SRI SHANMUGHA COLLEGE OF ENGINEERING AND TECHNOLOGY

BS3171- CHEMISTRY LAB MANUAL

FOR FIRST YEAR B.E/B.TECH- DEGREE COURSES
(Common to all Branches)
REGULATION-2021

1
 ANNAUNIVERSITY REGULATON 2021

BS3171 CHEMISTRY LABORATORY

(Any seven experiments to be conducted)

LIST OF EXPERIMENTS

1. Preparation of Na2CO3 as a primary standard and estimation of acidity of a water sample using the
primary standard

2. Determination of types and amount of alkalinity in water sample. - Split the first experiment into two

3. Determination of total, temporary & permanent hardness of water by EDTA method.

4. Determination of DO content of water sample by Winkler’s method.

5. Determination of chloride content of water sample by Argentometric method.

6. Estimation of copper content of the given solution by Iodometry.

7. Estimation of TDS of a water sample by gravimetry.

8. Determination of strength of given hydrochloric acid using pH meter.

9. Determination of strength of acids in a mixture of acids using conductivity meter.

10. Conductometric titration of barium chloride against sodium sulphate (precipitation titration)

11. Estimation of iron content of the given solution using potentiometer.

12. Estimation of sodium /potassium present in water using flame photometer.

13. Preparation of nanoparticles (TiO2/ZnO/CuO) by Sol-Gel method.

14. Estimation of Nickel in steel

15. Proximate analysis of Coal

TOTAL: 30 PERIODS

2
 CONTENTS

S.No. DATE EXPERIMENT MARKS SIGNATURE

3
EXPERIMENTS

4
5
 1. DETERMINATION OF TOTAL, TEMPORARY & PERMANENT
HARDNESS OF WATER BY EDTA METHOD
Aim

To estimate the amount of total hardness, permanent hardness and temporary hardness
present in the given sample of water by EDTA method.

Chemicals Required

 Standard Hard water

 Sample water
 EDTA
 Ammonia Buffer
 Eriochrome Black-T (EBT)

Principle

Disodium salt of Ethylene Diamine Tetra Acetic acid (EDTA) is a well known
Complexing agent. Its structure is shown in the figure 1.
Disodium salt of EDTA is used to estimate the various hardness of the given water
containing the Ca2+and Mg2+ ions. When the EDTA is added to hard water, it reacts with
calcium and magnesium ions present in water to form stable EDTA metal complexes. From
the volume of EDTA consumed the hardness can be calculated. Eriochrome Black-T is used as
an indicator. The indicator forms a weak complex with the metal ions present in the water and
gives wine red colour.

6
TITRATION: I

STANDARDIZATION OF EDTA

Standard Hard water Vs EDTA

Volume of Burette Readings

Volume of Concordant
Standard
S.No. Initial Final EDTA Value Indicator
Hard water
(ml) (ml) (ml)
(ml)
1.

Eriochrome
2.
Black-T
(EBT)

3.

Calculation:
Volume of Standard hard water = 20 ml.

Volume of EDTA (V1) = ml.

1 ml of Standard hard water contains 1 mg of CaC03

20 ml of Standard hard water contains 20 mg of CaCO3.

20 ml of standard hard water consumes V1 ml of EDTA

i.e., V1 ml of EDTA solution = 20 mg of CaCO3

1 ml of EDTA solution = 20/V1 mg of CaCO3 equivalent.

Note:

 Hardness of water can be expressed in terms of calcium carbonate equivalents and in

mg/l or ppm unit
 ppm = parts per million and 1 mg/l = 1 ppm.

7
 When the EDTA is added into the hard water, the metal ion forms a stable metal
complex with EDTA by leaving the indicator. When all the metal ions are taken by EDTA from
the indicator metal ion complex, the wine red colour changes into steel blue, which denotes the
end point. The metal EDTA complex is stable at pH 8-10. This pH range can be maintained by
adding ammoniacal buffer (NH4Cl+NH4OH).
Temporary hardness can be removed by boiling the water and filtering the given hard
water sample. During boiling soluble bicarbonates are converted into insoluble carbonates.
Ca (HCO3)2  CaCO3 ↓+CO2 +H2O
Mg (HCO3)2  Mg CO3↓ +CO2 + H2O
The filtrate is collected in the conical flask,EBT indicator and buffer solution are
added.It is then titrated against the EDTA.

