ANNA UNIVERSITY

REGIONAL CAMPUS COIMBATORE

DEPARTMENT OF CHEMISTRY

LABORATORY MANUAL

ENGINEERING CHEMISTRY LABORATORY

(For First Year B.E. Programmes)

COURSE CODE: BS
3171

0
GENERAL INSTRUCTIONS TO THE STUDENTS
I. LABORATORY SAFETY
The following points are important and must be followed to avoid any kind of accidents inside
the laboratory:
a) Do not smoke, drink and eat inside the laboratory.
b) Try to wear laboratory coat and safety goggles.
c) Do not perform any unauthorized experiments without the permission of the instructors.
d) For any kind of chemical burn, wash the area with plenty of water and inform your
instructor promptly.
e) Do not pipette out liquids by mouth use suction bulbs.
f) Do not try to smell, taste any chemicals without the instructions of the concerned person.
g) Do not add water to the concentrated acids.
h) Do not touch any unknown chemicals by hands.
i) Before leaving the laboratory, wash your hands properly.

II. GENERAL RULES

a) Try to understand the experiment before you start it. If you have any query, discuss with
the instructor.
b) If some reagent/apparatus is not found, ask your laboratory attendant.
c) Finish the experiments within the specified time period.
d) Regular submission of the laboratory note book is mandatory. Late submission will not be
entertained for evaluation.
e) Never use mobile phones inside the laboratory.
III. SCIENTIFIC ASPECTS
While you are in the process of writing laboratory notebook, please keep the following pointsin
mind:
a) Scientific notations
b) Proper units
c) Number of significant digits
d) Error analysis
e) Graphs
i. it must have a name and the axes should be specified
ii. the data points should be clear on the graph
iii. if possible, the error bars may be provided

1
 Laboratory Safety Precautions
SAFETY INSTRUCTIONS

Safety signs and instructions from demonstrators and academic

supervisors must be strictly obeyed.
These activities are strictly forbidden in all laboratory areas or in
adjacent rooms.

SUPERVISION OF LABORATORY WORK

No one is to perform experimental work unless a demonstrator or a

member of the academic staff is present in the laboratory.

EYE PROTECTION

All persons must wear approved safety spectacles or goggles in

chemical laboratories.

PROTECTIVE CLOTHING

All persons carrying out experimental work must wear the appropriate
protective clothing.

REPORTING ACCIDENTS, FIRE AND DANGEROUS OCCURRENCE

All accidents resulting in injury, property damage or fire that might

cause injury, must be reported to the supervisor.

IN THE EVENT OF FIRE

1. Leave the building immediately by the nearest exit.

2. The person or persons responsible for starting and /or discovering
the fire must be available to brief with the Institute security
officer.

2
BS3171 PHYSICS AND CHEMISTRY LABORATORY L T P C
0 0 4 2
TOTAL: 30 PERIODS

CHEMISTRY LABORATORY: (Any seven experiments to be conducted)

COURSE OBJECTIVES:
 To inculcate experimental skills to test basic understanding of water quality parameters, such
as, acidity, alkalinity, hardness, DO, chloride and copper.
 To induce the students to familiarize with electroanalytical techniques such as, pH metry,
potentiometry and conductometry in the determination of impurities in aqueous solutions.
 To demonstrate the analysis of metals and alloys.
 To demonstrate the synthesis of nanoparticles

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

COURSE OUTCOMES:
 To analyse the quality of water samples with respect to their acidity, alkalinity, hardness and
DO.
 To determine the amount of metal ions through volumetric and spectroscopic techniques
 To analyse and determine the composition of alloy
 To learn simple method of synthesis of nanoparticles
 To quantitatively analyse the impurities in solution by electroanalytical techniques

TEXT BOOK:

1. J. Mendham, R. C. Denney, J.D. Barnes, M. Thomas and B. Sivasankar, Vogel’s Textbook of

Quantitative Chemical Analysis (2009).

3
 INDEX

S. No. Date Name of the Experiment Remarks Signature

4
Exp No. 1 Date:
5
 DETERMINATION OF ALKALINITY

Aim

To be familiar with the concepts of alkalinity and acidity, and the measurement of alkalinity in
water.
Theory
Alkalinity is primarily a way of measuring the acid neutralizing capacity of water. Alkalinity is
the ability of water to resist change in pH, which is due to presence of certain species such as
hydroxide ions OH-, bicarbonate ions HCO3- and carbonate ions CO3-. The alkalinity of natural
waters is due primarily to the salts of week acids. Bicarbonates represent the major form of
alkalinity. The following reactions are occurring during titration;
pH range above 8.3
OH- + H+ → H2O
CO 2- + H+ → HCO -
3
pH range between 8.3 and 4.5
HCO3- + H+ → H2CO3

P=M OH-
P=0
HCO3-
P=1/2 M CO32-
P>1/2 M Presence of OH – and CO32-
P=<1/2M Presence of CO32- and HCO3-

The alkalinity of water can be determined by titrating the water sample with hydrochloric acid of
known values of pH, volume and concentrations. Based on stoichiometry of the reaction and
number of moles of hydrochloric acid needed to reach the end point, the concentration of
alkalinity in water is calculated. A titration curve of a bicarbonate containing water is presented
in following figure.

