SRI KRISHNA COLLEGE OF TECHNOLOGY

An Autonomous Institution
(Approved by AICTE and affiliated to Anna University)
Coimbatore, Tamil Nadu
Academic Year 2024-2025

DEPARTMENT OF SCIENCE AND HUMANITIES

PHYSICAL SCIENCE / APPLIED SCIENCE LABORATORY MANUAL

SUBJECT
PHYSICAL SCIENCE /APPLIED SCIENCE LABORATORY

Subject Code: 23PHS02/23PHS04

For FIRST YEAR B.E. STUDENTS

(Common to ALL)

(2024– 2025/Odd & Even)

1
 PREFACE

Welcome to Chemistry Laboratory!!!

The primary audience for this lab manual is first year undergraduate B.E / B.Tech

students. The experiments dealt with here are in accordance with the new syllabus. This

laboratory manual is designed to have students experience how scientists do research so that

they can use scientific knowledge to understand real-world science related issues that will

confront them in their personal, professional and civic lives. To do this, students must

understand how scientists acquire, evaluate and use scientific knowledge, and the implications

and limitations of this knowledge.

Chemistry laboratory deals with the students skills in learning of Physical and chemical

properties with systematic observations. The experiments are explained through the theme,

objective, Formulae with procedure along with tabulation and calculation system with it. Graphs

are attached wherever is applicable.

We wish you all a rewarding, interesting and insightful experience in the Chemistry

Laboratory.

FACULTY OF SCIENCE AND HUMANITIES

SRI KRISHNA COLLEGE OF
TECHNOLOGY
COIMBATORE – 641 042

Prepared by Approved by
Dr.K.R.Kanimozhi
Associate Professor/S&H Head/S&H
2
 PROFILE OF THE INSTITUTION

Nestled at the foothills of the Western Ghats, located in a sprawling

52-acre campus in Kovaipudur, Coimbatore, Sri Krishna College of
Technology (SKCT) is a vibrant institute of higher education established in
1985 promoted by Sri Krishna Institutions. An extraordinary freedom of
opportunity—to explore, to collaborate and to challenge oneself is the
hallmark of the Institute. Being an autonomous institute, affiliated to Anna
University, Chennai, and approved by AICTE, New Delhi, SKCT lays
strong emphasis on collaborative research and stands apart from other
institutes by its participatory work culture, student care programmes and high
industry interaction.
In a span of 40 years, it has emerged as one of the premier
engineering colleges for learning, discovery and innovation due to the
dynamic leadership of the Chairperson and Managing Trustee Smt S
Malarvizhi. Being an acclaimed educationalist, she continues to contribute
profusely for the glory and happiness of advancing generations. The college
is accredited with A Grade by NAAC and eligible undergraduate programs
are accredited by the National Board of Accreditation (NBA), New Delhi. The
college offers 11 undergraduate programmes and 6 postgraduate
programmes in engineering, technology, and Management Studies.

3
 VISION
Sri Krishna College of Technology aspires to be recognized as one of the
pioneers in imparting world class technical education through technology enabled
innovative teaching learning processes with a focus on research activities to cater, to
the societal needs.

MISSION
To be recognized as centre of excellence in science, engineering and technology through
effective teaching and learning processes by providing a conducive learning environment.

To foster research and development with creative and entrepreneurial skills by means of
innovative applications of technology.

DEPARTMENT OF SCIENCE AND HUMANITIES

VISION

The department strives to impart knowledge in basic sciences to

ensure that the student develop computational skills, critical thinking, and
problem solving skills in different engineering disciplines and to enhance their
communication skills to match with the global requirements.

MISSION

 To provide a strong foundation in basic sciences through quality undergraduate

instruction, curricular innovation and experiential learning, upon which students
may build professional careers

 To provide learning ambience to generate innovative and problem solving skills

with professionalism

 To communicate effectively, proficiently and professionally in order to reach the

global standards of business world.

 4
To induce ethical values and spirit of social commitment.
 PROGRAM OUTCOMES

PO 1: Engineering knowledge: Apply the knowledge of mathematics, science,

engineering fundamentals, and an engineering specialization to the solution of
complex engineering problems.
PO 2: Problem analysis: Identify, formulate, review research literature, and
analyze complex engineering problems reaching substantiated conclusions using
first principles of mathematics, natural sciences, and engineering sciences.
PO 3: Design/development of solutions: Design solutions for complex
engineering problems and design system components or processes that meet the
specified needs with appropriate consideration for the public health and safety, and
the cultural, societal, and environmental considerations.
PO 4: Conduct investigations of complex problems: Use research-based
knowledge and research methods including design of experiments, analysis and
interpretation of data, and synthesis of the Information to provide valid conclusions.
PO 5: Modern tool usage: Create, select, and apply appropriate techniques,resources,
and modern engineering and IT tools including prediction and modeling to complex
engineering activities with an understanding of the limitations.
PO 6: The engineer and society: Apply reasoning informed by the contextual
knowledge to assess societal, health, safety, legal and cultural issues and the
consequent responsibilities relevant to the professional engineering practice.
PO 7: Environment and sustainability: Understand the impact of the professional
engineering solutions in societal and environmental contexts, and demonstrate the
knowledge of, and need for sustainable development.
PO 8: Ethics: Apply ethical principles and commit to professional ethics and
responsibilities and norms of the engineering practice.
PO 9: Individual and team work: Function effectively as an individual, and as
a member or leader in diverse teams, and in multidisciplinary settings.
PO 10: Communication: Communicate effectively on complex engineering
activities with the engineering community and with society at large, such as,
being able to comprehend and write effective reports and design
documentation, make effective presentations, and give and receive clear
instructions.
PO 11: Project management and finance: Demonstrate knowledge and
understanding of the engineering and management principles and apply these
to one‘s own work, as a member and leader in a team, to manage projects and
in multidisciplinary environments.
PO 12: Life-long learning: Recognize the need for, and have the preparation
and ability to engage in independent and life-long learning in the broadest
context of technological change.

