A Laboratory Manual for

Chemistry
(3110001)

B.E. Semester -1/2 (Chemistry)

Common lab manual for all Govt. Engineering colleges (CTE, Gandhinagar)

Prepared by

1. Dr. Bhadreshkumar Sudani, GEC Valsad

2. Dr. Shashi Ranga, GEC, Valsad
 Certificate

This is to certify that Mr./Ms. ___________________________________

________ Enrollment No. _______________ of B.E. Semester _____ of
Chemical Engineering department of this Institute (GTU Code: _____ ) has
satisfactorily completed the Practical / Tutorial work for the subject Chemistry
(3110001) for the academic year …...

Place: __________
Date: __________

Name and Sign of Faculty member

Head of the Department

Chemistry (3110001)

Preface

Laboratory manual for the subject of “Chemistry-3110001” is intended for the use of first
year B.E. students. The main objective of the Chemistry Laboratory Manual is to furnish the
conceptual understanding of the basic principles of chemical science and engineering and related
analysis involved for the students to carry out laboratory experiments.

As experimental work is the heart of the engineering teaching learning process,

laboratory/practical/field work is for enhancing required skills as well as creating ability amongst
students to solve real time problems by developing relevant competencies in the psychomotor
domain. GTU has designed competency focused outcome-based curriculum for engineering
degree programs where sufficient weightage is given to practical work. It shows the importance
of enhancement of skills amongst the students and it pays attention to utilize every second of time
allotted for practical amongst students, instructors and faculty members to achieve relevant
outcomes by performing the experiments rather than having merely study type experiments. It is
essential for effective implementation of competency focused outcome-based curriculum that
every practical is keenly designed to serve as a tool to develop and enhance relevant competency
required by the various industries among every student. These psychomotor skills are very
difficult to develop through traditional chalk and board content delivery methods in the
classroom.
This manual is the foundation of certain basic concepts and skills that can be repeatedly
employed by the students in their future endeavors in and out industries. It is written as per the
new syllabus prescribed by the Gujarat Technological University in a simple language. Hence we
hope this book serves the students better with all details of experiments as per their syllabus.

The main aim of this book (manual) is to develop the habit of scientific reasoning and
providing answers to all the doubts that arise during the course of conducting experiments.
Utmost care has been taken while preparing this laboratory manual however there are chances of
improvement. Therefore, we welcome constructive suggestions for improvement and removal of
errors if any.
Chemistry (3110001)

Practical – Course Outcome matrix

Course Outcomes (COs):

1. Relate periodic properties such as ionization potential, oxidation states and electronegativity.
2. Analyze microscopic chemistry in terms of atomic and molecular orbital’s and intermolecular forces.
3. Describe the importance and relevance of chemistry in our everyday life.
4. Select the appropriate chemical material and utilization of it.
5. Interpret the methods of science as a logical means of problem solving.
6. Distinguish the ranges of the electromagnetic spectrum used for exciting different molecular energy levels in
various spectroscopic techniques.
Sr. CO CO CO CO CO CO
Objective(s) of Experiment
No. 1 2 3 4 5 6

0 Vision and Mission, PO’s, PEO’s, PSO’s and CO’s

To determine the total hardness of the given samples

1. √ √
by EDTA titrimetric method.

To estimate moisture content in the given coal

2. √ √
sample

To determine the amount of alkalinity present in the

3. √ √
given samples

To determine the amount of chloride present in the

4. √ √
given water sample by Mohr’s method.

To determine the Saponification Value of an oil

5. √ √ √
sample.

To determine the concentration of unknown

6. √ √
Solution Spectrophotometrically.

To determine the percentage of iron in the given

7. √ √
steel sample.
To determine the amount of copper in a given brass
8. √ √
sample.

Study Experiments (Any two)

9. To study the rate of corrosion by weight loss method. √ √

10. To carry out analysis of Pyrolusite ore. √ √

Chemistry (3110001)

1. Vision and Mission

(a) Commissionerate of technical Education

Vision:

 To provide globally competitive technical education;

 Remove geographical imbalances and inconsistencies;
 Develop student friendly resources with a special focus on girls’ education
and support to weaker sections;
 Develop programs relevant to industry and create a vibrant pool of technical
professionals.

(b) Government Engineering College, Valsad

Vision:

To strengthen learning outcomes, Employability and quality standards by

encouraging student centric approaches to become the preferred institute for the
meritorious students.

Mission:

 Design and deliver academic quality standards with regular pedagogical

intervention.
 Effective active learning mode for laboratory hours with attainment of
course outcome indicators
 Strategic attempt to support weaker students.
 Need based faculty development plan with exposure to the best practices.
 Conspire to inspire for creativity, innovation and holistic growth.