6
Table I

Standard Na2CO3 Vs Hydrochloric acid

Volume of Burette reading Volume of

S.No Na2CO3 (ml) unknown Concordant value(ml)
Initial (ml) Final (ml) HCl
(ml)
1 20 0

2 20
0

Calculation:
Volume of Standard Sodium Carbonate V1 = 20 ml

Strength of Standard Sodium Carbonate N1 = …….N

Volume of hydrochloric acid V2 = ………….. ml

Strength of hydrochloric acid N2 =.........................N

V1 N1 = V2 N2

N2 = V1 N1
V2

Strength of Hydrochloric acid Solution =-----------------------N

7
MATERIALS REQUIRED
Apparatus: Solutions

1. Burettes, 50 mL 1. NaOH solution 0.1N

2. Conical Flask 2. HCl solution 0.1N
3. Beaker 3. Phenolphtalein indicator
4. Pipette (20 ml) 4. Methyl orange indicator
5. Burette stand with clamp 5. Sodium carbonate solution
6. Water Sample
Procedure
The procedure for the determination of the alkalinity of a water sample by double indicator
method consists of the following steps:
a) Preparation of standard solution of sodium carbonate
b) Standardisation of hydrochloric acid solution by titrating against standard sodium carbonate
solution.
c) Determination of phenolphthalein end point by titrating against standardised hydrochloric acid
d) Determination of methyl orange end point by titrating against standardised hydrochloric acid
e) Calculation of the concentrations of hydroxide and carbonate ions.

Standardization of hydrochloric acid solution by titrating against standard sodium

carbonate solution
i) Fill up the burette with hydrochloric acid solution with the help of a funnel and mount it
on the burette stand. Note the reading on the burette and record it in the observation
Table 1 under the initial reading column.
ii) Carefully pipette out 20 cm3 of the standard sodium carbonate solution and transfer to a
clean 250 cm3 conical flask. Add two to three drops of methyl orange indicator.
iii) Titrate the yellow colored solution with constant swirling against a white background
(you may use a porcelain tile for the purpose) till a red colour is obtained. Record the
reading in the Observation Table under the final reading column.
iv) Repeat the titration to get at least two concordant readings and record the same in the
Observation Table

8
Table II
Standardized Hydrochloric acid Vs Water Sample A

Burette Reading
Volume of water sample Volume of Hydrochloric
A (ml) Initial Final ( P) Final (M) Acid Consumed

Calculations
Water sample-A Phenolphthalein alkalinity
Volume of Hydrochloric acid (phenolphthalein end point) V1=................ml
Strength of hydrochloric acid (N1) =.................N
Volume of water sample-A =.................ml (Concordant Value)
Phenolphthalein alkalinity = Vacid X Nacid X 50 X 1000/ Vwater sample
= ppm

Methyl Orange or Total Alaklinity

Volume of hydrochloric acid (methyl orange end point) =...........................ml
Strength of hydrochloric acid N2 =.........................N
Volume of water sample-A =.................ml (Concordant Value)
Methyl Orange alkalinity = Vacid X Nacid X 50 X 1000 / Vwater sample
= ppm

9
Titration I
Determination of phenolphthalein end point, PE by titrating against standardised
hydrochloric acid
i) Transfer 20 cm3 of the water sample into a conical flask; add 1 drop of phenolphthalein
indicator, and titrate the sample with the standardized HCl solution till a faint pink colour
persists. Record the initial and final burette readings in Observation Table I
ii) Repeat the titration to get at least two concordant readings and record the same in the
Observation Table 2

10
Table III
Standardized Hydrochloric acid Vs Water Sample B

Burette Reading
Volume of water sample Volume of Hydrochloric
B (ml) Initial Final ( P) Final (M) Acid Consumed

Calculations
Water sample-B Phenolphthalein alkalinity
Volume of Hydrochloric acid (phenolphthalein end point) V1=................ml
Strength of hydrochloric acid (N1) =.................N
Volume of water sample-B =.................ml (Concordant Value)
Phenolphthalein alkalinity = Vacid X Nacid X 50 X 1000/ Vwater sample
= ppm

Methyl Orange or Total Alaklinity

Volume of hydrochloric acid (methyl orange end point) =...........................ml
Strength of hydrochloric acid N2 =.........................N
Volume of water sample-B =.................ml (Concordant Value)
Methyl Orange alkalinity = Vacid X Nacid X 50 X 1000 / Vwater sample
= ppm

11
Titration II
Determination of methyl orange end point, ME by titrating against standardised
hydrochloric acid
i) Transfer 20 cm3 of the water sample into a conical flask; add 2-3 drops of methyl
orange indicator, and titrate the sample with the standardized HCl solution till
you obtain a red colour. Record the initial and final burette readings in
Observation Table II
ii) ii) Repeat the titration to get at least two concordant readings and record
the same in the Observation Table 3
Alternatively, step (I) and (II ) given above can be combined. In this method, 20 cm 3 of the water
sample taken in a conical is titrated with the standard HCl solution using phenolphthalein
indicator, till pink colour disappears. The titre value is recorded as the phenolphthalein end point,
PE and 2 to 3 drops of methyl orange indicator are added to the same solution and the titration is
continued until a red coloured end point is obtained. The titre value from the beginning of the
titration is recorded as the methyl orange end point, ME.

Result
Anions present in the given water samples

Alkalinity Water Sample A Water Sample B

1/2M

P>1/2 M or P=<1/2M

Types of species

12
13
Exp.No : 2
Date:
Aim:
To estimate theDETERMINATION OF TOTAL,
total, permanent and temporary hardnessTEMPORARY
of water by EDTA method. You are
& PERMANENT
provided with a standard HARDNESS
hard water solution OFMWATER
of strength 0.01 BY link solution.
and an EDTA
EDTA METHOD
Priniple:

Structure of Eriochrome Black T

EDTA forms stable complexes with divalent cations such as Ca2+ and Mg2+ .The indicator
is Eriochrome Black-T. At a pH of about 10, the indicator forms a wine red colour complex with
Ca2+ and Mg2+. On addition of EDTA solution, the EDTA snatches the metal ions from the metal
ion-indicator complex, rendering the indicator free.