5
 APPLIED SCIENCE LABORATORY L/T/P/C
23PHSO4 Common to B.E. CSE, IT, ECE, EEE, CSE (CYBER
SECURITY, AI&DS, AIML and IOT) 0/0/4/2

Nature of Course : E (Skill based)

Pre requisites : Basic Applied Science laboratory skills
Course Objectives:
1. To carry out experiments to understand the basic laws of magnetism.
2. To Understand of how objects become electrically charged and how electrical charge
is transferred from one object to another.
3. To understand the principles and applications of electrochemistry and learning electro-
analytical methods, and explore the knowledge of various energy sources and storage
devices.
4. To understand the concepts of photo-physical and photochemical processes in
spectroscopy.
Course Outcomes:
Upon completion of the course, students shall have ability to
CO1 To determine the magnetic field around a current carrying conductor and [E]
Planck’s constant.
CO2 To determine the rate of growth or decay in a resistor -capacitor circuit [E]
and to estimate the resonant frequency and Q-factor.
CO3 To determine the relationship between the magnetic flux density and the [E]
magnetizing field strength and to find the specific resistance of the wire.
CO4 To determine the pH, single electrode potential using reference [E]
electrodes, Strength of acids by conductometric titration and
Electroplating process based on electrolytic cell.
CO5 Interpret the principle and working of Spectroscopic technique. [E]

Lab Components:
1 Determination of Magnetic field along the axis of current carrying coil- [E]
Stewart and Gee method.
2 Determination of characteristics of RC circuit to find the time constant. [E]
3 Determination of characteristics of LCR circuits. [E]
4 Determination of Hysteresis loss. [E]
5 Determine the Specific resistance- Carey fosters bridge [E]
6 Determination of Planck’s Constant. [E]
7 Determination of strength of strong acid by pH metry. [E]
8 Estimation of dissolved oxygen in waste water using Winkler’s method. [E]
9 Determination of single electrode potential of Zinc and Copper by [E]
Potentiometric method.
10 Determination of cathode efficiency of Nickel using electroplating [E]
process.
11 Spectrophotometry-Estimation of iron in sample water. [E]
12 Conductometric titration - mixture of acids (HCl & CH3COOH) Vs NaOH [E]
Life Skills Experiments
13 Determination of pressure required to shut off the fuel pump nozzle. [E]
14 Determination of capacitance required to shut off the circuit in a circuit [E]
breaker.
15 Determination of earth, neutral and phase line in a circuit. [E]
16 To know the presence of dissolved oxygen in given water sample using [E]
glucose by redox principle.
17 To view the colour of the different medium of given water sample using [E]
litmus paper test.
6
 18 To detect the chlorine content in tap water using simple chemical [E]
method.
Total Hours: 36
Text Book:
1 Anoop Sing Yadav “Applied Physics Lab Manual” Vayu Education of India Publisher, 2018.
2 Sesha Sai Kumar Vemula, Manual for Experiments in Engineering Physics, LAP LAMBERT
Academic Publishing 2017
3 C. S. Robinson, Dr. Ruby Das, “A text book of Engineering practical physics”, Laxmi
Publications Pvt. Ltd., 2016.
4 S.L.Gupta and V Kumar “Practical Physics Volume -II”, Pragati Prakashan ., 2023.
5 Method of Sampling and Test (Physical and Chemical) for Water and Wastewater- Iron, 2003,
Part-53; First Revision.
6 Method of Sampling and Test (Physical and Chemical) for Water and Wastewater: pH Value
(2001; Part-50; Coagulation Test).
7 Method of Sampling and Test (Physical and Chemical) for Water and Wastewater, Chemical
Oxygen Demand, 2012, Part-58.
8 Science and Technology Laboratory Manual. E-Book. NIOS, 2012.
References:
1 Dr. Ruby Das and Prashant Kumar Sahu,A Textbook of Engineering Physics Practical ,
2016,2nd Edition
2 S. L. Gupta and Dr. V. Kumar, “Practical physics with viva voice”, Pragati Prakashan
Publishers, Revised Edition, 2009.
3 M. N. Avadhanulu, A. A. Dani and Pokely P.M, “Experiments in Engineering Physics”, S.
Chand&Co,2008.
4 Sawyer, C. N., McCarty, P. L., and Parkin, G. F. 2017. Chemistry for Environmental
Engineering. Fifth Edition, McGraw-Hill, Inc., New York.
5 American Public Health Association et al, Standard Methods for the Examinations of Water and
Waste Water, APHA. 2017.
6 AWWA, WEF, APHA, 2017, Standard Methods for the Examination of Water and Wastewater
(Method: 5210B, BOD).
Web References – Simulation Links / Animation Videos
1 https://vlab.amrita.edu/?sub=1&brch=192&sim=972&cnt=4
2 https://www.plexim.com/academy/analog-electronics/rc-time-constant
3 https://phet.colorado.edu/sims/html/circuit-construction-kit-ac/latest/circuit-construction-kit-
ac_all.html
4 https://www.allaboutcircuits.com/technical-articles/hysteresis-loss-estimation-modeling-and-
the-steinmetz-equation/
5 https://bop-iitk.vlabs.ac.in/exp/carey-foster-bridge/simulation.html
6 https://mpv-au.vlabs.ac.in/modern-physics/Determination_of_Plancks_Constant/
experiment.html
7 https://ee1-nitk.vlabs.ac.in/exp/determination-of-ph/simulation.html
8 https://ee1-nitk.vlabs.ac.in/exp/determination-of-biological-oxygen/simulation.html
9 https://www.youtube.com/watch?v=opSUkbaR2Sc
10 https://mm-coep.vlabs.ac.in/exp/electrochemical-machining-process/simulation.html
11 https://ee1-nitk.vlabs.ac.in/exp/determination-of-total-iron/simulation.html
12 https://www.youtube.com/watch?v=e_uFXjU9v7o
Continuous
Assessment End
Total
Semester
Total Examinati
Formati Summative
Total Continuou on
ve Assessment
Assess s
ment Assessme
nt