(c) Chemical Engineering department

Vision:

To be a hub of creative learning to prepare globally acceptable professional

chemical engineers with ethics and integrity.

Mission:

 To inculcate quality education to students through open access

laboratories and resources.
Chemistry (3110001)

 To develop team work, leadership quality and entrepreneurial aptitude

among students and prepare socially responsible professional chemical
engineers.
 To strengthen linkages with industries by partnering in collaborative
projects and research.
 To develop ecosystem for innovative sustainable solutions to social
problems.
2. Program outcome as prescribed by NBA

PO1 Engineering knowledge: Apply the knowledge of mathematics, science, engineering

fundamentals, and an engineering specialization to the solution of complex
engineering problems.
PO2 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.
PO3 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.
PO4 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.
PO5 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.
PO6 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.
PO7 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.
PO8 Ethics: Apply ethical principles and commit to professional ethics and
responsibilities and norms of the engineering practice.
PO9 Individual and team work: Function effectively as an individual, and as a member
or leader in diverse teams, and in multidisciplinary settings.
PO10 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
PO11 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.
PO12 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.

3. Program Educational Objectives (PEO’s) of chemical engineering department

Chemistry (3110001)

 . To prepare graduates who will be able to apply the fundamental knowledge of

chemical engineering to solve practical problems of chemical Industries.
 To prepare professional chemical engineers with creativity to contribute in
chemical engineering and allied research.
 To prepare graduates who will be potential academicians, or entrepreneurs with
socio-economic responsibilities.

4. Program specific outcomes (PSO’s) of chemical engineering department

i) Graduates will be able to apply concept of process design, synthesis, control, simulation and
optimization to solve chemical engineering problems.
ii) Graduates will be able to apply their chemical engineering skills in dealing with social,
industrial and environmental requirements towards sustainable development.

4. Course outcomes (CO’s) of Chemistry Course

 Relate periodic properties such as ionization potential, oxidation states and

electronegativity.
 Analyze microscopic chemistry in terms of atomic and molecular orbital’s and
intermolecular forces.
 Describe the importance and relevance of chemistry in our everyday life.
 Select the appropriate chemical material and utilization of it.
 Interpret the methods of science as a logical means of problem solving.
 Distinguish the ranges of the electromagnetic spectrum used for exciting different
molecular energy levels in various spectroscopic techniques
Chemistry (3110001)

Industry Relevant Skills

The following industry relevant competencies are expected to be developed in the student by
undertaking the practical work of this laboratory.
● After completing the course students will be able to …
1. Conduct laboratory tests according to procedures and able to do selection of test
equipment/ Instrumentation procedures.
2. Analyze chemicals to provide useful, accurate technical information to necessary
personnel.
3. Prepare samples for analysis using lab techniques and perform sample preparation for
qualitative and quantitative laboratory testing.

Guidelines for Faculty members

1. Teachers should provide the guideline with demonstration of practicals to the students
with all features.
2. Teacher shall explain basic concepts/theory related to the experiment to the students before
starting of each practical
3. Involve all the students in the performance of each experiment.
4. Teachers are expected to share the skills and competencies to be developed in the
students and ensure that the respective skills and competencies are developed in the
students after the completion of the experimentation.
5. Teachers should give opportunities to students for hands-on experience after the
demonstration.
6. Teachers may provide additional knowledge and skills to the students even though not
covered in the manual but are expected from the students by the concerned industry.
7. Give practical assignments and assess the performance of students based on tasks
assigned to check whether it is as per the instructions or not.
8. Teacher is expected to refer to the complete curriculum of the course and follow the
guidelines for implementation.

Instructions for Students

1. Students are expected to carefully listen to all the theory classes delivered by the faculty
members and understand the COs, content of the course, teaching and examination scheme,
skill set to be developed etc.
2. Students shall organize the work in the group and make a record of all observations.
3. Students shall develop maintenance skills as expected by industries.
4. Students shall attempt to develop related hand-on skills and build confidence.
5. Students shall develop the habits of evolving more ideas, innovations, skills etc. apart from
those included in scope of manual.
6. Students shall refer to technical magazines and data books.
7. Students should develop a habit of submitting the experimentation work as per the schedule
and s/he should be well prepared for the same.
Chemistry (3110001)