Temporary hardness = Total hardness - Permanent hardness

PROCEDURE

Titration-I: Standardization of EDTA

The burette is washed well with the distilled water and rinsed a little amount of the
given EDTA solution and filled with the same EDTA solution upto zero mark without any air
bubbles. 20 ml of standard hard water solution is pipetted out into a clean conical flask. 5 ml
of ammonia buffer solution and 2 drops of Eriochrome Black-T indicator are added. The
solution turns wine red in colour. The content of the conical flask is titrated against EDTA
solution taken in the burette. The end point is the change of colour from wine red to steel blue.
The volume of EDTA consumed is noted. The titration is repeated to obtain concordant values.

Let the volume of EDTA consumed be V1 ml

8
TITRATION-II

ESTIMATION OF TOTAL HARDNESS

Standardized EDTA Vs Hard Water sample

Volume of Volume of Concordant

Burette Readings
S.No. water sample EDTA Value Indicator
Initial Final
(ml) (ml)
(ml) (ml)
1.

Eriochrome
2.
Black-T
(EBT)
3.

Calculation
Volume of water sample = 20ml.

Volume of EDTA (V2) = ml.

20 ml of the water sample consume = V2 ml of EDTA

= V2× 1 ml of EDTA

= V2× 20 / V1 mg of CaCO3

1000 ml of the water sample contains = V2× 20/V1× 1000/20 mg of CaCO3

= V2/V1× 1000 ppm.

Total hardness of the water sample = ppm.

9
Titration-II: Estimation of Total hardness of water sample

The burette is re-filled upto zero mark without any air bubbles. 20 ml of the given
water sample is pipetted out into a clean conical flask. 5ml of ammonia buffer solution and 2
drops of EriochromeBlack –T indicator are added successively. The solution turns wine red in
colour. The content of the conical flask is titrated against EDTA solution taken in the burette.
The end point is the change of colour from wine red to steel blue. The volume of EDTA
consumed is noted. The titration is repeated to get concordant values.

Let the volume of EDTA consumed be V2 ml.

Titration-III: Estimation of Permanent hardness of water sample

100 ml of the given sample of water is taken in a clean 250 ml beaker and boiled for10-
15 minutes. It is then cooled and filtered. The filtrate is collected in a 100 ml standard flask.20
ml of this made up solution is pipetted out into a clean conical flask. 5 ml of ammonia buffer
solution and 2 drops of Eriochrome Black –T indicator are added. The solution turns wine red
in colour. The content of the conical flask is titrated against EDTA solution taken in the burette.
The end point is the change of colour from wine red to steel blue. The volume of EDTA
consumed is noted. The titration is repeated to get concordant values.

Let the volume of EDTA consumed be V3 ml.

Estimation of Temporary Hardness

Temporary hardness of the water sample is calculated by subtracting

permanent hardness from total hardness.

Temporary hardness = Total hardness - Permanent hardness

TITRATION-III

10
ESTIMATION OF PERMANENT HARDNESS

Standardized EDTA Vs Boiled Hard Water sample

Volume of
Boiled Burette Readings Volume of Concordant
S.No. Water EDTA Value Indicator
Initial Final
sample (ml)
(ml) (ml)
(ml)

1
Eriochrome
Black-T
2
(EBT)
3

Calculation:
Volume of boiled water sample = 20 ml.

Volume of EDTA (V3) = ml.

20 ml of the Boiled water sample consumes = V3 ml of EDTA

= V3× 1 ml of EDTA

= V3× 20/V1 mg of CaCO3

1000 ml of the water sample contains = V3× 20/V1× 1000/20 mg of CaCO3

= V3/V1× 1000 ppm.