7
75 25 100 60 40 100

Assessment based on Continuous and End Semester Examination

Continuous
Assessmen
t (60%) End Semester
Practical
[100 Marks]
Examination (40%)
Bloom’s
Level FA SA [100 Marks]
(75 Marks) (25 Marks)

Remember 0 0 0
Understand 10 10 10
Apply 30 30 30
Analyze 30 30 30
Evaluate 30 30 30
Create 0 0 0

Mapping of Course Outcomes (CO) with Programme Outcomes (PO) Programme

Specific Outcomes (PSO)
P
COs O PSOs
s
1 2 3 4 5 6 7 8 9 10 11 12 1 2 3
CO1 3 2 1 2 2 1 1
CO2 1 2 2 1 1
3 2
CO3 3 2 1 2 2 1 1
CO4 3 2 1 2 2 1 1
CO5 3 2 1 2 2 1 1

Strongly Moderately Reasonably

3 2 1
agreed agreed agreed

8
OBJECTIVES

 To determine the pH of the test solution.

 To estimate the amount of dissolved oxygen present in the given water sample.

 To determine the single electrode potential of Zinc and Copper by the given solution.

 To determine the cathode efficiency of nickel plating.

 To determine the amount of iron content of an unknown solution by

spectrophotometry.
 To determine the strength of strong and weak acids (HCl and
CH3COOH) by conductometric titration using NaOH.

OVER AND ABOVE SYLLABUS

 To know the presence of dissolved oxygen in given water sample using

glucose by redox principle.
 To view the colour of the different medium of given water sample using litmus
paper test.
 To detect the chlorine content in tap water using simple chemical method.

9
REQUIRED LABORATORY MATERIALS
 Applied Science/Physical Science Laboratory manual
 A scientific electronic calculator and other writing tools.

GENERAL RULES OF LABORATORY SAFETY

 The chemicals used in this laboratory are likely to be corrosive and/or toxic. Avoid
skin contact with any of these chemicals. If contact does occur; consciously wash the

area of contact with water.

 Do not perform any unauthorized experiments.

 Students at this level must not work alone in this laboratory. 

 Adequate foot covering is requiring at all times. Do not wear sandals. Do not come to
the laboratory with bare feet.

 Cold and hot objects often look the same. Remember always to exercise caution when
picking up laboratory glassware and tools. 

 Always notify the instructor in case of an injury.

 As for the disposal of waste chemicals, when in doubt ask the instructor.

 If you spill any reagents, clean them up immediately. If necessary, rinse well with
water.

 Keep your desk and reagent table clean and tidy at all times. At the end of the
experiments, clean the apparatus and table. Return the reagent bottle to the lab

assistant.

 Dispose the solid waste in waste baskets. Do not put them in the sink.

 If you break any glassware or equipment’s, immediately inform the lab assistant.

 Do not place bags or books on the lab benches. Keep them on the shelves provided for
this purpose.

10
LIST OF EXPERIMENTS

S. No. Title of the Experiment Page

No.
1 Determination of strength of strong acid by pH-metry. 16

2 Determination of dissolved oxygen present in given waste water sample

22
using Winkler’s titrimetric method.
3 Determination of single electrode potential of Zinc and Copper by
30
Potentiometric method.
4 Determination of cathode efficiency by electroplating of nickel. 33

5 Estimation of iron in water by spectrophotometry. 44

6 Conductometric titration - mixture of acids (HCl & CH3COOH) Vs NaOH 50

Virtual Labs – Simulation Experiments

Note: Understanding the concepts by simple demonstrations
To know the presence of dissolved oxygen in given water sample using
7 56
glucose by
redox principle.
To view the color of the different medium of given water sample using
8 57
litmus
paper test.
9 To detect the chlorine content in tap water using simple chemical test. 58

11
12
 6
5
4
3
2
1
No
Exp.
Date
Title of the Experiment

Preparation and Understanding (10

13
marks)

Experimental Setup(20 marks)

Table of Contents

Execution of the experiment (30

marks)

Calculation (10), Viva (10)

and result* (10) – 30 marks
Observation Marks

Documentation (10 marks)

Total (100)
of
Signature

the faculty
 Total marks =

14
 Table: Volume of NaOH Vs pH

Sl. No Volume of NaOH (ml) pH

1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20

Model Graph: Volume of NaOH Vs pH

Exp. No.: Date:

DETERMINATION OF STRENGTH OF STRONG ACID BY pH METRY

AIM
To determine the strength of given hydrochloric acid by pH metry. You are provided
with a standard solution of NaOH of strength 0.2 N.

MATERIALS REQUIRED
pH Meter, Combined glass electrode, 100ml beaker, Burette, Pipette, glass rod, HCl,
NaOH solution.

PRINCIPLE
All pH meters have provision for standardizing the glass electrode in a buffer solution
of known pH. This is necessary because different electrodes have different asymmetry
potentials. Once the adjustment has been made, so that the meter registers correctly the
known pH of the buffer solution, the instrument gives the pH of other solution without any
calculation.

