, ferrous sulphate etc. During the reaction,
KMn04 undergoes reduction to form colorless potassium sulphate and Manganous sulphate.
Using a standard solution of potassium permanganate, solutions of reducing agents can be estimated.
Potassium permanganate solution is pink in color and when reduced, changes into potassium and

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manganous salts which are colorless in solution. Therefore reducing agents decolourise the pink
solution.
So no other indicator is required to denote the end point in the titrations with potassium
permanganate. Potassium permanganate acts as a self indicator. KMn04 solution should always be
taken in the burette. The upper meniscus burette reading to be taken.

PREPARATION OF STANDARD SOLUTIONS

In volumetric analysis, the amount of a substance (acid, base or salt) is estimated using a
standard solution. A solution of known concentration (Normality or Molarity) is called a standard
solution. Some of the standard solutions are prepared by weighing out accurately and dissolving the
weighed solute in a suitable solvent and making up the solution to a known volume. Standard
solutions of oxalic acid, sodium carbonate, ferrous ammonium sulphate (Mohr’s salt) etc. are prepared
in this way. These substances are available in the pure form and are called primary standard
substances. Their solutions of known concentrations are called primary standard solutions as other
solutions are standardized against them. A primary standard substance must have the following
characteristics:

(1) It should be easily available in the pure state.

(2) It should be stable and unaffected by the atmosphere.
(3) It should not decompose on storage.
(4) It should be readily soluble in water.

Substances which do not meet the above requirements are called secondary standard
substances. Standard solutions of these substances cannot be prepared by dissolving their known
amount in a solvent. For the preparations of standard solutions of such substances, as HCl, H2SO4,
KMnO4, NaOH etc. solutions of approximate concentration are prepared and then standardized by
titrating against a suitable primary standard solution.

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OBSERVATION Na2CO3 X HCl (Methyl orange)

Sl no Volume of sodium carbonate Burette reading Volume of HCl
solution pipetted in ml solution used (ml)
Innitial Final

Volume of HCl used , VHCl = -------------- ml

CALCULATIONS:

Normality of sodium carbonate solution =0.1 N

Volume of sodium carbonate solution = 20 ml

Volume of hydrochloric acid, used, VHCl = --------- ml

Normality of HCl = N HCl

V HCl X NHCl = V Na2CO3 X N Na2CO3

N HCl = V Na2CO3 X N Na2CO3

V HCl

Weight of HCl= N HCl X 36.5= ------------ g/L

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Expt. No: 1
Date:
STANDARDISATION OF HYDROCHLORIC ACID

AIM:
Standardise and estimate the amount of hydrochloric acid in one litre of the solution. You are
provided with decinormal solution of sodium carbonate.

PRINCIPLE:
Standardisation is based on the neutralisation reaction between hydrochloric acid and sodium
carbonate solution.

Na2CO3 + 2HCl 2 NaCl +CO2 +H2O

PROCEDURE:
20ml of sodium carbonate solution is pipetted out into a clean conical flask. A drop of methyl
orange is added as indicator. It gives a yellow colour to the solution. This is titrated against
hydrochloric acid taken in the burette. The endpoint is change of colour from yellow to pink. The
titration is repeated to get concordant values.

RESULT:

1. Normality of hydrochloric acid = ----------------N

2. Weight of HCl per litre of the solution= ---------------g

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OBSERVATION:-

NaOH X H2SO4 ( Phenolphthalein indicator)

Sl no Volume of sodium hydroxide Burette reading Volume of H2SO4

solution pipetted in ml solution used (ml)
Initial Final

Volume of H2SO4 used , VH2SO4 = -------------- ml

CALCULATIONS:

Normality of sulphuric acid solution =0.1 N

Volume of sulphuric acid solution, Va = ------ml

Volme of sodium hydroxide solution , Vb= 20 ml

Normality of NaOH Solution =Nb

V a X Na = Vb X N b

Nb = V a X Na

Vb

Weight of NaOH = N b X 40= ------------ g/L

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Expt. No: 02
Date
STANDARDISATION OF SODIUM HYDROXIDE

AIM:

Standardise the given sodium hydroxide solution and estimate the weight of sodium hydroxide per
litre of the solution. You are provided with decinormal solution of sulphuric acid.

PRINCIPLE:

Standardisation is based on the neutralisation reaction between sodium hydroxide and sulphuric acid.

2 NaOH + H2SO4 Na2SO4 +2 H2O

PROCEDURE:

20ml of sodium hydroxide solution is pipetted out into a clean conical flask. A drop of
phenolphthalein is added as indicator. It gives a pink colour to the solution. This is titrated against
sulphuric acid taken in the burette. The endpoint is just disappearance of pink colour. The titration is
repeated to get concordant values.

RESULT:

1. Normality of sodium hydroxide = ----------------N

2. Weight of NaOH per litre of the solution= ---------------g

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OBSERVATION:

Std NaOH Vs HCl (Phenolphthalein)

Trail BURETTE READING( in ml) VOLUME HCl USED

No: (in ml)
INITIAL FINAL

Titre Value=……….ml

CALCULATION:

N1V1=N2V2
N1= Normality of NaOH solution= (Wt per liter) / (Eqvt wt) =4/40= 0.1N

V1= Vol of NaOH soln = 20ml

V2= Vol of HCl soln = ……….ml

N2= Normality of HCl solution= (N1V1) / V2 = (0.1N x 20) / (………) =….N

Normality = (Wt per liter) / (Eqvt wt)

(Wt per liter) = Normality x Eqvt wt

Weight of HCl in 1L soln, w = Normality of HCl x Eqvt wt of HCl = N2 x 36.5 = ……..x 36.5 = ….g

Weight of HCl in 500ml soln = w/2 =……….g

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Expt. No: 3
Date:
ESTIMATION OF HYDROCHLORIC ACID

AIM:
(1)To determine the Normality of the given HC1 solution using a standard solution of NaOH
containing 4 g of NaOH per liter.
(2)To calculate the amount of HC1 present in 500 ml of the solution.