Permanent hardness of the water sample = ppm.

Estimation of Temporary Hardness

Temporary hardness = Total hardness - Permanent hardness

= ppm

11
RESULT:

(i) Amount of Total hardness present in the given sample of water = ppm

(ii)Amount of Permanent hardness present in the given sample of water = ppm

(iii)Amount of Temporary hardness present in the given sample of water = ppm

12
Strength of HCl = -------------- N

The end point when phenolphthalein is used as an indicator = P

The end point when methyl orange is used as an indicator =M

Relationship
Nature of Amount of individual
in between OH- HCO3- CO32-
alkalinity alkalinities
P &M
P= M only OH- (P or M) x 0.1 x 50 xxx 0.0 0.0
20

2P = M only CO 32- (2P or M) x 0.1 x 50 0.0 0.0 xxx

20

P =0, M≠0 only HCO3- M x 0.1 x 50 0.0 xxx 0.0

20

2P > M OH- &CO 32- OH- = (2P - M) x 0.1 x 50

20
xxx 0.0 xxx
2-
CO3 = 2 (M-P) x 0.1 x 50
20

2P < M HCO3&CO 2- HCO3- = (M-2P) x 0.1 x 50

3
20
CO32- = (2P) x 0.1 x 50
20 0.0 xxx xxx

13
2. ESTIMATION OF HCl USING Na2CO3 AS PRIMARY STANDARD
AND DETERMINATION OF ALKALINITY IN WATER SAMPLE

AIM
To determine the type and amounts of alkalinity in the given water sample. A
standard solution of Na2CO3 of strength N is given.

CHEMICALS REQUIRED

 Hydrochloric acid
 Water sample
 Sodium Carbonate
 Phenolphthalein
 Methyl orange

PRINCIPLE
Alkalinity in water is due to the presence of soluble hydroxides, bicarbonates
and carbonates. Alkalinity can be determined by
 Potentiometric methods
 Using pH meter
 Titrimetry using different indicators
Determination of various types and amounts of alkalinity is easily carried out by
titration with standard HCl employing the indicators phenolphthalein and methyl
orange independently or in succession.
The following reactions occur when different types of alkalinity are neutralized
with acid.
OH- + H+  H2 O completed at PH 8.2-9.0 ------------(1)
CO32- + H+  HCO3 -------------------------------------------------------------------------------------------- (2)
HCO3- + H+  (H2CO3)  H2O + CO2 completed at PH 4.2-5.5--------- (3)
Neutralization (1) & (2) will be notified by phenolphthalein end-point while all
the three will be accounted by methyl orange end-point. Bicarbonate in equation (3)
may be due to the existence of soluble free bicarbonate salts or bicarbonates resulting
from half neutralization of soluble carbonates (eqn. (2).

14
TITRATION: 1
STANDARDISATION OF HCl
Standard Na2CO3 Vs HCl

Volume of
Volume of
Standard Burette Readings Concordant
S.No. HCl Indicator
Na2CO3 Initial Final value
(ml)
(ml) (ml) (ml)
1.
2. Methyl orange
3.

Calculation of strength of HCl:

Volume of Na2CO3 (V1) = 20 ml.

Strength of Na2CO3 (N1) = 0.1 N

Volume of HCl (V2) = ml.

Strength of HCl (N2) = ?

V1N1 = V2N2

N2 = V1 N1 / V2

= N

Strength of HCl = N

15
 Various steps to be followed:
a) A known volume of water sample is titrated against std. HCl using first
phenolphthalein indicator till end-point (P) and the titration is continued without
break using methyl orange indicator till the equivalence end-point (M).
b) It indicates that,
(i) 2P = M => Presence of only CO 32-