Measurements of pH are also employed to monitor the course of acid base titrations.
The pH values of the solution at different stages of acid base neutralization are determined
and are plotted against the volumes of the acid / alkali added. On adding a base to an acid, the
 1 
pH rises slowly in the initial stages pH  log   , and then it changes rapidly at the end

 (H ) 

point. Then it flattens out. The end point of the titration can be detected where the pH
changes most rapidly. However, the shape of the inflexion point (i.e., where the pH changes
abruptly) and symmetry of the curve on its two sides, depends upon the ionisability of the
acid and the base used and on the basicity of the acid. Since the pH of the solution is related
to the H+ ion concentration given by pH = - log[H+] measurement of pH of the solution gives
the concentration of H+ ions in the solution. When NaOH is added slowly from the burette to
the solution of HCl, the fast-moving H+ ions are progressively replaced by slow moving Na+
ions. As a result, pH of the solution increases.

H+ + Cl- + Na+ + OH- NaCl + H2O

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

 pH/V

Volume of NaOH

Differential Graph: Volume of NaOH Vs pH / V

 The increase in pH takes place until all the H+ ions are completely neutralized (upto
the end point) after the end point, further addition of NaOH increases pH sharply as there is
an excess of fast moving OH- ions.

PROCEDURE

Standardize the electrode in a buffer solution of known pH. The burette is filled with
Std. NaOH solution. Exactly 20 ml of the given HCl solution is pipetted out into a clean
beaker. It is then diluted by adding 20 ml of distilled water. The glass electrode is dipped in it
and connected with a pH meter.

Now NaOH solution is gradually added at the intervals of 1ml from the burette to the
HCl solution taken in the beaker and pH of the solution is noted for each addition. This
process is continued until at least 5 readings are taken after the endpoint. The observed pH
values are plotted against the volume of NaOH added. From the S graph and the differential
graph, the end point is noted.
CALCULATION

Volume of NaOH V1 = ……………. ml (titre value)

Normality of NaOH N1 = ……………. N

Volume of HCl V2 = 20 ml

Normality of HCl N2 = ?

................ ml  0.2
Normality of HCl N2 =
20

Estimation of HCl

Amount of HCl present in 1000 ml = Normality x Equivalent weight

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

= g.

100
Amount of HCl present in the given solution = 
1000

=........................g
RESULT

1. The strength of HCl present in one litre of the given solution = ........................ N

2. The amount of HCl present in one litre of the given solution = ........................ g
REVIEW QUESTIONS

1. What does a pH meter actually measure?

2. What are the electrodes used in pH meter?

3. How do you make sure that the pH meter works well and the readings are accurate one?

4. How is a glass electrode constructed?

5. What is meant by ionic product of water?

Exp. No.: Date:

DETERMINATION OF DISSOLVED OXYGEN IN WASTE WATER USING

WINKLER’S TITRIMETRY METHOD
AIM

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

CHEMICALS REQUIRED
Potassium dichromate, Sodium thio-sulphate, Potassium iodide, Starch, Sulphuric
acid, Manganous sulphate.

PRINCIPLE

The amount of dissolved oxygen in water is estimated using Winkler’s reagent

(manganous sulphate, alkali – iodide, concentrated sulphuric acid.) Water sample is collected
carefully in iodine flask (to avoid aeration or deaeration). Initially manganous sulphate and
alkali – iodide reagents are added to the iodine flask and the following reactions will occurs,
Mn2+ + 2OH- Mn(OH)2 (White)

2Mn(OH)2 + ½ O2 + H2O MnO(OH)2 (Yellow brown)

The precipitate is dissolved 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

2Na2S2O3 + I2 Na2S4O6 + 2NaI

PROCEDURE

TITRATION – I

STANDARDISATION OF SODIUM THIOSULPHATE

The burette is washed and rinsed with sodium thiosulphate solution. Then the burette
is filled with the given sodium thiosulphate solution. 20 ml of 0.01 N potassium dichromate
solutions is pipetted out into a clean conical flask. To this, 5 ml of dil. sulphuric acid and 10
ml of 10 % potassium iodide are added and titrated against sodium thiosulphate solution.
When the solution becomes straw yellow in colour, 1 ml of starch indicator is added and then
the titration is continued. The end point is change of dark blue colour to pale green colour.
The titration is repeated until concordant value is obtained.

TITRATION – II

ESTIMATION OF DISSOLVED OXYGEN

300 ml of the water sample is taken in the BOD bottle, 2 ml of manganese sulphate
and 2 ml of alkali – iodide is added. The stopper is replaced and the flask is inverted and
shaken several times for the through mixing of reagents. The flask is left aside for some time.
When half of the precipitate settles down, the stopper is removed and 2 ml of concentrated
sulphuric acid is added.

The stopper is replaced and the flask is inverted several times for complete dissolution of
the precipitate. 203 ml of this solution is taken in conical flask titrated against standardized
sodium thiosulphate solution. 1 ml of starch indicator is added when the solution becomes
light yellow. 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 can be calculated.
TITRATION1: STANDARDISATION OF SODIUM THIOSULPHATE

Burette solution : Sodium thiosulphate

Pipette solution : Potassium dichromate
Reagents added : 10ml of KI+5ml of dil H2SO4
Indicator : Starch
End Point : Colour change from blue to green

Potassium Dichromate Vs. Sodium Thiosulphate

S.No. Volume of Burette Reading (ml) Volume of Concordant

Potassium Sodium Value (ml)
dichromate Initial Final Thiosulphate
(ml) (ml)
1 20 0
2 20 0
3 20 0

CALCULATION

Volume of potassium dichromate V1 = 20 ml

Strength of potassium dichromate N1 = 0 .025 N

Volume of sodium thiosulphate V2 = .…….…. ml (Titre Value)

Strength of sodium thiosulphate N2 = ?

V1N1 = V2N2

V1N1
N2 =
V2
20X 0.025N
Strength of sodium thiosulphate N2 =
........