APPARATUS REQUIRED:
50 ml burette, 20 ml pipette, 250 ml conical flask etc.

PRINCIPLE:
Standardisation of HCl is based on the neutralization of HCl by NaOH solution.
HCl + NaOH → NaCl + H2O.
A known volume of standard NaOH solution is titrated against HC1 using phenolphthalein as
indicator. Since we know the volume and normality of NaOH and the volume of HCl required
neutralizing the NaOH, the normality of HCl can be calculated.

PROCEDURE:
A burette is washed with water and rinsed with the given HCl solution. The burette is filled
with the HC1 solution, the tap is opened and the nozzle of the burette also is filled with the acid. After
air bubbles have escaped, the level of the acid is brought to the zero mark and te reading of the burette
is noted Clamped the burette in the burette stand. A pipette is washed with water and rinsed with the
NaOH solution. Pipetted out 20 ml of NaOH solution into a clean conical flask. Added one or two
drops of phenolphthalein to the solution in the conical flask. The solution turned pink. Hydrochloric
acid from the burette is added to the NaOH solution in the conical flask, little by little. Meanwhile the
flask is kept gently shaking. The addition of the acid is stopped when the pink colour is just
discharged. This is the end point of the titration. The final reading of the burette is noted and the
titration is repeated to get concordant values.

RESULT:

1. Normality of the given HCl solution =......................................................... N

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2. Weight of HCl in 500 ml of the solution =.................................................. g

OBSERVATION:

Std Na2CO3 Vs H2SO4 (Methyl orange)

Trail BURETTE READING( in ml) VOLUME H2SO4 USED

No: (in ml)
INITIAL FINAL

Titre Value =…………………..ml

CALCULATION:

N1V1=N2V2

N1= Normality Na2CO3 of solution= (Wt per liter) / (Eqvt wt) =5.6/53= 0.1056N

V1= Vol of Na2CO3 soln = 20ml

V2= Vol of H2SO4 soln = ……….ml

N2= Normality of H2SO4solution= (N1V1) / V2 = (0.1056N x 20) / (………) =………... N

Normality = (Wt per liter) / (Eqvt wt)

(Wt per liter) = Normality x Eqvt wt

Weight of H2SO4 in 1L soln, w = Normality of H2SO4 x Eqvt wt of H2SO4 = N2 x 49 = …..x 49 = ---.g

Weight of H2SO4 in 250ml soln = w/4 =……….g

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Expt. No: 04
Date:
ESTIMATION OF H2SO4
AIM:
(1)To determine the normality of the given sulphuric acid solution using standard solution of
Na2CO3 containing 5.6 g per liter.
(2) To calculate the weight of H2 SO4 in 250 ml of the solution.

PRINCIPLE:
The experiment is based on the neutralization of H2SO4 with Na2CO3.
Na2CO3 + H2SO4 →4 Na2SO4 + H2O + CO2.
A definite volume of the standard sodium carbonate solution is titrated against the H 2SO4
solution using methyl orange indicator. Methyl orange is golden yellow in alkali solution and orange
red in acid solution. From the titer value, then normality of the H2 SO4 solution and the weight of
H2SO4 per liter can be calculated knowing that the equivalent weight of H2SO4 is 49.

PROCEDURE:
A pipette is washed with water and rinsed with the given Na2CO3 solution. 20 ml of the
Na2CO3 solution is pipetted out into a clean conical flask. One or two drops of methyl orange
indicator are added to the solution so as to impart to it a golden yellow color. A burette is washed with
water and rinsed with the H2SO4 solution and filled with it. After air bubbles have escaped, the level
of the acid is brought to the zero mark and the reading of the burette is noted. The solution in the
conical flask is titrated against H2SO4 taken in the burette. The addition of the acid is stopped when
the golden yellow color just changes to orange red. The Titration is repeated till concordant values are
obtained. From the titer value, the normality and weight of H2SO4 per liter can be calculated.

RESULT:

1. Normality of the H2SO4 solution = ....................................N

2. Weight of H2SO4 in 250 ml of the solution = ………………..g

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OBSERVATION 1:
Std Na2CO3 Vs H2SO4 (Methyl orange)

Trail BURETTE READING( in ml) VOLUME H2SO4 USED

No: (in ml)
INITIAL FINAL

Titer Value =…………………..ml

CALCULATION:

N1V1=N2V2
N1= Normality Na2CO3 of solution= (Wt per litre) / (Eqvt wt) =5.4/53= 0.1018N
V1= Vol of Na2CO3 soln = 20ml
V2= Vol of H2SO4 soln = ……….ml
N2= Normality of H2SO4solution= (N1V1) / V2 = (0.1018N x 20) / (………) =…. N

OBSERVATION 2:

Std H2SO4 Vs NaOH (Phenolphthalein)

Trail BURETTE READING( in ml) VOLUME H2SO4 USED

No: (in ml)
INITIAL FINAL

Titre Value =…………………..ml

CALCULATION:

N1V1=N2V2
N1= Normality of H2SO4solution……….N
V1= Vol of H2SO4 soln = ……….ml
V2= Vol of NaOH soln = 20ml
N2= Normality of NaOH solution = (N1V1) / V2 = (…….N x ----) / (20) =…. N
Normality = (Wt per liter) / (Eqvt wt)

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Weight of NaOH in 1L soln, w = Normality of NaOH x Eqvt wt of NaOH = ……..x 40 = ………….g

Weightt of NaOH in 250ml soln = w/4 =……….g

Expt. No: 05
Date:
ESTIMATION OF NaOH

AIM:
(1)To determine mine the normality of the given NaOH solution using a standard solution of
Na2CO3 containing 5.4 g per liter of solution and a link solution of H2SO4.
(2) To calculate the amount of NaOH present in 250 ml of solution.