(ii) P =0, M#0 => Presence of only HCO3-

(iii) 2P > M => Presence of OH- & CO 32-

(iv) 2P < M => Presence of HCO3- & CO32-

(Mixture of OH- & HCO3-are not listed since they do not exist together and are
considered equivalent to CO32-).
PROCEDURE
TITRATION – I
STANDARDISATION OF HCl
Exactly 20 ml of the given standard Na2CO3 solution is pipetted out into a
clean conical flask and 2 drops of methyl orange indicator is added. The solution is
titrated against the given HCl taken in the burette. The yellow colour of the solution in
the conical flask changes into reddish orange at the end-point. The titre value is noted
down from the burette and the titration is repeated to get concordant value.
TITRATION – II
ESTIMATION OF ALKALINITY IN WATER SAMPLE
Exactly 20 ml of water sample is pipetted out into a clean conical flask. Few
drops of phenolphthalein indicator are added and titrated against the standardized HCl
taken in the burette. The end-point is the disappearance of pink colour, which is noted
as P. Into the same solution few drops of methyl orange indicator is added. The
solution changes to yellow. The titration is continued further by adding same HCl
without break till the end-point is reached. The end point is the colour change from
yellow to reddish orange. The titre value is noted as M.

16
TITRATION – II
ESTIMATION OF ALKALINITY IN WATER SAMPLE
Standard HCl Vs Water sample

S.No Volume of Volume of HCl

Indicator
. water (ml)
sample
For Phenolphthalein For Methyl Orange end
(ml)
end point(P) point(M) 1. Phenolphthalein
1
2. Methyl orange
2

If the date satisfies the condition P > 𝟏 M

𝟐

Calculation of OH- alkalinity:

Volume of HCl (V1) = 2P -M
= ml.
Strength of HCl (N1) = N.
Volume of water sample (V2) = 20 ml.
Strength of water sample due to OH-alkalinity (N2) = ?
V1N1 = V2N2
N2 = V1N1 / V2

= N.

Amount of OH- present in strength of water sample due to OH- X

1 liter of the given water sample = Equivalent weight of CaCO3 X 1000 ppm

Hydroxide alkalinity = ppm.

17
The experiment is repeated to get concordant values. From the magnitudes of P & M
values, the type of alkalinity present in the water sample is inferred and the individual
amounts are calculated and reported.

18
Calculation of Carbonate alkalinity: (CO32-)
Volume of HCl (V1) = 2 M – 2P

= ml.

Strength of HCl (N1) = N.

Volume of water sample (V2) = 20ml.

Strength of water sample due to CO32- alkalinity (N2) = ?

V1N1 = V2N2

N2 = V1N1 / V2

= N.

Amount of CO32- present in strength of water sample due to CO32- X

1 liter of the given water sample = Equivalen t we ight of C aCO3 X 1000 ppm

Carbonate alkalinity = ppm.

19
RESULT
(1) The type of alkalinity present in the water sample =
(2) The individual amounts of alkalinity present in the water sample
(i) Hydroxide alkalinity = ppm
(ii) Carbonate alkalinity = ppm.

20
TITRATION-I

STANDARDISATION OF SODIUM THIOSULPHATE SOLUTION

Std. Potassium dichromate solution Vs Sodium thiosulphate solution.

Volume of Burette Readings Volume of

Concordant
S.No. K2Cr2O7 Initial Final Na2S2O3 Indicator
value
(ml) (ml) (ml) (ml)

1.

2. starch

3.

Calculation:

Volume of potassium dichromate solution V1 = 20 ml.

Strength of potassium dichromate solution N1 = 0.01N

Volume of sodium thiosulphate solution V2 = ml.

Strength of sodium thiosulphate solution N2 =

V1N1 = V2N2

N2 = V1N1/ V2

= N.

Strength of Sodium thiosulphate solution = N

21
 3. DETERMINATION OF DO CONTENT OF WATER SAMPLE BY
WINKLER’S METHOD
AIM

To estimate the amount of dissolved oxygen present in the water sample by Winkler’s
method.