N2 = ……… N
TITRATION – II: ESTIMATION OF DISSOLVED OXYGEN

Burette solution : Sodium thiosulphate

Pipette solution : water sample
Reagents added : 2 ml Mn(SO4)2 + 2 ml alkali iodide
Indicator : Starch
End Point : Disappearance of blue colour

Water Sample Vs Sodium Thiosulphate

S. Volume of Burette Reading Volume of Concordant Indicator

No. water (ml) Sodium value (ml)
sample Initial Final thiosulphate
(ml) (ml) (ml) (ml)

1 203 0 STARCH

CALCULATION

Volume of Sodium thiosulphate V1 = ml (Titre Value)

Normality of Sodium thiosulphate N1 = N

Volume of water sample V2 = 203 ml

Normality of water sample (or) N2 = ?

Normality of dissolved oxygen in water
............... ml  ........... N
=
203
= ….. ……… N

Amount of dissolved oxygen = ………… N X 8 X 1000 ppm

Present in one litre of tap water
= ppm
REVIEW QUESTIONS

1. What is Winkler’s method?

2. What is the purpose of adding MnSO₄?

3. What is the indicator used? Why?

4. Why starch is added at the end of the titration?

5. What is the equivalent weight of oxygen?

RESULT

The amount of dissolved oxygen present in the given water sample is = .................... ppm
Calculation

1. Zinc-Calomel cell

Zn / Zn++ // Hg2Cl2 : KCl (satd.) Hg at 250C

Ecell = Ezn (OP) + Ecalomel (RP)

Ecalomel (RP) = 0.2422 V

Ezn = Ecell - Ecalomel (RP)

2. For Copper -Calomel cell,

Hg / Hg2Cl2 : KCl (satd.) Cu++/Cu at 250C

Ecell = Ecalomel (OP) + ECu (RP)

Ecalomel (OP) = 0.2422 V

ECu = Ecell - Ecalomel (OP)

Exp. No.: Date:

DETERMINATION OF SINGLE ELECTRODE POTENTIAL OF AN

ELECTRODE
AIM
To determine the single electrode potential of zinc and copper in different
concentration solution by potentiometric method.

MATERIALS REQUIRED
Potentiometer, Calomel electrode, Zinc electrode, Copper electrode, Graduated
pipette, glass rod, 100 ml volumetric standard flask.

PRINCIPLE

A metal in contact with its electrolyte forms an electrode and develops a potential.
This is called single electrode potential. The absolute value of this cannot be determined. But
this can be combined with a standard electrode like standard hydrogen electrode or with a
reference electrode like calomel electrode and an electrochemical cell is formed. The
potential difference of this cell is determined from which the single electrode potential is
computed.

PROCEDURE:

1. 1 Molar solution of ZnSO4 and CuSO4 is prepared separately.

2. Zinc electrode is dipped in ZnSO4 solutions.

3. A calomel electrode is also immersed in the same solution.

4. The calomel electrode is connected to the positive and zinc electrode to the negative
terminal of the potentiometer. The potential of the cell is noted down. From the emf
of the cell, the potential of zinc electrode is calculated, since the potential of calomel
electrode is known.
 Sl. No Molarity Copper (V) Zinc (V)

1 1M

2 0.1 M

3 0.01 M

Calculation:
 5. 1molar ZnSO4 solution is diluted 10 times. From this, 10 ml of ZnSO 4 is pipetted out
into a 100 ml standard flask and made up to the mark with deionized water. Taking
this solution, in zinc half-cell, the emf is measured again. ZnSO4 is further diluted to
0.01M and the potential is found out as before. This effect of change of concentration
on potential is determined.

6. Copper rod and calomel electrode are dipped in 1M CuSO4 solution.

7. The two electrodes are connected to potentiometer, Cu to positive and calomel to

negative terminals. The potential is read.

8. The copper sulphate solution is prepared in different concentration, 0.1 and 0.01 by
dilution.

9. The diluted solutions are taken in copper half-cell, one by one and the potential of the
cell is measured. Knowing the potential of calomel electrode, the potential of copper
electrode is calculated.

10. The effect of change of concentration on the potential of copper electrode is also
found out.

RESULT

The Potential of the given copper electrode at different concentrations of the electrolyte:

i) For 1M V
ii) For 0.1M V
iii) For 0.01M V

The Potential of the given zinc electrode at different concentrations of the electrolyte:

i) For 1M V
ii) For 0.1M V
iii) For 0.01M V
REVIEW QUESTIONS

1. What is single electrode potential?

2. Define the term standard single potential.

3. What are factors affecting the electrode potential?

4. Define the term EMF series.

5. What does a pH meter actually measure?

Exp. No.: Date:

ELECTROPLATING OF NICKEL AND DETERMINATION OF CATHODE

EFFICIENCY

AIM:
To determine the cathode efficiency of nickel plating.

APPARATUS REQUIRED
DC power supply, beaker, copper plate, nickel plate.

PRINCIPLES AND FUNDAMENTALS:

Electroplating is a widely used metal finishing process to coat a single metal or an

alloy on a conducting substrate. The object to be plated is made as cathode by connecting it to
the negative terminal of the power supply. The plating takes place due to the reduction of
metal ions from the bath solution
Mn+ + ne- M

The other electrode, which is connected to the positive terminal becomes the anode
and undergoes dissolution

M Mn+ + ne-

The soluble anode replenishes the ions into the bath solution.

The deposition process obeys Faraday’s law. The quantity of metal deposited at the
cathode and the quantity that is dissolved from the anode are directly proportional to the
coulombs of electricity passed. To operate the electroplating processes, the following
components and regents are required.