Ca2+
+ Eriochrome Black-T [Ca-EBT/ Mg-EBT]
Mg2+ (EBT) (wine red colour)

[Ca-EBT/Mg-EBT] + EDTA [Ca-EDTA/Mg-EDTA] + EBT

(Colourless) (Steel blue)

14
Titration – I: Standardisation of EDTA Solution

Standard hard water Vs EDTA Indicator: Eriochrome Black T

Volume of Burette reading Volume of
S.No Std. hard EDTA Concordant value(ml)
water (ml) Initial (ml) Final (ml) (ml)
1 20 0

2 20
0

Calculation:
Volume of the standard hard water sample V1 = 20 ml

Strength of the standard hard water sample N1 =

Volume of EDTA V2 = ………….. ml

Strength of EDTA N2 =.........................M

V1 N1 = V2 N2

N2 = V1 N1
V2

Strength of the EDTA Solution =-----------------------M

Titration I:
15
Standardization of EDTA
The burette is washed with distilled water and then rinsed with unknown EDTA solution

and filled with the same. 20 ml of standard hard water is pipetted out into a clean conical flask.

To this, 5 ml of buffer solution (a mixture of ammonium chloride and ammonium hydroxide)

and 2 drops of 0.5% EBT indicator are added. The contents of the flask are titrated against the

EDTA solution. The end point is the colour change from wine red to steel blue. The titration is

repeated for concordancy.

Titration – II:
16
Estimation of Total hardness of water
Hard water sample Vs Standardized EDTA solution Indicator: EBT

Volume of Burette reading Volume of

S.No hard water EDTA Concordant value(ml)
sample (ml) Initial (ml) Final (ml) (ml)
1 20 0

2 20 0

Calculation:

Volume of EDTA V1 = ………….. ml

Strength of EDTA N1 = . ………… M

Volume of the hard water sample V2 = 20 ml

Strength of the hard water sample N2 = ?

V1 N1 = V2 N2

N2 = V1 N1
V2

Strength of the hard water sample =-----------------------M

Total hardness of hard water sample =..............................M x 50 x 1000

= ppm

17
Titration II:

Estimation of total hardness of water

The burette is washed with distilled water and then rinsed with EDTA solution and filled
with the same. 20 ml of hard water is pipetted out into a clean conical flask. To this, 5 ml of
buffer solution (a mixture of ammonium chloride and ammonium hydroxide) and 2 drops of
0.5% EBT indicator are added. The contents of the flask are titrated against the EDTA solution.
The end point is the colour change from wine red to steel blue. The titration is repeated for
concordancy.

18
Titration – III

Estimation of permanent hardness of water

Boiled Hard water sample Vs Std.EDTA Indicator: EBT

Volume of Burette reading Volume of

S.No boiled hard EDTA Concordant value(ml)
water (ml) Initial (ml) Final (ml) (ml)
1 20 0

2 20 0

Calculation- Titration III

Volume of EDTA V1 = ………….. ml
Strength of EDTA N1 = …………. M
Volume of the boiled hard water sample V2 = 20 ml
Strength of the boiled hard water sample N2 = ?
V1 N1 = V2 N2

N2 = V1 N1
V2
=
Strength of the boiled hard water sample =-----------------------M
Permanent hardness of water sample =..............................M x 50 x 1000
= ppm

Temporary hardness of water = Total hardness – Permanent hardness

= -
= ppm as CaCO3 equivalent

19
Titration III

Estimation of permanent hardness of water

20 ml of hard water is pipetted out into a clean beaker and the solution is boiled for 5 to
10 minutes. It is then cooled and filtered. The precipitated salts of Ca 2+ and Mg2+ ions are filtered
off. To the filtrate, 5ml of buffer solution and 2 drops of 0.5% EBT indicator are added. The
contents of the flask are titrated against the EDTA solution. The end point is the colour change
from wine red to steel blue. The titration is repeated to get concordant value.

Result:

Total hardness of the water sample = ppm

Permanent hardness of the water sample = ppm.

Temporary hardness of the water sample = ppm

20
21
Ex No: 3 Date:

ESTIMATION OF DISSOLVED OXYGEN

Aim:
IN WATER [WINKLER’S
To estimate the amount of dissolved oxygen (DO) in the given water sample by Winkler’s
method. A standard link solution of potassium dichromate of strength 0.01N and sodium
thiosulphate solution are provided.

Principle:
Air is dissolved in pure water to a definite proportion. Hence, oxygen content in water is
always a constant and is 8 mg/L at 25°C and 14 mg/L at 0°C. This amount may decrease as the
impurity level increases because of aerobic oxidation. If water is highly polluted, oxygen level
may go even to zero. Thus, the oxygen content in water may give some ideas about the level of
organic impurities. Thus, the estimation of dissolved oxygen in water is useful in studying water
pollution and corrosion effects of boiler feed water.
Water sample is collected carefully avoiding aeration / deaeration in ground stoppered flask.
Initially manganese sulphate and alkali-iodide reagents are added and the reactions occur as
follows

Mn2+ + 2OH- Mn (OH)2 (White)

Mn (OH)2 + 1/2O2 MnO (OH)2 (Yellow brown)

After half an hour, the precipitate is dissolves in minimum amount of concentrated sulphuric
acid. The liberated iodine is titrated against Na2S2O3 using starch indicator.

MnO (OH)2 + 2H2 SO4 Mn(SO4)2 + 3H2O

Mn (SO4)2 + 2KI MnSO4 + K2SO4 + I2

2Na2S2O3 + I2 Na2S4O6 + 2NaI

22
Titration I: Standardization of sodium thiosulphate
Potassium dichromate Vs Sodium thiosulphate Indicator: Starch

Volume of Burette reading (ml) Volume of

Potassium sodium
S.No Concordant
dichromate Initial Final thiosulphate
value(ml)
(ml) (ml)
1 0.0

2 0.0

3 0.0

Volume of standard Potassium dichromate V1 = 20ml

Strength of standard Potassium dichromate N1 =------------------N

Volume of sodium thiosulphate V2 =----------------ml

Strength of sodium thiosulphate N2 = ?