CHEMICALS REQUIRED

 Potassium dichromate
 Sodium thiosulphate
 Manganous sulphate
 Potassium iodide
 Starch
 Sodium hydroxide
 Sulphuric acid
PRINCIPLE:

Oxygen dissolved in water to the extent of 7-9 mgs/lit at a temperature range of 250
-350 C. The estimation of dissolved oxygen in water is useful in studying the corrosion effect
of boiler feed water and water pollution. The amount of dissolved oxygen in water is
estimated using Winkler’s reagent (Potassium bromide +Potassium bromate). Water sample
is collected carefully avoiding aeration/deaeration in ground stopperd flask. Initially
Manganous sulphate and alkali-iodide reagents are added and the reaction occur as follows
Mn2++2OH- → Mn (OH) 2 ↓ (white)
Mn (OH) 2 +1/2 O2 → MnO (OH) 2 ↓ (yellow brown)
The precipitate dissolves in concentrated sulphuric acid and the liberated iodine is titrated
against Na2S2O3
MnO (OH) 2+2H2SO4 →Mn(SO4)2 + 3H2O
Mn (SO4)2 + 2KI → MnSO4 + K2SO4 + I2
2 Na2S2O3 + I2 → Na2S4O6 + 2NaI

22
TITRATION-II

ESTIMATION OF DISSOLVED OXYGEN.

Std. Sodium thiosulphate solution Vs water sample.

S.No. Volume of Burette Readings Volume Concordant Indicator

water of value
sample (ml) Initial Final(ml) Na2S2O3
(ml) (ml)
1.
2. starch
3.

Calculation:

Volume of sodium thiosulphate solution V1 = ml.

Strength of sodium thiosulphate solution N1 = N

Volume of water sample V2 = 20 ml.

Strength of water sample N2 = ------

V1N1 = V2N2

N2 = V1N1/ V2

= N.

Amount of dissolved oxygen present in 1 litre = Normality of water sample X

of the water sample Equivalent weight of O2 X 1000

= ppm.

23
PROCEDURE:

Titration – I: Standardisation of sodium Thiosulphate solution.

The burette is washed and rinsed with sodium thiosulphate solution. Then the burette
is filled with the given sodium thiosulphate solution. 20ml of 0.01N Potassium dichromate
solution is pipetted out into a clean conical flask. To this 5ml of sulphuric acid and 15 ml of
5% potassium iodide are added. This is titrated against sodium thiosulphate solution. When the
solution become straw yellow in colour, starch indicator is added and then the titration is
continued. The end point is disappearance of blue colour and appearance of light green colour.
The titration is repeated to get the concordant value.

Titration – II: Estimation of dissolved oxygen.

100-150 ml of water sample is taken in a iodine flask, 2ml of manganese sulphate and
2ml of alkali-iodide are added. The stopper is replaced and the flask is inverted and shaked
several times for the rough mixing of reagents. The flask is left aside for some time. When half
of the precipitate is settles down, the stopper is removed and 2ml of conc. sulphuric acid is
added.
The stopper is replaced and the flask is kept inverted for several times for complete
dissolution of the precipitate. 100ml of this solution is pipetted out and titrated against standard
sodium thiosulphate solution. When the solution becomes light yellow starch indicator is added
.The titration is repeated until the blue colour is disappeared. From the titre value the strength
of dissolved oxygen is calculated and hence the amount of dissolved oxygen in the water
sample is calculated
The equivalent weight of oxygen is 8.

RESULT:

Amount of dissolved oxygen present in 1 litre of the water sample = ppm.

24
TITRATION –I

STANDARDISATION OF SILVER NITRATE SOLUTION

Std. NaCl Vs AgNO3

Volume of Burette Readings Volume of

standard AgNO3 Concordant
S.No. Initial Final Indicator
NaCl solution solution value
(ml) (ml)
(ml) (ml)
1.
2. K2CrO4
3.

Calculation:

Volume of sodium chloride solution (V1) = 20 ml.

Strength of sodium chloride solution (N1) = 0.01 N.

Volume of silver nitrate solution (V2) = ml.

Strength of silver nitrate solution (N2) =

V1N1 = V2N2

N2 = V1N1 / V2

Strength of silver nitrate solution = N.