PRINCIPLE:
The experiment involves double titration. First titration is standardization of the link solution
H2SO4 using a, standard solution of Na2CO3.
Na2CO3 + H2SO 4 → Na2SO4 + H2O + CO2.
The second titration involves estimation of NaOH using standard H2SO4. It is based on the
neutralization of the acid with NaOH.
2 NaOH + H2SO4 → Na2SO4 + 2H2O

PROCEDURE:
(A) Standardisation of sulphuric acid: A burette is washed with water and rinsed with the
given H2SO4 solution. It is filled with the given H2SO4 solution, the level of the acid is brought to the
zero mark and the reading of the burette is noted. 20 ml of the Na2CO3 solution is transferred into a
clean conical flask after rinsing a clean pipette with the alkali solution. One or two drops of methyl
orange indicator are added to the solution in the conical flask. It is then titrated against the H2SO4
solution till golden yellow color of the solution is changed to orange red. The final reading of the
burette is noted. The titration is repeated to get concordant values. From the titer value, the normality
of H2SO4 can be calculated.
(B) Estimation of NaOH: A pipette is washed with water and rinsed with the given NaOH
solution. 20 ml of NaOH solution is pipetted out into a clean conical flask. One or two drops of
phenolphthalein indicator are added to the solution in the conical flask so as to get a pink colour to it.
It is then titrated against H2SO4 solution taken in the burette. The end point is the disappearance of
pink colour. The titration is repeated to get concordant values. From the titre value, the normality and
weight per liter of NaOH can be calculated.

RESULT:

1. Normality of the NaOH solution =.................................... N

2. Weight of NaOH in 250 ml of the solution = ......................... g

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OBSERVATION 1:

Std Oxalic acid Vs NaOH (Phenolpthalein)

BURETTE READING( in ml) VOLUME OXALIC

Trail
ACID USED
No:
INITIAL FINAL (in ml)

Titre Value =…………………..ml

CALCULATION:

N1V1=N2V2
N1= Normality Oxalic Acid of solution= (Wt per liter) / ( Eqvt wt) =6.2/63= 0.0984N
V1= Vol of Oxalic Acid soln = ………ml
V2= Vol of NaOH soln =20ml
N2= Normality of NaOH solution= (N1V1) / V2 = (……. x ……..) / (20) =… … N

OBSERVATION 2:

Std NaOH Vs HNO3 (Phenolpthalein)

Trail BURETTE READING( in ml) VOLUME HNO3 USED

No: (in ml)
INITIAL FINAL

Titre Value =…………………..ml

CALCULATION:

N1V1=N2V2
N1= Normality of NaOHsolution ……….N
V1= Vol of NaOH soln = 20ml

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V2= Vol of HNO3 soln = ………ml

N2= Normality of HNO3 solution = (N1V1) / V2 = (…….N x 20) / (………) =…. N
Normality = (Wt per liter) / (Eqvt wt)
Weight of HNO3 in 1L soln, w = Normality of HNO3 x Eqvt wt of HNO3 = ……..x63 = ………….g
Weight of NaOH in 250ml soln = w/4 =……….g

Expt. No: 06
Date:
ESTIMATION OF HNO3
AIM:
(1)To determine the strength of the given HNO3 solution using a standard solution of oxalic
acid containing 6.2 g of crystalline oxalic acidl in one liter of solution and a link solution of
NaOH.
(2)To calculate the amount of HNO3 present in 250 ml of the given solution.

PRINCIPLE:
This experiment involves double titration. First sodium hydroxide solution is standardized
using the standard solution of oxalic acid.
H2C2O4 + 2NaOH → Na2C2O4 + 2H2O
The second titration involves the estimation of HNO3 using the standardized NaOH.
HNO3 + NaOH → NaNO3 + H2O

PROCEDURE:
1. Standardization of NaOH: A burette is washed with water and rinsed with the given
standard solution of oxalic acid. The initial reading of the burette is noted. A pipette is washed with
water and rinsed with the given NaOH solution. 20 ml of the NaOH solution is pipette out into a clean
conical flask. One or two drops of phenolphthalein indicator is added to the NaOH solution and
titrated against oxalic acid from the burette, till the pink color of the solution is just disappeared. The
titration is repeated to get concordant values.

2. Estimation of HNO3: A burette is washed with water and rinsed with the given HNO3
solution. It is filled with HNO3 solution, the level of the acid is brought to the zero mark and the
reading of the burette is noted. 20 ml of the NaOH solution is transferred into a clean conical flask
after rinsing a clean pipette with the alkali solution. One or two drops of phenolphthalein indicator are
added to the solution in the conical flask. It is then titrated against the HNO3 solution till pink color of
the solution is just disappeared. The final reading of the burette is noted. The titration is repeated to
get the concordant values. From the titer value, the normality of HNO3 can be calculated.