V1 N1 = V2 N2

N2 = V1 N1
V2

Strength of sodium thiosulphate N2 =-----------------------N

23
 From the equations, it is clear that amount of iodine is indirectly equal to the amount
oxygen. That is, one equivalent weight of oxygen is equivalent to one equivalent weight of
iodine which is equal to one molecular weight of sodium thiosulphate.
Sodium thiosulphate solution can be standardised using standard potassium dichromate
solution. When potassium iodide solution is added to acidified potassium dichromate solution,
iodine is liberated as below:
K2Cr2O7 + 7 H2SO4 +6 KI 4K2SO4 + Cr2(SO4)3 + 7 H2O+3I2
The liberated iodine is titrated against sodium thiosulphate solution. Starch is added near the end
point as indicator. The end point is the disappearance of blue colour leaving behind a pale green
colour due to the formation of chromium sulphate.

Procedure:

Titration I: Standardization of sodium thiosulphate

The burette is washed and rinsed with sodium thiosulphate solution. Then the burette is filled
with this sodium thiosulphate solution up to zero mark without any air bubbles. 20 ml of 0.01N
potassium dichromate solution is pipette out by means of clean and rinsed pipette into a clean
iodine flask.
About 10 ml of dilute sulphuric acid and 10 ml of 5 % potassium iodide solution are added.
The liberated iodine is titrated at once against sodium thiosulphate solution taken in the burette.
When the solution in the iodine flask becomes straw yellow colour, 1 ml of freshly prepared
starch solution is added as indicator and the titration is continued. The end point is the
disappearance of blue colour and the appearance of pale green colour. Titre value is noted and
titrations are repeated for concordant value.

24
Titration II : Estimation of dissolved oxygen

Water sample Vs. Sodium thiosulphate Indicator: Starch

Burette reading Volume of

(ml) Sodium
Volume of water Concordant
thiosulphate(ml)
S. No. sample (ml) value (ml)
Initial Final
1 0.0

2 0.0

3 0.0

Calculation:
Volume of sodium thiosulphate V1 =-------------------ml
Strength of sodium thiosulphate N1 =-------------------N
Volume of water sample V2 = 100ml
Strength of water sample (or) Strength
of dissolved oxygen in water N2 = ?

V1 N1 = V2 N2

N2 = V1 N1
V2

= ml × N

100

Amount of dissolved oxygen in one litre

Of tap water = Normality × Eq.wt.of O2 ×1000mg

=-------------N × 8 × 1000
=..................mg/L

25
Titration II: Estimation of dissolved oxygen
250 mL iodine flask is filled with tap water slowly through the sides upto the neck. 2 mL
alkali iodide mixture (sodium hydroxide and potassium iodide) and 2 ml of 5 % manganous
sulphate solution are added and stoppered properly. There should not be any air bubble inside the

flask. The flask is inverted and shaken seveal times for thorough mixing of reagents. The flask is
kept aside for about 15 minutes for settling of the precipitate. When half of the precipitate settles
down, the stopper is removed and few ml of concentrated sulphuric acid is added with much
caution to get a clear yellow solution due to the liberation of iodine. 100 ml of the water sample
is pipetted out into the iodine flask and titrated against standardized sodium thiosulphate
solution. When the solution becomes light yellow, starch indicator is added. The titration is
continued until the blue colour disappears. From the titre value, the strength of dissolved oxygen
is calculated and hence the amount of dissolved oxygen in the water sample is calculated.

Result:
Amount of dissolved oxygen in tap water =------------------------mg/L

26
 Titration I
Standardization of Silver Nitrate
Standard Sodium chloride Vs Silver nitrate Indicator: Potassium chromate

Burette reading (ml) Volume of

Volume of Sodium
S.No Silver Nitrate Concordant
Chloride (ml) Initial Final (ml) value(ml)
1 0.0

2 0.0

3 0.0

Volume of standard sodium chloride V1 = 20 ml

Strength of standard sodium chloride N1 =------------------N

Volume of silver nitrate V2 =----------------ml

Strength of silver nitrate N2 = ?

V1 N1 = V2 N2

N2 = V1 N1
V2

Strength of silver nitrate N2 =-----------------------N

27
Ex No: 4 Date:

Aim: DETERMINATION OF CHLORIDE CONTENT OF

WATER SAMPLE BY ARGENTOMETRIC
METHOD
To estimate the amount of chloride ion present in the given water sample by argentometric
method (Mohr’s method). A standard solution of sodium chloride of strength 0.01N and a link
solution of AgNO3 are provided.

Principle:
Natural water contains Cl- ion in the form of NaCl, KCl, CaCl2 and MgCl2. The total Cl- ion
can be estimated by argentometric method. It is known as Mohr ’s titration. Here Cl- ion solution
is titrated with AgNO3 using potassium chromate (K2CrO4) as the indicator. It is a precipitation
titration.
AgNO3 + NaCl AgCl + NaNO3
(in water) White ppt

When all the Cl- ion is removed, AgNO3 added from the burette will react with K2CrO4 to
give a reddish brown colour due to the formation of Ag2CrO4 . This is the end point. This
reaction takes place only at the end point, since a precipitation reaction takes place in preference.

2AgNO3 + K2CrO4 Ag2CrO4 + 2KNO3

(Yellow) (Reddish brown)
Procedure:

Titration I Standardisation of silver Nitrate

The burette is washed well with distilled water and rinsed with a small amount of silver
nitrate 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 a small amount of standard
sodium chloride solution. 20 ml of this solution is pipetted out into a clean conical flask. 1 ml of
2 % K2CrO4 indicator solution is added and titrated against AgNO3 solution taken in the burette.