25
 4. DETERMINATION OF CHLORIDE CONTENT OF WATER
SAMPLE BY ARGENTOMETRIC METHOD

AIM
To estimate the amount of chloride ion present in the given water sample being supplied
with standard solution of sodium chloride of strength 0.01 N and an approximately N/20
solution of silver nitrate.

CHEMICALS REQUIRED

 Sodium chloride
 Silver nitrate
 Potassium chromate
 Water sample

PRINCIPLE:

Generally water contains chloride ions (Cl-) ions in the form of NaCl, KCl, CaCl2 and
MgCl2. The concentration of chloride ions more than 250 ppm is not desirable for drinking
purpose. The total chloride ions can be determined by argentometric method (Mohr’s Method).
In this method Cl- ion solution is directly titrated against AgNO3 using potassium
chromate (K2CrO4) as the indicator.

AgNO3+ Cl- → AgCl↓+ NO-3

(In wate r) (White precipitate)
At the end point, when all the Cl- ions are removed. The yellow colour of the chromate
changes into reddish brown due to the following reaction.

2AgNO3 + K2CrO4 → Ag2CrO4 ↓ + 2KNO3

(Yellow) (Reddish brown)

TITRATION II

26
ESTIMATION OF CHLORIDE IN WATER SAMPLE

Std. Silver nitrate solution Vs water sample.

Volume of
Voume. of Burette Readings
AgNO3 Concordant
S.No. water Indicator
Initial Final Solution value
sample(ml)
(ml) (ml) (ml)

1.

2. K2CrO4

3.

Calculation:
Volume of silver nitrate solution (V1 ) = ml
Strength of silver nitrate solution (N1 ) = N
Volume of water sample (V2) = ml
Strength of water sample (N2) = ?
V1N1 = V2N2
N2 = V1N1 /V2
=
Strength of water sample = N.

Amount of chloride ion present in 1 litre of

the water sample = Eq. weight of Cl- × strength of
Cl- ion in water sample×1000 ppm

= 36.45 × strength of Cl- ion × 1000ppm

PROCEDURE:

27
Titration – I: Standardisation of silver nitrate solution:

The burette is washed well with distilled water and rinsed with the small amount
of AgNO3 solution. It is then filled with the same solution upto the zero mark without any air
bubbles. The pipette is washed with distilled water and rinsed with small amount of standard
NaCl solution. 20ml of this solution is pipetted out into a clean conical flask. 1ml of 2% K2CrO4
indicator is added and titrated against AgNO3 solution taken in the burette. The end point is the
change of colour from yellow to reddish brown followed by coagulation of white precipitate.
The titration is repeated for concordant values.
Titration – II: Estimation of chloride in water sample:

20ml of the given water sample is pipetted into a clean conical flask and 1ml of
2% K2CrO4 indicator solution is added. It is then titrated against standardized AgNO3
solution taken in a burette. The end point is the change of colour from yellow to reddish
brown followed by coagulation of white precipitate. The titration is repeated for concordant
values.
Equivalent weight of chloride ion is 35.46

RESULT:

Amount of chloride ion present in 1 litre of the given water sample = ppm

28
 Volume of
SI. No PH ∆PH ∆V ∆PH /∆V
NaOH (ml)

1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30

29
 5. DETERMINATION OF STRENGTH OF GIVEN HYDROCHLORIC
ACID USING PH METER
AIM
To determine the strength of given HCl by pH metry. A standard solution of 0.1 N
NaOH is provided.
MATERIAL REQUIRED:
 pH meter
 Glass electrode
 Beaker
 Standard N/10 NaOH
 Approximately N/10 HCl
 Burette, pipette, glass rod etc.,
PRINCIPLE:
The PH of a solution is related to H+ ions concentration by the following formula.
pH = -log 10 [H+]
When NaOH is added slowly to HCl, H+ ions get neutralized by OH- ions. The pH increases
slowly.
H+ Cl- + Na+ OH-  Na+ Cl- + H 2O
When all H+ ions of HCl are neutralized at the end point, addition of NaOH causes steep
increase in PH because of the addition of excess of OH- ions.
PROCEDURE:
The burette is washed with distilled water, rinsed with NaOH solution and filled with
the same upto zero mark. 20 ml of the given HCl solution is taken in a 100 ml beaker. It is
then diluted to 20ml with distilled water.
The glass electrode is immersed in the beaker and connected to pH meter without adding
NaOH the pH reading is noted. Then the pH readings are noted for 1 ml addition of NaOH up
to 30 ml.
Two graphs S-graph (volume of NaOH vs pH) and peak graph (Volume of NaOH vs Δ
PH /ΔV) are drawn. The end point is calculated from the graphs.