RESULT:

1. Normality of the given HNO3 solution =..................... N

2. Weight of HNO3 solution in 250 ml of the solution = .............................. g

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OBSERVATION 1:-

K2CO3 X HCl (methyl orange)

Sl no Volume of potassium Burette reading Volume of HCl

carbonate solution pipetted solution used (ml)
in ml Innitial Final

Volume of HCl used , Va =---------ml

CALCULATION:-

Mass of potassium carbonate in 500 ml = 3.45 g

Volume of potassium carbonate solution, Vb = 20 ml
Equivalent mass of potassium carbonate = 69
Normality of potassium carbonate solution, Nb = Weight in g/l
Equivalent weight
Normality of HCl = Na
At the end point Na Va = Nb Vb
Na = Nb Vb = 20 X Nb
va Va
= ---------------- N
Normality of Hydrochloric acid, Na = ----------------- N

OBSERVATION 2 :-

KOH X HCl ( Phenolphthalein )

Sl no Volume of potassium Burette reading Volume of HCl

hydroxide solution pipetted solution used (ml)
in ml Innitial Final

Volume of HCl used , V a = -----------ml

CALCULATION:-
Normality of hydrochloric acid, Na = --------------------- N
Volume of hydrochloric acid , Va =------------------------ ml
Volume of KOH solution, V b = 20ml
Normality of KOH solution = Nb
At the end point, Na Va = Nb Vb
Nb = Va Na
Vb
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Equivalent weight of KOH = 56

Weight of KOH in 1L of the solution = -----x56 = ----------g
Weight of KOH in 500 ml of the solution = Weight in L = --------g
2

Expt. No: 07
Date:
ESTIMATION OF POTTASSIUM HYDROXIDE

AIM:

Estimate the weight of potassium hydroxide in 500 ml of the given solution. You are provided
with potassium carbonate solution containing 3.45g per 500 ml and approximately decinormal
solution of hydrochloric acid.

PRINCIPLE:

Since both potassium hydroxide solution and potassium carbonate solution are basic in nature,
solution of hydrochloric acid is used as link solution.

KOH + HCl KCl +H2O

K2CO3 + 2HCl 2KCl + CO2 +H2O

PROCEDURE:

A. Standardisation of Hydrochloric acid:-

20 ml of potassium carbonate solution is pipetted out into a clean conical flask. A drop of
methyl orange indicator is added when the solution is turned yellow in colour. The solution is
titrated against hydrochloric acid taken in a burette. The endpoint is the change of yellow
colour to pink. The titration is repeated to get concordant values.

B.Estimation of potassium hydroxide

20 ml potassium hydroxide solution is pipette out into a clean conical flask. A drop of
phenolphthalein indicator is added and the solution will turn into pink colour. This solution is
titrated against hydrochloric acid taken in the burette. The end point is the decolourisation of
pink colour. The titration is repeated to get concordant values.

RESULT:-
1. Normality of hydrochloric acid = ------------------N
2. Weight of potassium hydroxide in 500 ml = --------g

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OBSERVATION 1:-

KOH X HNO3 ( Phenolphthalein )

Sl no Volume of potassium Burette reading Volume of

hydroxide solution pipetted HNO3solution used
in ml Innitial Final (ml)

Volume of HNO3 used, Va = -----------ml

CALCULATION:-
Normality of nitric acid, =Na
Volume of nitric acid , Va =------------------------ ml
Volume of KOH solution, V b = 20ml
Normality of KOH solution = Nb = 0.1 N
At the end point, Na Va = Nb Vb
Na = Vb Nb
Va
¶ = 20X 0.1
-----
Normality of nitric acaid, Na= -------N

OBSERVATION 2:-

Na2CO3 X HNO3 ( methyl oramge)

Sl no Volume of Na2CO3 solution Burette reading Volume of HNO3

pipetted in ml solution used (ml)
Innitial Final

Volume of HNO3 used, Va = ----------------ml

CALCULATIONS:-

Normality of nitric acid, Na = ---------N

Volume of nitric acid, Va = ---------ml
Volume of sodium carbonate, Vb = 20 ml
Normality of sodium carbonate = Nb
At the end point, Na Va = Nb Vb
Nb = Va Na
Vb
Normality of sodium carbonate solution , Nb = ------- N
Equivalent weight of sodium carbonate = 53
Weight of sodium carbonate in the whole of the given solution = ------------ X 53 = -----------g
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Expt. No: 8
Date:
ESTIMATION OF SODIUM CARBONATE

AIM:

Estimate the weight of sodium carbonate in the whole of the given solution. You are provided with
decinormal solution potassium hydroxide and approximately decinormal nitric acid solution.

PRINCIPLE:

Since both sodium carbonate solution and potassium hydroxide solution are basic in nature .
the given nitric acid solution is taken as link solution.

KOH +HNO3 KNO3 +H2O

Na2CO3 +2 HNO3 2 Na2CO3 +CO2 +H 2O

Using standard potassium hydroxide solution given nitric acid is standardised. Using this
standard nitric acid solution, sodium carbonate is estimated.

PROCEDURE:

A. Standardisation of nitric acid:-

20ml of potassium hydroxide solution iis pipette outbinto a clean conical flask. A drop of
phenolphthalein is bis added and a npink colour is produced. It is then titrated against nitric
acid solution taken in the burette. The end point is decolourisation of pink colour. The titration
is repeated to get concordant values.

B.Estimattion of Sodium carbonate:-

The given sodium carbonate solution is made upto 100 ml in a standard measuring flask.
20 ml of the made up solution of sodium carbonate is piptted out into a clean conical flask. A
drop of methyl orange is added and the solution turns yellow in colour. It is then titrated
against nitric acid solution taken in the burette. The endpoint is the change of colour from
yreloow to pink. The titration is repeated to get concordant values.