28
Titration II: Estimation of chloride ion in water sample

Water sample Vs AgNO3 Indicator: Potassium Chromate

Volume of water Burette Reading Volume of

Concordant
S.No sample ( ml ) Ag NO3
value (ml)
( ml ) Initial Final ( ml )
1

Calculation:

Volume of AgNO3 V1 =
Strength of AgNO3 N1 =
Volume of water sample V2 =
Strength of water sample N2 = V1 N1
V2

Amount of chloride ion in = Eq.wt × Strength of chloride ion

1 litre of water sample
= 35.45 ×..................g
=....................g
=......................× 1000 mg.

29
The end point is the change of colour from yellow to permanent reddish brown colour followed
by the coagulation of white precipitate. Titre value is noted and titrations are repeated for
concordant value.
Titration II: Estimation of chloride ion in water sample

20 ml of the given water sample is pipetted out by means of a clean and rinsed pipette
in to a clean conical flask. 1 ml of 2 % K2CrO4 indicator solution is added and titrated against
AgNO3 solution taken in the burette. The end point is the change of colour from yellow to
permanent reddish brown colour followed by the coagulation of white precipitate. Titre value is
noted and titrations are repeated for concordant value. Equivalent weight of chloride ion (Cl -) =
35.45g

Result:
Amount of chloride ion present in the given water sample =....................mg/l

30
31
Ex No: 5 Date:

ESTIMATION OF COPPER CONTENT OF THE GIVEN SOLUTION

Aim:
BY IODOMETRY
Estimate the amount of copper in the given solution by iodometric method. You are provided
with a standard solution of potassium dichromate of strength 0.1N and sodium thiosulphate
solution as link.
Principle:

The strength of copper sulphate solution is determinded by iodometric method. When

potassium iodide is added to a solution of copper sulphate a white cuprous iodide (Cu 2I2) is
precipitated and an equivalent amount of iodine is liberated. The free iodine is titrated against
standard solution of sodium thiosulphate using starch as an indicator, as soon as all the liberated
iodine is reduced to iodide (NaI) the blue colour of the iodo starch complex will disappear. The
colour of precipitate in the conical flask will be white, Cu2I2. This indicates the end point.

The reactions involved are:

2CuSO4+4KI Cu2I2+2K2SO4+I2
2Na2SO4+I2 Na2S4O6+2NaI
From the titre values, the strength of copper sulphate solution and the amount of copper
are calculated. Sodium thiosulphate is standardized using standard potassium dichromate as in
the following equation.

K2Cr2O7+7H2SO4+6KI 4K2SO4+Cr2(SO4)3+3I2+7H2O

The librated iodine is titrated against sodium thiosulphate using starch as indicator. The
end point is the appearance of green colour. From the equations it is clear that the equivalent
weight of crystalline copper sulphate is its molecular weight i.e. 249.54 and that of copper is its
own atomic weight i.e. 63.54.

32
Titration I: Standardization of sodium thiosulphate
Potassium dichromate Vs Sodium thiosulphate Indicator: Starch

Volume of Burette reading (ml) Volume of

Potassium sodium
S.No Concordant
dichromate Initial Final thiosulphate
value(ml)
(ml) (ml)
1 0.0

2 0.0

3 0.0

Volume of standard Potassium dichromate V1 = 20ml

Strength of standard Potassium dichromate N1 =------------------N

Volume of sodium thiosulphate V2 =----------------ml

Strength of sodium thiosulphate N2 = ?

V1 N1 = V2 N2

N2 = V1 N1
V2

Strength of sodium thiosulphate N2 =-----------------------N

33
PROCEDURE:
Ttration I: Standardisation of sodium thiosulphate
The burette is washed and rinsed with sodium thiosulphate solution. Then the burette is
filled with this sodium thiosulphate solution upto zero mark without any air bubbles. 20 Ml of
0.1N potassium dichromate solution is pipetted out by means of clean and rinsed 20 ml pipette
into a clean conical flask.

About 10ml 10% potassium iodide solution are added. The liberated iodine is titrated at
once against sodium thiosulphate solution taken in the burette. When the solution in the conical
flask becomes straw yellow colour, 1 ml of freshly prepared starch solution is added as indicator
and the titration is continued. The end point is the disappearance of blue colour and the
appearance of pale green colour. Titre value is noted titrations are repeated for concordant
values.

34
Titration II: Estimation of Copper
Sodium thiosulphate Vs Copper sulphate Indicator: Starch

Burette reading (ml) Volume of

Volume of Copper
sodium
S.No sulphate Concordant
Initial Final thiosulphate
(ml) value(ml)
(ml)
1 0.0

2 0.0

3 0.0

Volume of sodium thiosulphate V1 =------------------ml

Strength of sodium thiosulphate N1 =------------------N

Volume of copper sulphate V2 = 20.0 ml

Strength of copper sulphate N2 = ?

V1 N1 = V2 N2

N2 = V1 N1
V2

Strength of copper sulphate N2 =-----------------------N

Equivalent weight of copper = 63.54

The amount of copper present in 1L = 63.54 × Normality

= g

35
Titration II: Estimation of Copper

20ml of the given copper sulphate solution is pipetted out by means of a clean and rinsed
20ml pipette into a clean conical flask. Ammonium hydroxide is added drop by drop till a
permanent precipitate is formed. The precipitate is redissolved by adding drop by drop acetic
acid.