Electrically conducting cathode (the article or job)

Electrically conducting anode

An inert vessel

A regulatable D.C power source

(i) Bath components

The bath contains highly soluble salts (electrolytes) of a desired metal to be plated.
Electrolytes are also essential for the conductivity of the bath and the buffers are needed to
control the pH at the desired range. Some complexing agents are also added to keep the
deposition at more negative potentials.

For example, according to the emf series, iron is more active than copper and hence
when iron is in contact with a copper solution, there would be a spontaneous plating of
copper on the iron articles. Such coatings are very poor, ununiform and would readily peel
away. To overcome this trouble, the complexing agents such as cyanides, hydroxides, and
sulphonates are added which would polarize the deposition potential and ensures that the
plating takes place only during the electrolysis. To obtain desired structural morphological
coatings, a wide range of organic compounds are added as additives in low concentrations.

(ii) Mechanisms of plating:

The deposition mechanism has two distinct stages. At the start of the process, the
deposition of the metal occurs on the electrode surface and initiates nucleation. Then, the
electrode is fully covered by a few atomic layers of the deposited metal, the layer thickens
with macroscopic deposits. The quality of an electrodeposited finish is dependent upon a
wide range of process variables such as electrolyte compositions, additives, pH, temperature,
current density, electrode-cell geometry and flow conditions.

(iv) Surface pretreatment and plating:

In any electrochemical processes, the surface pretreatment of the object is very

important. For electroplating, the following operations are carried out during surface
pretreatment.

Mechanical cleaning by wire

brushing or sand blasting or Rinsing Pickling Washing
emery sheet cleaning to remove in water
surface impurities.

Drying and weighing. Degreasing in

organic solvents.

Flow chart for surface preparation job

Calculations:

Plate I: (Current Density = A/dm2)

Calculation of area of the plate in dm2 and current

Weight of copper plate before nickel deposition (W1) = g

Weight of copper plate after nickel deposition (W2 ) = g

Weight of nickel deposited (W2 ─ W1) = g

Theoretical weight of nickel deposited as per

Faraday’s first law = ZIt

= 0.3041x 10-3 x I x 900.

= g

Actual weight deposited

Cathode efficiency of nickel plating = -----------------------------
X100
Theoretical weight

= %
 After the surface preparation, the cleaned metal is electroplated by keeping it as the
cathode in between two suitable anodes. In the laboratory, nickel is plated on a metal strip

using Watt’s bath of the following compositions

Nickel sulphate – 240 g/lit

Nickel Chloride – 60 g/lit

Boric acid – 30 g/lit

The actual weight of nickel deposited at a particular current density and for specified
time duration is determined by reweighing the plate and noting the gain in weight. The
theoretical weight of nickel ought to be deposited is calculated using Faraday’s first law of
electrolysis.
m = ZIt

Where, Z = Electrochemical equivalent of Nickel, I = Current in Ampere and t = time in

seconds.

Note:
Eq. weight of nickel
Electrochemical equivalent of Nickel (Z) = --------------------------
F

= 29.345 / 96,500

= 0.3041 X10-3 g/coulombs.

The efficiency of nickel plating is = Actual weight

X 100
Theoretical weight

38
Calculations:

Plate II: (Current Density = A/dm2)

Calculation of area of the plate in dm2 and current

Weight of copper plate before nickel deposition (W1) = g

Weight of copper plate after nickel deposition (W2 ) = g

Weight of nickel deposited (W2 ─ W1) = g

Theoretical weight of nickel deposited as per

Faraday’s first law = ZIt

= 0.3041x 10-3 x I x 900.

= g

Actual weight deposited

Cathode efficiency of nickel plating = -----------------------------
X100
Theoretical weight

= %

39
PROCEDURE:

A strip of copper or brass plate is cleaned by following the above-mentioned sequence

(Flow chart) and weighed (W1). A convenient area is marked on the plate, and the current to
be supplied for the given current density rating is calculated. The prepared strip is kept as the
cathode in the Watt’s bath such that the marked area is immersed in the bath and two well
cleaned nickel sheets are used as anodes and placed on both the sides of the cathode. Definite
ampere of current is passed through the cell for 15 min. The plate is then removed, washed,
dried and weighed (W2). From the weight of nickel deposited (W2-W1), the cathode
efficiency of nickel plating is calculated. The experiment is simultaneously carried out for
two more samples at different current densities.

40
Calculations:
Plate III: (Current Density = A/dm2)

Calculation of area of the plate in dm2 and current

Weight of copper plate before nickel deposition (W1) = g

Weight of copper plate after nickel deposition (W2 ) = g

Weight of nickel deposited (W2 ─ W1) = g

Theoretical weight of nickel deposited as per

Faraday’s first law = ZIt

= 0.3041x 10-3 x I x 900.

= g

Actual weight deposited

Cathode efficiency of nickel plating = -----------------------------
X100
Theoretical weight

= %

41
RESULT:

i) The cathode efficiency of nickel plating at a current density of A/dm2 is

%

ii) The cathode efficiency of nickel plating at a current density of A/dm2 is

%

iii) The cathode efficiency of nickel plating at a current density of A/dm2 is

%

42
REVIEW QUESTIONS

1. State Faraday’s first law of electrolysis.

2. If you were to use soluble anode in the electroplating processes, then would you expect
any change in the metal ion concentration of the bath?

3. The pH is known to change during electroplating. What are pH buffers?

4. Are additives really needed in industrial electroplating? If yes, state the reasons.

5. Can you identify the electroplated components used in the automotive and electronic
industries?

6. Write the general anodic and cathodic reactions during electroplating.

7. How do you plate metals on articles without electricity?

43
Exp. No.: Date:

ESTIMATION OF IRON IN WATER BY SPECTROPHOTOMETRY

AIM

To estimate the amount of iron present in a given samples of water using

spectrophotometer.