Common Safety Instructions

1. The performance of unauthorized experiments is strictly forbidden.

2. Be careful when handling hot glassware and apparatus in the laboratory. Hot glassware looks
just like cold glassware.
3. Use full-length, long-sleeved laboratory coats or chemical-resistant aprons, chemical splash
goggles, shoes and all the safety standards during the laboratory session.
4. Do not eat or drink anything in the laboratory. Food and drink, open or closed, should never
be brought into the laboratory or chemical storage area.
5. Never point the open end of a test tube containing a substance at yourself or others.
6. Never fill a pipette using mouth suction, always use a pipetting device for taking chemicals
for testing.
7. Make sure no flammable solvents are in the surrounding area when using Bunsen burners
and do not leave them unattended. Also turn off all heating apparatus, gas valves, and water
faucets when not in use.
8. Do not take away any equipment or chemicals from the laboratory without permission of
faculty/laboratory in charge.
9. Keep all your belongings like coats, bags, and other personal items in designated areas, not
on the bench tops or in the aisle ways.
10. Notify your laboratory in charge / faculty of any sensitivities that you may have to particular
chemicals if known.
11. Properly dispose of broken glassware, weigh boats, gloves, filter paper, and paper towels
and other sharp objects.
12. Know the location of all the exits in the laboratory and building including fire extinguishers,
alarm systems with pull stations, fire blankets, eye washes, first-aid kits etc.
13. In case of an emergency or accident, follow the established emergency plan as explained by
the teacher and evacuate the building via the nearest exit.
14. Do not directly touch any chemical with your hands. Always use a spatula to remove a solid
reagent from a container
15. Never handle bottles that are wet or too heavy for you.
Chemistry (3110001)

Index
(Progressive Assessment Sheet) (Any 8 to be performed by student)
Sr. No. Objective(s) of Experiment Page Date of Date of Assessme Sign. of Remar
No. perform submiss nt Teacher ks
ance ion Marks with date

To determine the total hardness of the given

1.
samples by EDTA titrimetric method.

To estimate moisture content in the given coal

2.
sample

To determine the amount of alkalinity present

3.
in the given samples

To determine the amount of chloride present

4.
in the given water sample by Mohr’s method.

To determine the Saponification Value of an

5.
oil sample.

To determine the concentration of unknown

6.
Solution Spectrophotometrically.

To determine the percentage of iron in the

7.
given steel sample.
To determine the amount of copper in a given
8.
brass sample.
To study the rate of corrosion by weight loss
9.
method.
10. To carry out analysis of Pyrolusite ore.
Total
 Experiment No: 1
Estimation of Hardness of Water in the given water sample
Date:

Competency and Practical Skills:

1. Able to set up appropriate equipment for a titration correctly.
2. Have basic knowledge of coordination compounds, ligands etc.
3. Know about different indicators and their role to determine the end point of a titration
4. Able to record observations using the correct SI units to the appropriate number of decimal places
5.

Relevant CO’s : CO3: Describe the importance and relevance of chemistry in our everyday life.
CO4: Select the appropriate chemical material and utilization of it.

Objectives: (a) To describe hardness of water

(b) To show difference between hard and soft water
(c) To show the disadvantages of using hard water
(b) To estimate hardness in water sample

Glassware/Instruments: Burette, Pipette, Conical flask, Beaker, Weighing balance, Measuring

cylinder, Funnel, Glass rod, Tile Burette stand etc.

Chemicals: 0.01 M EDTA solution, Ammonia buffer, Erichrom black-T (EBT) indicator, Distilled
water, Tap water/ water sample

Theory:

● Water is crucial compound for life on earth. Pure water is odorless, tasteless and nearly
colorless. It is an important Engineering material as used in a number of industries like
thermal Power Plants, textile industries, Hydropower, Agriculture, Mining etc.
● It is obtained from surface or underground water sources. Water quality parameters like
dissolved oxygen, pH, Alkalinity and hardness etc are often measured prior to industrial use.
● The property of water to form an insoluble curd with soap instead of lather. OR soap
destroying property is known as hardness.

● Hardness is caused due to the presence of soluble salts like Bicarbonates (HCO3-), Sulphates
(SO42-) and Chlorides (Cl-) of Calcium (Ca2+), Magnesium (Mg2+) and some other heavy
metals.
● It arises due to dissolution of salts of rocks/soils, basically due to soluble salts of Calcium
and Magnesium. Bicarbonates arise when rainwater dissolves CO2 and comes in contact
with soil. Hardness due to bicarbonate salts is removed by heating and is known as
temporary hardness, while rest is termed as permanent hardness
● Hardness in a water sample can be estimated by complexometric titration using the standard
 solution of EDTA.
● EDTA (Ethylenediamine tetra acetic acid) forms colorless stable complexes with Ca2+ and
Mg2+ ions present in water at pH = 9-10. To maintain the pH of the solution at 9-10, buffer
solution (NH4Cl + NH4OH) is used. Erichrom Black-T (E.B.T) is used as an indicator.
● First EBT is added in hard water maintaining pH by using a buffer. The hardness causing
cations (Ca2+ and Mg2+ ) present in water form an unstable, wine-red colored complex with
EBT indicator.