About 5ml of 10% solution of potassium iodide is added. The liberated iodine is titrated
against sodium thiosulphate solution taken in the burette. 1ml of freshly prepared starch solution
is added as indicator towards the end point. The end point is the disappearance of blue colour.
The titration is repeated till concordant values are obtained. From the titre values, the strength of
copper sulphate and the weight of copper in the whole of the given solution can be calculated.
The equivalent weight of copper is 63.54.

RESULT
The strength of copper sulphate solution =................................N
The amount of copper present in the given solution =.................................g

36
 HCl vs Std.NaOH

Table 1

Volume of NaOH
S.No (V) ml pH
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20

37
Exp No: 6 Date:
Aim:
pH TITRATION

To determine the strength of approximately 0.1 N hydrochloric acid solution by pH titration.

Principle:
pH titrations are frequently used to find out the end point of acid base titrations especially

in the case of coloured solutions where visual indicators cannot be used.

When an acid is titrated with a base the H + ions of the acid is progressively consumed

increasing the pH only slightly. Near the end point the change of pH is very large due to

presence of small excess of either H+ ions or OH- ions.

Procedure:

Pipette out 20ml of the given hydrochloric acid solution into a clean 100ml beaker. Dilute

it to 50ml. Immerse the pH electrode and connect it to a standardized pH meter and note the

initial pH. Take the standard 0.1N NaOH solution in the burette. Add NaOH solution in small

increments initially and drop by drop in the vicinity of the equivalence point and thereafter. Stir

the solution thoroughly after each addition and note the pH. Plot a graph taking ΔpH/ ΔV in the y

axis and volume of base in the x axis. The volume of base which corresponds to the maximum of

the curve is the end point. From the titre value, calculate the strength of hydrochloric acid

solution.

38
Table 2

Volume of Average
NaOH volume
S.No (V) ml pH ΔV(ml) ΔpH ΔpH/ ΔV v (ml)
1

2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
Calculation:
Volume of NaOH V1 =..................................ml
Strength of NaOH N1 =..................................N
Volume of HCl V2 =..................................ml
Strength of HCl N2 = V1 N1
V2

N2=

Strength of HCl N2 =.........................N

39
Result:

Strength of the given hydrochloric acid solution =.........................N

40
Model Graph

TITRATION Mixture of strong and weak acids Vs NaOH

Volume of Volume of
Conductance Conductance
S.No NaOH added S.No NaOH
(S) (S)
(ml) added (ml)

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

41
Exp No: 7 Date:

AIM: CONDUCTOMETRIC ACID-BASE TITRATION

(Mixture of weak and strong acids Vs Strong base)
To determine the amount of strong and weak acids present in the solution by
Conductometric titration using standard sodium hydroxide solution of strength 0.1N.

PRINCIPLE:

Solutions of electrolytes conduct electricity due to the presence of ions. Specific conductance
of a solution is proportional to the concentration of ions present in it. Conductance of the
solution is measured during titration.

When sodium hydroxide solution is added slowly from the burette to the mixture, HCl (Strong
acid) gets neutralized first. Since the fast moving H+ ions are replaced by slow moving Na+ ions,
decrease in conductance takes place until the end point is reached.

H+ Cl- + Na+OH- NaCl + H2O (1st neutralization)

After the complete neutralization of HCl, the neutralization of CH3COOH commences,

CH3COOH + Na+OH- CH3COONa + H2O (2nd neutralization)

Since CH3COONa is stronger electrolyte than CH3COOH, conductivity slowly increases

until CH3COOH is completely neutralized. When the end point is reached, addition of NaOH
will cause sudden increase in the conductance. This is due to the introduction of fast moving OH -
ions.

42
Step 1
Calculation of strength of HCl
Volume of NaOH V1 =.................................(x1) ml
Strength of NaOH N1 =..................................N
Volume of HCl V2 =.................................ml
Strength of HCl N2 = V1 N1
V2
=.................................N

The amount of HCl present in the 1 litre of the given solution

= Strength of HCl× Eq. wt of HCl
=……………….× 36.5
=.........................g

Step 2
Calculation of strength of CH3COOH
Volume of NaOH V1 =....................................(x2 - x1) ml
Strength of NaOH N1 =.................................N
Volume of CH3COOH V2 =.................................ml
Strength of CH3COOH N2 = V1 N1
V2
=.................................N

The amount of CH3COOH present in the 1 litre of the given solution

= Strength of CH3COOH × Eq. wt of CH3COOH
=……………….× 60
=.........................g

43
PROCEDURE:
Pipette out 20 mL of the acid mixture into a clean beaker. Dilute with distilled water up
to 100 mL. Dip the conductivity cell and connect it with a conductivity meter and note down the
initial conductance.
Fill standard NaOH solution in the burette. Add NaOH solution to the mixture in 1 mL
portions and stir the solution thoroughly and note down the conductance each time. The
conductivity is going on decreasing upto the 1st neutralization point (A). Plot a graph by taking
volume of NaOH in the X- axis and conductance in Y- axis. Extrapolate the straight lines, the
point of intersection of first and second line gives the volume of standard NaOH, required to
neutralize the strong acid (x1). Continue the titration even after the first end point is over.
After the first end point, when NaOH is added conductance increases gradually. This
increase in conductance is observed until the 2 nd neutralization point (B) is reached. In the same
graph, extrapolate the straight lines, the point of intersection of second and third straight line
gives the volume of standard NaOH, required to neutralize the strong and weak acids (x 2). From
the titre values (x1 and x2), calculate the strength of strong (HCl) and weak acid (CH 3COOH)
solutions.

Result:
i) The amount of HCl present in the given mixture =.......................g
ii) The amount of CH3COOH present in the given mixture =.........................g

44
Table 1
FAS vs Std. K2Cr2O7

S.No Volume of K2Cr2O7 Emf (E) mv

(V) ml
1

2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20

45
Exp No: 8 Date:

Aim:
To determine the amount of ferrous ion in the given solution by a potentiometric redox
titration.