RESULT:-
1. Normality sodium carbonate solution = ........N
2. Weight of sodium carbonate in the whole of thye given solution =-----g

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OBSERVATION 1:-

NaOH X H2SO4 ( Phenolphthalein )

Sl no Volume of sodium hydroxide Burette reading Volume of H2SO4

solution pipetted in ml solution used (ml)
Innitial Final

Volume of H2SO4 used , Va = -----------ml

CALCULATION:-

Normality of sulphuric acid, =Na

Volume o f sulphuric acid , Va =------------------------ ml
Volume of NaOH solution, V b = 20ml
Normality of NaOH solution = Nb = 0.1 N
At the end point, Na Va = Nb Vb
Na = Vb Nb
Va
= 20X 0.1

Normality of nitric acaid, Na = -------N

OBSERVATION 2:-

K2CO3 X H2SO4 ( methyl oramge)

Sl no Volume of K2CO3 solution Burette reading Volume of H2SO4

pipetted in ml solution used (ml)
Innitial Final

Volume of H2SO4 used, Va = ----------------ml

CALCULATIONS:-

Normality of sulphuric acid, Na = ---------N

Volume of nitric acid, Va = ---------ml
Volume of pottassium carbonate, Vb = 20 ml
Normality of pottassium carbonate = Nb
At the end point, Na Va = Nb Vb
Nb = Va Na
Vb
Normality of pottassium carbonate solution , Nb = ------- N
Equivalent weight of pottassium carbonate = 69
Weight of pottassium carbonate in the whole of the given solution = ------------ X 69 = ---------g

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Expt. No: 9
Date:
ESTIMATION OF POTASSIUM CARBONATE

AIM:

Estimate the weight of potassium carbonate in the whole of the given solution. You are provided with
0.1 sodium hydroxide solution and approximately decinormal solution of sulphuric acid.

PRINCIPLE:

Since both potassium carbonate solution to be estimated and the standard solution of sodium
hydroxide are basic, a link solution of sulphuric acid is to be used.

K2CO3 + H2SO4 K2SO4 +CO2 +H2O

2 NaOH + H2SO4 Na2SO4 + 2H2O

Equivalent mass of H2SO4 = 49

Equivalent mass of K2CO3 = 69

PROCEDURE:

A. Standardisation of sulphuric acid:-

20 ml of sodium hydroxide is pipette out into a clean conical flask and titrated against sulphuric
acid taken in the burette using phenolphthalein as indicator which gives a pink colour to the
solution. The end point is the change of colour frompink to colourless. The titration is repeated
to get concordant values.
B. Estimation of potassium carbonate:-
The given solution of potassium carbonate is made upto 100 ml in a standard measuring flask.
20 ml of this potassium carbonate solution is pipette out into a clean conical flask and a adrop of
methyl orange is added which gives a yellow colour to the solution. The solution is titrated
against sulphuric acid taken in the buette. The end point is change of colour from yellow to red.
The titration is repeated to get concordant values.

RESULT:-

1. Normality of H2SO4 solution =--------N

2. Weight of K2CO3 in whole of the given solution = -----------g

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 ENGINEERING CHEMISTRY LAB

OBSERVATION 1:-

NaOH X H2SO4 ( Phenolphthalein )

Sl Volume of sodium Burette reading Volume of H2SO4

no hydroxide solution pipetted Innitial Final solution used (ml)
in ml

Volume of H2SO4 used , Va = -----------ml

CALCULATION:-
Mass of H2SO4 in 250 ml solution = 5.2g
Equivalent weight of sulphuric acid = 49

Normality of sulphuric acid,Na = 5.2/49 = ………N

Volume of sulphuric acid solution,Va = …….ml

Volume of sodium hydroxide solution,Vb = 20ml
Normality of sodium hydroxide solution = Nb
At the end point,
Va.Na=Vb.Nb
Nb = Va Na =………..N
Vb
OBSERVATION 2:-
NaOH X H2C2O4. 2H2O ( Phenolphthalein )

Sl Volume of K2CO3 Burette reading Volume of H2SO4

no solution pipetted in ml Innitial Final solution used (ml)

Volume of oxalic acid used, Va = ----------------ml

CALCULATIONS:-

Volume of oxalic acid, Va = ---------ml

Volume of NaoH solution,VB = 20ml

Normality of NaOH solution,Nb=……..N
Normality of oxalic acid solution = Na
At the end point,
Va.Na =Vb.Nb ie, Na = Vb Nb =………..N
Va

Equivalent weight of oxalic acid = 63

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 ENGINEERING CHEMISTRY LAB

Weight of oxalic acid in whole of given solution(100ml) = …………N X 63

=…………g

Expt. No: 10
Date:
ESTIMATION OF OXALIC ACID

AIM:

Estimate the weight of oxalic acid in the whole of the given solution. You are provided with
sulphuric acid solution containing 5.2 g of acid per litter and approximately decinormal solution of
sodium hydroxide

PRINCIPLE :

The estimation is based on the neutralization reaction between oxalic acid and sodium hydroxide
and between sodium hydroxide and sulphuric acid, .Sodium hydroxide act as link solution

2NaOH + H2SO4 Na2SO4 + 2H2O

2 NaOH + H2C2O4 Na2 c2o4 + 2H2O

Equivalent mass of H2SO4 = 49

Equivalent mass of H2C2O4. 2H2O = 63

PROCEDURE:

A. Standardisation of sodium hydroxide:-

20 ml of sodium hydroxide is pipette out into a clean conical flask and titrated against sulphuric
acid taken in the burette using phenolphthalein as indicator which gives a pink colour to the
solution. The end point is the change of colour from pink to colourless. The titration is repeated
to get concordant values.
B. Estimation of oxalic acid:-
The given solution of oxalic acid is made up to 100 ml in a standard measuring flask.
20 ml of sodium hydroxide solution is pipette out into a clean conical flask and a drop of
phenolphthalein is added which gives a pink colour to the solution. The solution is titrated
against oxalic acid taken in the burette. The end point is change of colour from pink to
colourless. The titration is repeated to get concordant values.