MATERIALS REQUIRED

Spectrophotometer, Ferrous ammonium sulfate solution, KMnO4, H2SO4, HNO3,

KSCN, Volumetric standard flask 100ml, Cuvettes, Graduate pipette.

PRINCIPLE
I0
log  ct
It
I0
log A
It

Where, A = ct
I0 = Intensity of incident light
It = Intensity of transmitted light
C = Concentration of solution
t = Thickness of the cell
 = Molar absorption co – efficient

Fe3+ + 6 SCN- [Fe (SCN)6]3-

Beer – Lambert’s Law

The intensity of a beam of monochromatic light decreases exponentially as the

concentration of the absorbing substance in solution and the thickness increases
independently. The law can be written in the form of mathematical equation

I0
A = log  ct
It

44
 LAYOUT OF SPECTROPHOTOMETER

AC Power
Choose max Photomultiplier tube

Source Monochromator Sample cell Detector

(Diffraction grating) l = 1cm

Amplifier

Out put
OBSERVATION:
λmax = 480 nm

1 ml = 1 mg/l of iron (Ferric ion, Fe3+)

Preparation of various concentration of Iron solution

VOLUME VOLUME VOLUME VOLUME FINAL CONCENTRATION

OF IRON OF 10% OF 10% OF VOLUME OF IRON
S.No. SOLUTION HNO3 KCNS WATER (ml) SOLUTION (mg/l)
(ml) (ml) (ml) (ml)

1. 2 1 1 6 10 2

2. 4 1 1 4 10 4

3. 6 1 1 2 10 6

4. 8 1 1 0 10 8

5. Unknown 1 1 x 10 --

45
Keeping path length constant say t, the variation is with reference to only concentration,

It = I0 l0-ct

Fe3+ ions do not give any colour in solution. However, a red colour can be produced,
when it reacts with potassium thiocyanate solution and complementary for this colour will be
in the blue region ( = 480nm). So in the spectrophotometer, this radiation is allowed to pass
through the solution. The spectrophotometer will measure the incident radiation, and the
transmitted radiation. To measure I0, a blank solution (without Fe3+) is taken and the
transmitted light will be measured. Its absorbance is measured for various concentrations; a
calibration graph can be drawn with absorbance Vs Concentration.

PROCEDURE

The spectrophotometer is switched on and warmed up for 10 minutes. The

wavelength is adjusted for  = 480 nm. Blank solution is kept in the cell and transmittance
(I0) is measured. Usually, the instrument is calibrated for I 0 = 100, for which absorbance is
zero. This solution is kept whose concentration is known and the absorbance is measured.
Similarly various known concentration of iron solution (2, 4, 6, 8, 10 ml) after adding nitric
acid and thiocyanate solution, are kept in the instrument one by one and absorbance is
measured in each case. A calibration graph is drawn by plotting absorbance against
concentration.

Now, the unknown solution treated with nitric acid and thiocyanate is kept in
photometer and the absorbance is measured. From the absorbance measured, the
concentration of the unknown solution is obtained from the calibration graph.

46
S.No CONCENTRATION
OF IRON SOLUTION
ABSORBANCE (OD) TRANSMITTANCE (%)
(ml)
(1 ml = 1 mg/l of Fe3+)

1. 2

2. 4

3. 6

4. 8

5. Unknown

47
RESULT

The amount of iron present in a given sample of water = ..................... mg/l

48
MODEL GRAPH

49
 CONDUCTOMETRIC TITRATION OF MIXTURE OF
ACIDS (HCl & CH3COOH)

Exp.No: Date:
AIM
To determine the amount of a strong acid and a weak acid (HCl and CH 3COOH) present in one litre of the
given mixture of acid solution by Conductometric titration using standard NaOH of 0.1 N
APPARATUS REGUIRED

Conductivity meter, Conductivity cell, Burette, Beaker ,Glass rod

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

HCl + NaOH NaCl + H2O (Ist neutralization)

After the complete neutralization of all HCl, the neutralization of CH 3COOH starts,

CH3COOH+ NaOH CH3COONa + H2O (IInd neutralization)

Since CH3COOHNa is stronger electrolyte than CH3COOH, conductivity slowly increases until all
CH3COOH is completely neutralized. When the end jpoint is reached, addition of NaOH will cause sudden
increase in the conductance. This is due to the presence of fast moving OH - ions.

50
TITRATION OF MIXTURE (HCl + CH3COOH) Vs NaOH
S.No. Volume of NaOH (ml) Conductance Ω -1

10

11

12

13

14

15

16

17

18

19

20

21

22

51
PROCEDURE
The burette is washed well with water and rinsed with the given standard NaOH solution. It is then filled

with NaOH solution upto the zero level. 20 ml of the given mixture of acids (HCl + CH 3COOH) is pipette

out into a clean 100ml beaker. The conductivity cell is placed in it and then diluted to 50 ml by adding

conductivity water, so that the electrodes are well immersed in the solution. The two terminals of the cell

are connected with a conductivity bridge. Now 1 ml of NaOH from the burette is added to the solution,

taken in the beaker, stirred for some time and then conductivity is measured. (The conductivity is going on

decreasing upto the end point). This process is repeated until at least five readings are taken after the end

point (A) has been reached.

After the end point, again NaOH is gradually added, which causes increase in conductance. This increase in

conductance is observed until the end point (B) is reached. After the second end point, sudden increase in

conductance is observed on further addition of NaOH. The reading (conductivity) is continuously measured

for each addition of NaOH and are tabulated. Now the graph is plotted between the volume of NaOH Vs

conductivity. From the graph the first end point (A) and the second end point (B) are noted. From the end

points the amount of HCl and CH3COOH present in 1 litre of the mixture of solution is calculated.