Principle:
Ferrous ion can be oxidized by potassium dichromate according to the equation
2+
6Fe + Cr 2O 72- + 14H+ 2Cr3+ + 6Fe3+ + 7H 2O

Depending on the ratio of oxidant to reductant, the potential of the system changes
according to the Nernst equation
E=E0 + (0.0591/n) log ([Fe3+]/ [Fe2+]) at 25°C..............................(1)
3+ 2+
(Fe / Fe )

E=E0 + (0.0591/n) log ([Cr2O72-]/ [Cr3+]) at 25°C.............................(2)

2- 3+
(Cr2O7 / Cr )
When FeSO4 is taken as titrant and potassium dichromate as the titrant, the potential of
the system is determined by the equation (1) till the end point. After the end point the potential is
determined by the equation (2). Hence an abrupt change of potential will be expected in the
vicinity of the end point.
Procedure:
Pipette out 20ml of FAS solution into a clean 250ml beaker. Add 20ml of dilute sulphuric
acid and dilute the mixture to 100ml. Dip a platinum electrode into the solution and form the
following cell.
Pt/ Fe 2+, Fe3+, [H+]//SCE
Connect the terminals to a potentiometer bridge and note the initial emf. Take the
standard 0.1N potassium dichromate solution in the burette. Add dichromate in small increments
initially and drop by drop in the vicinity of end point and thereafter stir the solution thoroughly
after each addition and note the potential. Plot the graph taking ΔE/ ΔV in y axis and volume in x
axis. The volume of potassium dichromate which corresponds to the maximum of the curve is
the end point. From the titration value calculate the strength and amount of ferrous ion in one
litre solution.
Equivalent mass of Fe2+ is 55.85g.equiv -1.

37
Table 2 FAS VS std. K2Cr2O7
Volume of Average volume
S.No K2Cr2O7 (V) ΔV ΔE ΔE/ ΔV of K2Cr2O7
ml Emf (E) v (ml)

Calculation:
Volume of K2Cr2O7 V1 =..................................ml
Strength of K2Cr2O7 N1 =.................................N
Volume of FAS V2 =.................................ml
Strength of FAS N2 = V1 N1
V2
=.................................N

Amount of ferrous ion in 1 litre = Strength of FAS× Eq.wt of ferrous ion

of the solution
= × 55.85

=..............................g

38
Result:
Amount of ferrous ion in 1 litre of the given solution=….......................g.

39
Model Graph

TITRATION

Strong acid and Strong Base

Volume of Volume of
Conductance Conductance
S.No NaOH added S.No NaOH
(S) (S)
(ml) added (ml)

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

40
 Exp No: 9 Date:

ESTIMATION OF SODIUM AND POTSSIUM PRESENT IN WATER USING

FLAME PHOTOMETER.

AIM:
Estimate the amount of sodium and potassium present in the given water sample using flame
photometer.
PRINCIPLE AND INSTRUMENTATION

Flame photometry or flame emission spectroscopy is based on the principale of emission of

certain radiation in the visible region by metal atoms such as Li, Na, K and Ca. atoms are formed from
their solution, during atomization in the flame at about 1700 oC. the whole process is explained by the
following steps for sodium estimation.
Na+Cl- Na+Cl- Evaporation
NaCl(s) NaCl(g) Na+Cl Atom
Salt solution (Aerosol) ↓
Emission of yellow light
Na Na*
↓
Detector

The intensity of the emitted radiation is measured.

The concentration of sodium can be known by drawing a calibration graph. This method is
employed when the concentrations are in the range 1-10 ppm. Air at the pressure of 0.55kg/cm 2 is
placed into nebulizer and the solution in a beaker is sucked into the nebulizer through the capillary tube.
This joins air stream to form aerosol. LPG gas is supplied to the flame chamber at a regulated rate and
mixed with air in the chamber. The mixture is burnt at the top of the burner. Radiations from the
resulting flame are passed through the photovoltaic cell. The output of the cell is seen in the display.
A calibration graph is drawn between intensity of emitted radiation (flame photometer reading,
FPMR) and concentration. The FPMR for unknown concentration is found out. The concentration of
unknown solution can be determined from the calibration graph.

41
Determination of Sodium and Potassium

λmax of Sodium = 589 nm λmax of Potassium = 766.5 nm

S.No Concentration FPMR Concentration FPMR

of Sodium of Potassium
(mg/L) (mg/L)

7 Unknown Unknown

42
PROCEDURE: Estimation of Sodium
The instrument is switched on and air supply and gas supply are regulated. Distilled water is sent
through the capillary tube and ignition is started. After the instrument is warmed up for 10 minutes, it is
adjusted to zero reading in the display. The λ max for sodium is 589 nm. Sodium chloride solution of
concentration 8 ppm is then kept in the instrument and the reading is adjusted to 100. After this
calibration of the instrument, no adjustment should be made.
Solution of known concentrations (1,2,3,4,5,6 ppm) are taken and FPMR are noted for each
concentration. Using this calibration graph was drawn taking FPMR in the y-axis and concentration in
the x-axis.
Finally the FPMR reading for unknown solution is found. The concentration of the unknown solution
can be determined using the calibration graph.

Estimation of Potassium
Similar procedure is adopted for the determination of potassium in water sample. The lamda λ max
for potassium is 766.5nm.

Result:
Amount of sodium present in the given sample of water = -------------------mg/L or ppm
Amount of potassium present in the given sample of water= -------------------mg/L or ppm

43
 TABLE

BaCl2 Vs Na2SO4

Volume of BaCl2 = 20 ml

Volume of Volume of
Conductance Conductance
S.No Na2SO4 S.No NaOH
(mho) (S)
added (ml) added (ml)

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

Model Graph

Exp No: 10 Date:

44
 AIM:
CONDUCTOMETRIC PRECIPITATION TITRATION
To determine the amount of USING BaCl2- Na
BaCl2 present SO4given solution by Conductometric
in 2the
titration using standard Na2SO4 solution of ………….. N.