30
Model Graph

Calculation:
Step I: Calculation of Strength of HCl:
Volume of NaOH (V1) = ml (from graph)
Strength of NaOH (N1) = 0.1 N
Volume of HCl (V2) = ml
Strength of HCl (N2) = (V1 x N1) / V2
Strength of HCl = ---------------------- N
Step II: Calculation of amount of HCl:
Amount of HCl present in 1000ml
of the solution = Strength of HCl X Equivalent weight of HCl

=
= g.

31
RESULT:
i). Strength of the given HCl solution = N
ii). Amount of HCl present in 1 litre of the solution = g

32
 Volume of Conductance Volume of Conductance
S.No. S.No.
NaOH(ml) (mho) NaOH(ml) (mho)

1 26
2 27
3 28
4 29
5 30
6 31
7 32
8 33
9 34
10 35
11 36
12 37
13 38
14 39
15 40
16 41
17 42
18 43
19 44
20 45
21 46
22 47
23 48
24 49
25 50

33
6. DETERMINATION OF STRENGTH OF ACIDS IN A MIXTURE OF
ACIDS USING CONDUCTIVITY METER
AIM
To determine the amount of strong acid and weak acid present in 1 litre of the given
mixture of acids by Conductometric titration using standard NaOH of 0.1 N.
MATERIAL REQUIRED
 Conductivity Bridge
 Conductivity Cell
 Beaker
 Standard 0.1 N NaOH
 Given HCl&CH3COOH
 Burette
 Pipette
 Glass rod etc.,
PRINCIPLE:
Solution of electrolytes conducts electricity due to the presence of ions. Since specific
conductance of a solution is proportional to the concentration of ions in it, conductance of the
solution is measured during the titration.
HCl + NaOH  NaCl + H2O (I neutralization)
CH3COOH + NaOH  CH3COONa + H2O (II neutralization)
When a solution of HCl is titrated against NaOH, the fast moving hydrogen ions are
progressively replaced by slow moving sodium ions. As a result, conductance of the solution
decreases. This decrease will take place until the first neutralisation point is reached. Further
addition of alkali results in formation of sodium acetate.
Since sodium acetate is stronger than acetic acid conductivity slowly increases until all
acetic acid is completely neutralized. This is due to the presence of fast moving OH - ions. Any
more addition of alkali increases the conductance sharply.

34
Model Graph

STEP I
Calculation of strength of HCl
Volume of the mixture (HCl), V1 = 20 ml
Strength of the mixture (HCl), N1 =
Volume of the NaOH, V2 = (A) ml
Strength of the NaOH N2 = 0.1 N

According to the law of Volumetric analysis V1N1 = V2N2

N1 = V2N2 / V1
Strength of HCl = N

Calculation of amount of HCl

The amount of HCl present in1000 ml
of the given solution = Equivalent weight of HCl x Strength of HCl

= 36.5 x....................... N

= g

35
PROCEDURE
The burette is filled with NaOH solution upto zero mark. 20 ml of the given unknown
solution (mixture of a weak & a strong acid) is taken in a clean 100 ml beaker and diluted to
20 ml using distilled water. A conductivity cell is dipped into the solution and the terminals
are connected to the conductivity bridge. The burette solution is added to the unknown
solution in the beaker in 1 ml increments. The solution is stirred using a glass rod, and the
observed conductance values are recorded from the meter. The conductance decreases at the
beginning, then gradually increases and finally shows a steep increase.
The titration hence shows two end-points (i.e.) I neutralization (strong acid) & II
neutralization (weak acid). The titration is repeated with the same procedure. The accurate
end-point is obtained by plotting a graph between observed conductance vs. volume of NaOH
added.