52
STEP I
CALCULATION OF STRENGTH OF HCl
Volume of the mixture (HCl), V1 = 40 ml
Strength of the mixture (HCl), N1 = …………..?
Volume of the NaOH, V2 = …………………….. (A) ml
Strength of the NaOH, N2 = 0.2 N
According to the law of volumetric analysis, V1N1 = V2N2
N1=V2N2/V1
=………………ml x 0.2 N/40
CALCULATION OF AMOUNT OF HCl
The amount of HCl present in 1000 ml of the
given solution = strength of HCl x Eq. wt of HCl
=…………….. N x 36.5
=…………….. gms
STEP II
CALCULATION OF STRENGTH OF CH3COOH
Volume of the mixture (CH3COOH), V1 = 40 ml
Strength of the mixture (CH3COOH), N1 = …………..?
Volume of the NaOH, V2 = …………………….. (B) ml
Strength of the NaOH, N2 = 0.2 N
According to the law of volumetric analysis, V1N1 = V2N2
N1 =V2N2/V1
=………………ml x 0.2 N/40

CALCULATION OF STRENGTH OF CH3COOH

The amount of CH3COOH present in
1000 ml of the given solution = strength of CH3COOH x Eq.wt. of CH3COOH
=……………………..N x 60
=……………………..gms

53
REVIEW QUESTIONS

1. What is conductance?

2. What is the unit of conductance?

3. What are the factors that affect conductivity of a solution?

4. What is a cell?

5. What is the principle involved in conductometric titration?

6. What are the advantages of conductometric titration?

7. Give an example for strong and weak acid?

RESULT

The amount of HCl present in 1 litre of the given solution = ………….. gms

The amount of CH3COOH present in 1 litre of the given solution = ……………. gms

54
 VIRTUAL LAB – SIMULATION LINKS / ANIMATED VIDEOS

LINKS

https://ee1-nitk.vlabs.ac.in/exp/determination-of-ph/simulation.html

https://ee1-nitk.vlabs.ac.in/exp/determination-of-biological-
oxygen/simulation.html

https://www.youtube.com/watch?v=opSUkbaR2Sc

https://mm-coep.vlabs.ac.in/exp/electrochemical-machining-
process/simulation.html

https://ee1-nitk.vlabs.ac.in/exp/determination-of-total- iron/simulation.html

https://www.youtube.com/watch?v=e_uFXjU9v7o

55
 UNDERSTANDING THE CONCEPTS BY SIMPLE DEMONSTRATIONS

Demonstration-1

Aim

To know the presence of dissolved oxygen in given water sample using glucose by redox
principle
\

Ingredients
 Glucose
 Sodium Hydroxide
 Methylene Blue

Principle

Glucose (an aldehyde) in an alkaline solution is slowly oxidized by dissolved oxygen,

forming gluconic acid. In the presence of sodium hydroxide, gluconic acid is converted to
sodium gluconate. Methylene blue speeds up the reaction, acting as an oxygen transfer agent.
By oxidizing glucose methylene blue, itself is reduced and becomes colorless (formation of
leucomethylene blue). The indicator here is reduced by the glucose in the presence of base
which is thereby oxidized by the fresh dioxygen – redox process.

Procedure

 Take two one litre Erlenmeyer flasks filled with tap water. 2.5 g of glucose are dissolved
in one of the flasks (A) and 5 g of glucose are dissolved in another flask (B).
 Just prior to that, add 2.5 g of sodium hydroxide in flask A and 5 g in flask B.
 Add approximately 1 ml of 0.1% solution of methylene blue into each flask. Stoppered
the flask and shaken to dissolve the dye.
 Set aside the flask.

Observation

 The blue colour of the solutions gradually disappears as glucose is oxidized by the
dissolved oxygen.
 It is noted that the flask having twice the glucose concentration uses the dissolved
oxygen in about half the time and the colour change is quick than the other flask.

56
Demonstration-2

Aim
To view the color of the different medium of given water sample using litmus paper test

Ingredients
 PH paper
 Acidic water (Lime juice)
 Soft water
 Basic water (Bleaching solutions, antacids etc)

Principle

The measure of the hydrogen ion concentration (pH) of the water as ranked on a
scale of 1.0 to 14.0. The lower the pH of water, the more acidic it is. The higher the pH of
water, the more basic, or alkaline

Procedure
 Dip the pH test strip into the water
 Observe the colour of the pH test strip

Observation

pH range Description Colour of pH test strip

0-3 Strong acid Red
3–6 Weak acid Orange or yellow
7 Neutral Green
8–11 Weak base Blue
> 11 Strong base Violet or Indigo

57
Demonstration-3
Aim
To detect the chlorine content in tap water using simple chemical method
Ingredients
 o-Tolidine 1.0gm
 Hydrochloric acid 100 mL
 Distilled water 900 mL

Principle
A solution of o-Tolidine in hydrochloric acid reacts with active chlorine
present in water to form a yellow product. This test is applicable to water that have
been treated with chlorine or hypochlorite such as potable water, swimming pools
or condenser water where the residual (free) chlorine range between 0-2ppm. At a
pH less than 4, chlorine develops a colour with o-Tolidine reagent, varying from pale
yellow at low concentration to dark yellow at higher concentration.

Procedure
 Add 1ml of o-Tolidine reagent to100 mL of the sample and mix thoroughly.
 Allow the sample to stay in dark for 5-15minutes for the colour to develop if
the sample is free of chloramine and nitrite and iron are each less than 0.3
ppm. If chloramine is present, allow it to stand for full 15 minutes.
 If the sample is highly alkaline, it may give blue-green colour instead of
yellow. Add 1mLof 1:4 hydrochloric acid to reduce the pH to 4 or less.

Observation
 Compare the colour produced with that of standard colour comparison chart.
 Match the correct colour and report as ppm of chloride.

58
59