Eriochrome Black -T(EBT Indicator)

H2In- + Ca2+ ↔ CaIn- + 2H1+

Wine Red

● This unstable M-EBT complex gets converted into M-EDTA complex at the end point
giving the sky blue colour. EDTA chelates with hardness causing ion in quantitative amount
and releases EBT.

EDTA MOLECULE EDTA CHELATING WITH METAL

EDTA(aq) + CaIn–(aq) + 2H+(aq) → H2In–(aq) + CaEDTA(aq)

pink blue
Set up diagram:

Safety and necessary Precautions:

1. Wear lab coat, safety glasses and gloves.

2. Avoid skin and eye contact with chemicals.
3. In case of skin contact, rinse the area for several minutes. For eye contact, flush eyes with water
and seek immediate medical advice.

Procedure:

1. Fill the burette with Standard 0.01 M EDTA solution.

2. Take 25 ml water sample, in conical flask
3. To maintain PH add around 1 ml of ammonia buffer (mixture of NH4Cl + NH4OH).
4. Now add 2 drops of EBT Indicator which gives wine red color
5. Titrate it with Standard 0.01 M EDTA solution till wine red color converts into sky blue.
6. Note down burette reading.
7. Repeat the process till constant reading is obtained.
8. Note down the concordant reading. Suppose the concordant burette reading is x ml.

Observations:

Burette :- 0.01 M EDTA solution.

Pipette :- 25 ml water + 1 ml ammonia buffer.

Indicator :- 5 drop EBT.

Color change at end point: - wine red to Sky blue.

 Observation table:

Sample Trial No. Volume of Burette Reading Volume of

Name or Water Sample EDTA used
No. Taken (in ml) Initial Final Diff. (Mean)
(in ml) (in ml) (in ml)

Calculation:

Molecular weight of CaCO3 = 40 +12 +48 = 100

Now, 1000 ml 1 M EDTA = 100g hardness as CaCO3

1 ml 1M EDTA = 0.1 g hardness as CaCO3

1 ml .01 M EDTA = 0.001 g or 1 mg hardness as CaCO3

x ml .01 M EDTA = x mg hardness as CaCO3 in 25 ml water

Hardness in mg /L = 40 × x mg/L ( where x is burette reading)

Result:

25 ml water sample reading = …………ml of 0.01M EDTA solution.

Total hardness =……………………….mg/L

Conclusion:

Quiz:

1. Total hardness of water can be determined by titrating the fixed volume of water against the
standard ___________ solution.
a) Soap b)alkaline soap c) acidic soap d) alcoholic soap

2. The water which form lather directly with the soap is called _________
a) Hard water b) Soft water c) heavy water d) very hard water

3. EDTA has the ability to form _________ with metal ions

a) Stable complex b) unstable complex c) salt d) double salt

4. To prepare EDTA solution, ___________ grams of EDTA is dissolved in one liter of water.
 5. Name the salts which cause hardness to the water?

6. What are the limits of hardness in potable water given by different agencies?

7. What are the limits of hardness in effluent water given by different agencies?

8. Give types of hardness.

9. (a) Differentiate between (a) Hard water and soft water

(b) Temporary and permanent hardness

10. (a) Full form of EBT is……….

(b) EDTA form ……… coordinate bonds with metal cation.

Suggested Reference: Laboratory Manual of Engineering Chemistry, by S K. Bhasin & Sudha Rani.
Publisher: Dhanpat Rai Publishing Company Ltd.

References used by the students: (Sufficient space to be provided)

Rubric wise marks obtained:

Rubrics 1 2 3 4 5 Total
Marks
 Experiment No: 2
To Estimate moisture content in the given coal sample
Date:

Competency and Practical Skills:

1. Able to Perform task with due consideration to safety rules

2. Able to arrange and set weighing balance, hot air oven etc.
3. Skilled to do calculation and maintains tables for data observed during experimentation

Relevant CO’s: CO3: Describe the importance and relevance of chemistry in our everyday life.
CO4: Select the appropriate chemical material and utilization of it.