RESULT:-

1.Normality of sodium hydroxide solution =--------N

2. Weight of oxalic acid in whole of the given solution = -----------g

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 ENGINEERING CHEMISTRY LAB

OBSERVATION

oxalic acid X KMnO4 (KMnO4 act as self indicator)

Sl no Volume of oxalic acid Burette reading Volume of KMnO4
solution pipetted in ml solution used (ml)
Initial Final

Volume of KMnO4 used = -------------- ml

CALCULATIONS:

Normality of oxalic acid solution =0.1 N

Volume of oxalic acid solution = 20 ml

Volume of KMnO4 used = --------- ml

Normality of KMnO4 = N KMnO4

V oxalic acid X N oxalic acid = V KMnO4 X N KMnO4

N KMnO4 = V oxalic acid X N oxalic acid

V KMnO4

=…………………N

Equivalent mass of KMnO4 = 31.6

Weight of potassium permanganate in one litter of the solution = N KMnO4 X 31.6

= ------------ g

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 ENGINEERING CHEMISTRY LAB

Expt. No: 11
Date:

STANDARDISATION OF POTASSIUM PERMANGANATE

AIM:
Standardise and estimate the amount of potassium permanganate in one litter of the solution.
You are provided with decinormal solution of oxalic acid.

PRINCIPLE:
Estimation is based on the reaction between potassium permanganate and oxalic acid.

2KMnO4 + 3H2SO4 K2SO4 +2MnSO4 +3H2O+ 5(O)

H2C2O4 + (O) H2O + 2CO2

Equivalent mass of KMnO4 = 31.6

Equivalent mass of oxalic acid = 63

PROCEDURE:
20ml of oxalic acid solution is pipetted out into a clean conical flask. 20ml of dilute sulphuric
acid is added to it. This mixture is heated at a temperature 600C to 700C. This hot solution is titrated
against potassium permanganate taken in the burette. The endpoint is the appearance of permanent
pale pink colour in the solution. The titration is repeated to get concordant values.

RESULT:

1. Normality of KMnO4 solution = ----------------N

2. Weight of KMnO4 in one litter of the solution= ---------------g

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 ENGINEERING CHEMISTRY LAB

OBSERVATION : 1

std oxalic acid X KMnO4 (KMnO4 act as self indicator)

Sl no Volume of oxalic acid Burette reading Volume of KMnO4
solution pipetted in ml solution used (ml)
Initial Final

Volume of KMnO4 used = -------------- ml

CALCULATIONS:

Normality of oxalic acid solution = 6.3/63 = 0.1 N

Volume of oxalic acid solution = 20 ml

Volume of KMnO4 used = --------- ml

Normality of KMnO4 = N KMnO4

V oxalic acid X N oxalic acid = V KMnO4 X N KMnO4

N KMnO4 = V oxalic acid X N oxalic acid

V KMnO4

=…………………N

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 ENGINEERING CHEMISTRY LAB

Expt. No: 12

Date:
ESTIMATION OF MOHR’S SALT

AIM:

Estimate the amount of Mohr’s salt in one litter of the solution. You are provided with
oxalic acid solution containing 6.3g oxalic acid in one litter and approximately decinormal potassium
permanganate solution.

PRINCIPLE:

Estimation is based on the reaction between potassium permanganate and oxalic acid and
that of Mohr’s salt and potassium permanganate solution . Both reactions are conducted in acid
medium.

1. 2KMnO4 + 3H2SO4 K2SO4 +2MnSO4 +3H2O+ 5(O)

H2C2O4 + (O) H2O + 2CO2

2. 2KMnO4 + 3H2SO4 K2SO4 +2MnSO4 +3H2O+ 5(O)

2FeSO4 + H2SO4 + (O) Fe2(SO4 )3 H2O

Equivalent mass of Mohr’s salt = 392

Equivalent mass of oxalic acid = 63

PROCEDURE:

A. Standardisation of potassium permanganate solution

20ml of oxalic acid solution is pipetted out into a clean conical flask. 20ml of dilute sulphuric acid is
added to it. This mixture is heated at a temperature 600C to 700C. This hot solution is titrated against
potassium permanganate taken in the burette. The endpoint is the appearance of permanent pale pink
colour in the solution. The titration is repeated to get concordant values.

B. Estimation of Mohr’salt solution

The given Mohr’s salt solution is made up to 100 ml in a standard flask. During making up of
solution 10ml of dilute sulphuric acid is added to avoid hydrolysis of Mohr;s salt.