PRINCIPLE:

Solutions of electrolytes conduct electricity due to the presence of ions. Since specific
conductance of a solution is proportional to the concentration of ions present in it.
Conductance of the solution is measured during titration.

In the precipitation titration, the ions are converted into insoluble precipitate, which will not
contribute to the conductance. When Na 2SO4 is added slowly from the burette to the solution of
BaCl2, BaSO4 gets precipitated while the chloride ions remain unchanged.
BaCl2 + Na2SO4 BaSO4 + 2 NaCl
The Ba2+ ions in the solution are replaced by free Na + ions. Since the mobility of Na + ions are
less than that of Ba2+ ions, the conductance of the solution decreases. After the end point, when
all the Ba2+ ions are replaced, further addition of Na 2SO4 increases the conductance. This is due
to the increase of Na+ and SO42- in the solution.

MATERIALS REQUIRED

1. Conductivity bride 2. Conductivity cell 3. 100 ml beaker 4. Std Na2SO4 solution 5. Given BaCl2 solution
6. Burette, pipette, glass rod etc., 7. Distilled water.

45
Calculation
Volume of BaCl2 mixture V1 = 20 ml
Strength of BaCl2 mixture N1 = ……..?
Volume of Na2SO4 V2 = ……….. ml
Strength of Na2SO4 N2 = ……………. N
According to law of volumetric analysis V1 N1 = V2 N2

V 2 N 2 … … … . … …..
N 1= =
V1 20

 Strength of BaCl2 =..............................N

The amount of BaCl2 present in the given solution = Strength of BaCl2× Eq. wt of BaCl2
=……………….× 122.14
=.........................gms/ lit

46
PROCEDURE
The burette is filled with Na2SO4 solution upto the zero level. 20 ml of the given BaCl2
solution is pipette out into a clean 100 ml beaker. The conductivity cell is placed in it and then
diluted to 40 ml by adding conductivity water. The two terminals of the cell are connected with
a conductivity bridge.
Now 1ml of Na2SO4 from the burette is added to the solution, taken in the beaker, stirred
and then conductivity is measured. This is continued upto the end point. (The conductivity is
going on decreasing up to the end point). After the end point, again Na 2SO4 is gradually added
and few more readings are noted.
Thus, the conductivity is continuously measured for each addition of Na 2SO4 and are
tabulated. Now the graph is plotted between the volume of Na 2SO4 andconductivity. From the
graph, end point is noted and hence the amount of BaCl 2 present in the given solution is
calculated.

RESULT
The amount of BaCl2 present in the given solution = .................gms

47
 Exp No: 11 Date:

AIM
SYNTHESIS OF ZINC OXIDE NANOPARTICLES USING SOL GEL
METHOD
To synthesize ZnO Nanoparticles using solgel process.

INTRODUCTION
Zinc oxide (ZnO), a wide bandgap (3.4 eV) II-VI compound semiconductor, has a stable wurtzite
structure with lattice spacing a = 0.325 nm and c = 0.521 nm. It has attracted intensive research effort
for its unique properties and versatile applications in transparent electronics, ultraviolet (UV) light
emitters, piezoelectric devices, chemical sensors and spin electronics. Invisible thin film transistors
(TFTs) using ZnO as an active channel have achieved much higher field effect mobility than amorphous
silicon TFTs. Zinc oxide is actually one of the best biofriendly absorbers of UV radiation that mainly
come on Earth from the Sun through the atmospheric ozone layer. A low-temperature method can be
used to produce an eco-friendly, cost-effective ZnO sol-gel that is compatible with a complementary
metal - oxide – semiconductor (CMOs) and integrated – circuits (IC). The sol-gel method is a vacuum
– free, safe, environmentally friendly, economic, easy process and is more versatile.
THEORY
This sol – gel process is a more chemical method (wet chemical method) for the synthesis of various
nanostructures, especially metal oxide nanoparticles. In this method, the molecular precursor (usually
metal alkoxide) is dissolved in water or alcohol and converted to gel by heating and stirring by
hydrolysis/ alcoholysis. Since the gel obtained from the hydrolysis/ alcoholysis process is wet or damp,
it should be dried usingsppropriate methods depending on the desired properties and application of the
gel. The materials obtained from the sol – gel method are used in various optical, elctroni, energy,
surface engineering, biosensors and pharmaceutical and separation technologies. This sol – gel method
is a conventional and industrial method for the synthesis of nanoparticles with different chemical
composition. The basis of the sol – gel method is the production of a homogeneous sol from the
precursors and its conversion into a gel. The solvent in the gel is the removed from the gel structure and
the remaining gel is dried. The properties of the dried gel depend significantly on the drying method.

48
MATERIALS AND EQUIPMENTS REQUIRED

 Zn(CH3CO2)2 H2O (2.1 g per batch)

 Ethanol (100 ml per batch)
49
  Mono Ethanolamine (MEA)
 100 ml Beaker
 500 ml Beaker
 Magnetic pellet
 Funnel
 Filter paper

PROCEDURE

The zinc acetate/ MEA molar ratio equaled 1:1, and the concentration of the ZnO precursor solution
was 0.5 M. The prepared mixture was stirred at 60°C for 2 h to obtain a clear homogeneous solution.
Add 50 ml of ethanol into this solution. A white precipitate will be deposited in the bottom of beaker.
Further, precipitate is dried and collected. Report the yield of this product.

RESULT

A white precipitate of ZnO nanoparticles were synthesized by sol gel method.

50