36
STEP II
Calculation of strength of CH3COOH
Volume of the mixture (CH3COOH), V1 = 20 ml
Strength of the mixture (CH3COOH), N1 =
Volume of the NaOH, V2 = (B-A) ml
=
Strength of the NaOH, N2 = 0. 1 N
According to the law of Volumetric analysis V1N1 = V2N2,
N1 = V2N2 / V1
Strength of CH3COOH = N
Calculation of strength of CH3COOH
The amount of CH3COOH present in 1000 ml = Strength of CH3COOH X
of the given solution Equivalent weight of CH3COOH
=
= g

37
RESULT
(i)The amount of HCl present in the given solution = g
(ii)The amount of CH3COOH present in the given solution = g

38
39
 7. ESTIMATION OF IRON CONTENT OF THE GIVEN SOLUTION
USING POTENTIOMETER
AIM

To estimate the amount of ferrous ion present in whole of the given solution
potentiometrically. A standard solution of potassium dichromate of strength ------------- N is
provided.

MATERIAL REQUIRED

 Potentiometer
 Pt electrode
 Saturated calomel electrode
 Standard K2Cr2O7 solution
 Given Ferrous iron solution.
 Beaker,
 Burette
 pipette
 glass rod etc.,

PRINCIPLE
Potentiometric titrations depend on measurement of emf between reference electrode
and an indicator electrode. When a solution of ferrous iron is titrated with a solution of
potassium dichromate, the following redox reaction takes place.

6 Fe2+ + Cr2O72- + 14 H+  6 Fe3+ + 2Cr3+ + 7 H2O

During this titration Fe2+ is converted in to Fe3+, whose concentration increases. At

the end point, there will be a sharp change due to sudden removal of all Fe2+ ions.

The cell is set up by connecting this redox electrode with a calomel electrode as shown
below:

Pt, Fe2+, Fe3+// KCl , HgCl2 (s), Hg

A graph between emf measured against the volume of potassium dichromate added is

drawn and the end point is noted from the graph.

40
 Volume of
Emf ∆E ∆V ∆E/∆V
S.No K2Cr2O7
(Volt) (Volt) (ml) (Volt/ml)
(ml)
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30

41
PROCEDURE

The burette is filled with K2Cr2O7 solution upto the zero mark. 20 ml of ferrous ion
solution is pipetted out into a 100 ml beaker. About 20ml of dil.H2SO4 and 10ml of distilled
water are added in it.

A platinum electrode and a calomel electrode are dipped into this solution and
connected to a potentiometer. Then 1ml of potassium dichromate is added to the solution and
stirred well .The emf is measured and the titration is continued by adding potassium dichromate
in 1ml increments up to 30 ml.

Two graphs S-graph (Volume of K2Cr2O7 vs Emf and peak graph (Volume of
K2Cr2O7 vs ΔE/ΔV) are drawn . The end point is noted from the graph.

42
Calculation:
Step I: Calculation of Strength of Ferrous iron
Volume of Potassium dichromate (V1) = ml (from graph)
Normality of Potassium dichromate (N1) = N
Volume of Ferrous ion solution (V2) = ml
Normality of Ferrous ion solution (N2) = (V1 x N1 ) / V2
=
Strength of Ferrous iron = -------------- N
Step II: Calculation of Amount Ferrous iron
Amount of Ferrous ion present in
1000ml of the solution = Strength of ferrous iron x Equivalent weight of Fe

=
= g

The amount of Ferrous ion present in 1000 ml of the given solution = --------------- g

43
RESULT

The amount of Ferrous ion present in whole of the given solution is = -------------- g

44