20ml of made up solution is pipetted out into a clean conical flask and 20ml of dilute sulphuric acid
is added to it. This mixture, while cold is titrated against potassium permanganate taken in the
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 ENGINEERING CHEMISTRY LAB

OBSERVATION :2

Mohr’s salt X std KMnO4 (KMnO4 act as self indicator)

Sl no Volume of Mohr;s salt Burette reading Volume of KMnO4
solution pipetted in ml solution used (ml)
Initial Final

Volume of KMnO4 used = -------------- ml

Normality of KMnO4solution =………….. N

Volume of KMnO4 used = --------- ml

Volume of Mohr;s salt solution = 20 ml

Normality of Mohr;s salt = N Mohr;s salt

V Mohr;s salt X N Mohr;s salt = V KMnO4 X N KMnO4

N Mohr;s salt = V KMnO4 X N KMnO4

V Mohr;s salt

=…………N

Equivalent mass of Mohr’s salt = 392

Weight of Mohr’s salt in one litter of the solution = N Mohr;s salt X 392

= ------------ g

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 ENGINEERING CHEMISTRY LAB

burette. The endpoint is the appearance of permanent pale pink colour in the solution. The titration is
repeated to get concordant values.

RESULT:-
3. Normality of hydrochloric acid = ------------------N
4. Weight of potassium hydroxide in 500 ml = --------g

MA’DIN POLYTECHNIC COLLEGE 30

OBSERVATION 1:-

Mohr salt X KMNO4

Sl Volume of Mohr Burette reading Volume of KMNO4

no saltsolution pipetted in ml Innitial Final solution used (ml)

Volume of KMNO used , Va = -----------ml

CALCULATION:-
Mass of Mohr salt in 100 ml solution = 3.92g
Equivalent weight of Mohr salt = 392

Normality of Mohr salt solution, N2 = Mass X1000 /Equivalent mass X volume

Volume of Mohr salt solution solution,V2 = 20 ml

Volume of KMNO4 solution,V1 = 20ml
Normality of KMNO4 solution = N1
At the end point,
V1N1=V2.N2
N1 = Va2N2 =………..N
V1
OBSERVATION 2:-
Oxallic acid X KMNO4

Sl Volume of oxalic Burette reading Volume of

no acidsolution pipetted in Innitial Final KMNO4 solution
ml used (ml)

Volume of KMNO4 used, Va = ----------------ml

CALCULATIONS:-

Normality of KMNO4 = N3=N1)=

Volume of KMNO4 solution,V3 = ----ml

Volume of oxalic acid solution,V4=20.ml
Normality of oxalic acid solution = N4
At the end point,
V3.N3 =V4.N4 ie, N4 = V3 N3 =………..N
V4

Equivalent weight of oxalic acid = 63

Weight of oxalic acid in whole of given solution(1000ml) = …………N X 63
=…………g
Weight of oxalic acid in 100 ml of given solution = W/10
 Expt. No: 13

Date:
ESTIMATION OF OXALIC ACID

AIM:

Estimate the amount of oxalic acid of hydrated oxalic acid, H2C2O4 .2H2O in the whole of the given
solution . You are provided with a solution of Mohrs salt FeSO4(NH4)2SO4.6H2O containing 3.92 g
of Mohrs asalt in 100 ml of the solution and approximately decinormal potassium permanganate
solution.

PRINCIPLE :

The estimation is based on the reactin between Ferrous sulphate present in MOhrs salt and potassium
permanganate solution.

2KMNO4 +3H2SO4 K2SO4 +2MnSO4 +3H2O+5[O]

2 FeSO4+H2SO4+[o] Fe2(SO4)3 + H2O

Since two molecular masses of Ferrous sulphate react with two equibalent masses of oxygen, the
equivalent mass of Ferrous sulphate ( FeSO4 7H2O) = molecular mass of FeSO47H2O=278

PROCEDURE:

A. Standardisation of potassium permanagnate:-

20 ml of standard Mohrs salt solution is pipette out into a clean conical flask. About 20 ml of
dilute sulphuric acid is added and this solution while cold is titrated against potassium
permanagante solution taken in the burette. The end point is the appearance of permanent pale
pink colour. The titration is repeated till concordant values are obtained.
B. Estimation of oxalic acid:-
20 ml of sodium hydroxide solution is pipetted out into clean conical flask . 20 ml of dilute
sulphuric acid is added to it and the mixture is heated to bearable warmth. The hot solution is
then titrated against potassium permanagante solution taken in the burette.The endpoint is the
appearance of permanent pale pink colour in the solution.The titration is repeated for concordant
values.

RESULT:-

1.Normality of KMNO4 solution =--------N

2. Weight of oxalic acid in whole of the given solution = -----------g

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Mohr’s salt X KMnO4 (KMnO4 act as self indicator)
Sl no ` Burette reading Volume of KMnO4
solution used (ml)
Initial Final

Volume of KMnO4 used,V1 = -------------- ml

CALCULATION

Mass of Mohr,s salt in 500 ml =19.6g

Equivalent mass of Mohr,s salt solution =392

Normality of Mohr,s salt solution,N2= MASS X1000

Equivalent mass Xvolume in ml

Volume of Mohr;s salt solution,V2 = 20 ml

Volume of potassium permanganate solution,V1=…….ml

Normality of KMnO4 =N1

At the end point,

V 1 X N 1 = V 2 X N2

N2XV2

V1

=…………………N

FeSO4X KMnO4 (KMnO4 act as self indicator)

Sl no ` Burette reading Volume of KMnO4

solution used (ml)
Initial Final

Volume of KMnO4 used,V3 = -------------- ml

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Expt. No: 14

Date:
ESTIMATION OF FERROUS IRON

AIM:

Estimate the amount of Ferrous Iron in whole of given ferrous sulphate solution. You are
provided with solution of mohr,s solution containing 19.6 g mohr,s salt in 0.5 liter of solution and
approximately decinormal potassium permanganate solution

PRINCIPLE:

Estimation is based on the reaction between ferrous sulphate and potassium permanganate
solution

2KMnO4 + 3H2SO4 K2SO4 +2MnSO4 +3H2O+ 5(O)

2FeSO4 + H2SO4 + (O) Fe2(SO4 )3 + H2O

Since two molecular masses of ferrous sulphste react with two equivalent masses of oxygen,the
equivalent mass of ferrous sulphat =278

The equivalent mass of ferrous iron=Atomic mass of iron=55.84

Mohr,s salt is a reducing agent due to the presence of ferrous sulphate in its molecule. Since
one molecular mass of Mohr,s salt contains one equivalent mass of ferrous sulphate,the
equivalent mass of Mohr s salt = molecular mass of Mohr,s salt =392
,

PROCEDURE:

A. Standardisation of potassium permanganate solution:- 20ml of standard Mohr,s salt solution

is pipetted out into a clean conical flask. 20ml of dilute sulphuric acid is added to it. While cold,
solution is titrated against potassium permanganate taken in the burette. The endpoint is the
appearance of permanent pale pink colour in the solution. The titration is repeated to get concordant
values.

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 CALCULATION

Normality of KMnO4 (N3 =N1)=………..N

Volume of potassium permanganate solution,V3=…….ml

Volume of ferrous sulphate solution =V4=20ml

Normality of of potassium permanganate solution=N4

At the end point,

V 3 X N 3 = V 4 X N4

N4 = N3XV3

V4

=…………N

The equivalent mass of ferrous iron= 55.84

Mass of ferrous iron in whole of given solution(100ml) = N4 X55.84

10

=…………

=…………g

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B. Estimation of ferrous iron

The given ferrous sulphate solution is made up to 100 ml in a standard flask. During making up of
solution 10ml of dilute sulphuric acid is added to avoid hydrolysis of ferrous sulphate

20ml of made up solution is pipetted out into a clean conical flask and 20ml of dilute sulphuric
acid is added to it and titrated against potassium permangantetaken in burette. The endpoint is the
appearance of permanent pale pink colour in the solution. The titration is repeated to get concordant
values.

RESULT:-
1. Normality of KMnO4 solution = ------------------N
2. Mass of ferrous iron in the whole of the given solution = --------g

MA’DIN POLYTECHNIC COLLEGE 36

OBSERVATION 1:-

ZnSO4X EDTA ( Eriochrome black T )

Sl Volume ZnSO4 solution Burette reading Volume EDTA

no pipetted in ml Innitial Final solution used (ml)

Volume of EDTA used , V1= -----------ml

CALCULATION:-
Mass of ZnSO4 .7 H2O in 100 ml solution = 0.72 g
Molecular weight of ZnSO4.7H2O = 287.36

Molarity of Zinc Sulphate solution, M2= MassX 1000/ Molar massX volume =(0.72/287.36)
X(1000/100) = 0.0256 M

Volume of zinc sulphate solution,V2 = 20 ml

Volume of EDTA solution,V1 = 20ml
Molarity of EDTA solution = M1
At the end point,
V1.M1=V2.M2
M1 = Va Ma =………..M
V1
OBSERVATION 2:-
ZnSO4 X EDTA ( Eriochrome Black T )

Sl Volume of ZnSO4solution Burette reading Volume of EDTA

no pipetted in ml Innitial Final solution used (ml)

Volume EDTA used, V3 = ----------------ml

CALCULATIONS:-

Molarity of EDTA v(M3=M1)= ---------M

Volume of Zn SO4 solution,V4 = 20ml

Molarity of ZnSO4 solution,M4=……..M4
At the end point,
V3.M3 =V4.M4 ie, M4 = V3 N3 =………..M
V4

Molar mass of zinc=65.34

Weight of zinc in whole of given solution(100ml) = …………M4 X 65.34/10
=…………g

MA’DIN POLYTECHNIC COLLEGE 37

Expt. No: 15 COMPLEXOMETRY
Date:
ESTIMATION OF ZINC

AIM:

Estimate the mass of zinc in the whole of the given solution of Zinc sulphate. You are provided with
0.025M EDTA and a solution of ZnSo4.7H2O containing 0.72 g of ZnSO4.7H2O in 100 ml.

PRINCIPLE :

Zn ions form complexes with EDTA(H2Y2-) which can be represented by the equation

Zn 2+ +H2Y2- Zn Y2- +2H+

The given EDTA solution is stamdardised using the standard ZnSO4 solution.The end point is
detected by using Eriochrome Black T indicator which has a blue colour in the Ph range between 7 to
11. The indicator react with Zn2+ ionto prosuce Zn-eriochrome black T indicator complex which has
a wine red colour.

PROCEDURE:

A. Standardisation of EDTA solution:-

20 ml of standard zinc sulphate solution is pipette into a clean conical flask and diluted to 100 ml
by adding distilled water. 2 ml of buffer solution (NH4Cl-NH4OH) of pH 10 and 3 to 4 drops of
Eriochrome black T indicator are added to it. The solutions are mixed and then titrated against
EDTA solution taken in the burette until the colour changes from wine red to blue which is the
endpoint. The titration is repeated till concordant values are obtained.
B. Estimation of Zinc:-

The given Zinc sulphate solution is made up to 100 ml in a standard measuring flask.
20 ml of made up solution is pipette out into a clean conical flask and diluted to 100 ml with
distilledwater. 2 ml of the buffer solution of pH 10 and 3 to 4 drops of eriochrome black t indicator
are added to it.titration is repeated until wine red colour changes to blue.

RESULT:-

1. Weight of zinc in whole of the given solution = -----------g

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