Objectives: (a) To describe types of coal and constituents

(b) To show difference between charcoal and coal
(c) To show the disadvantages of moisture in coal
(b) To estimate moisture content of coal

Glassware/Instruments: Crucible, Spatula, Tongs, Balance (sensitive to 0.0001 g), Desiccator

Chemicals: samples of coal, lignite, bituminous, anthracite or charcoal

Theory:

● Coal contains many properties, such as ash and sulfur content, that are frequently measured
to determine if a particular coal is suitable for use in a particular process. The most
frequently used analysis is a simple type of chemical analysis called proximate analysis.
● This consists of a determination of the moisture and ash content of the coal as well as an
estimate of the amount of gas that can be driven from the coal by heating. The final
component of a proximate analysis is an estimate of the nonvolatile carbon called fixed
carbon.
● The moisture content is determined by heating a small sample of powdered coal to a
temperature slightly above the boiling point of water (about 105-110 oCelsius). This heating
will evaporate the moisture from the coal. When the weight of the sample stops changing,
the weight loss is equivalent to the weight of the moisture.

Safety and necessary Precautions:

● Wear lab coat, safety glasses and gloves.

● Avoid skin and eye contact with chemicals.
● In case of skin contact, rinse the area for several minutes. For eye contact, flush eyes with
water and seek immediate medical advice.
● Don’t keep the oven open or loosely closed during heating.
Set up Diagram:

Procedure:
1. Take one clean crucible and heat it at 110-115 oC temperature for 20 min. in the
oven. After 20 min., remove the crucible from the oven and cool it in a desiccator
for 15-20 minutes.
2. Take the empty crucible using tongs, record the weight of the empty crucible (W1).
3. Transfer approximately 1 g of the coal sample to the crucible using a spatula. Then
record grams as (W2). Subtract the crucible from the sample mass (W1) and record
mass as (W3).
4. Place the crucible in a desiccator and transfer into a preheated oven and heat it at
101-105 oC temperature for 30 - 60 min.
5. Put the cover on the crucible and transfer into the desiccator for 15-20 minutes to
cool.
6. Weight the crucible to the nearest 0.0001 g and record the weight in grams as (W4).
7. Do the calculations and find the moisture content in the given coal sample.

Observations:

Weight of empty crucible = ___________g (W1)

Weight of crucible with coal = __________g (W2)

Weight of coal sample = _________g (W3) (W2 -W1)

Weight of heated crucible + coal = _________g (W4)

Weight of moisture = ___________g (W5) (W4 –W2)

Calculation:

% of moisture = (W5) x 100 / (W3)

Result:
The moisture content in the given coal sample is = ………… %

Quiz:

1. In proximate analysis, which of the following elements can be found?

a) % of moisture content b) % of carbon c) % of hydrogen d) % of nitrogen

2. High % of moisture is undesirable because _________

a) increases the cost of transport b) increases the cost of calorific value
c) Increases the cost of efficiency d) decreases the cost of storage cost

3. Ultimate analysis of coal is also called as

a) quantitative analysis b) elementary analysis
c) qualitative analysis d) secondary analysis

4. % of nitrogen can be determined by the process….

a) dulong’s formula b) orsat’s apparatus c) kjeldahl’s method d)fractional distillation

5. The determination of exact elemental percentage in the coal is known as :

a) proximate analysis b) ultimate analysis c) tempering d)combustion

6. Enlist the four (4) major types of coal with approximate % of C

7. How can we find the % of volatile matter in coal?

8. What is the difference between proximate and ultimate analysis?

9. Enlist applications of coal.

10. How can we find the % of fixed carbon in coal?

Suggested Reference:
Laboratory Manual of Engineering Chemistry, by S K. Bhasin & Sudha Rani. Publisher: Dhanpat Rai
Publishing Company Ltd. (+Ref. GTU Syllabus)

References used by the students: (Sufficient space to be provided)

Rubric wise marks obtained:

Rubrics 1 2 3 4 5 Total
Marks
 Experiment No: 3
To determine the amount of alkalinity present in the given samples.
Date:

Competency and Practical Skills:

1. Able to prepare standard solutions.

2. Able to Perform task with due consideration to safety rules
3. Able to do required calculation in volumetric analysis.

Relevant CO’s : CO3: Describe the importance and relevance of chemistry in our everyday life.
CO4: Select the appropriate chemical material and utilization of it.

Objectives: (a) To describe alkalinity of water and its cause..

(b) To show use of phenolphthalein and methyl orange as an indicator.
(c) To estimate alkalinity of given water sample
(d) To explain significance of alkalinity in water and wastewater treatment

Glassware/Instruments: Burette with Burette stand and porcelain dishes, conical flask, Pipettes
with rubber bulb, Measuring cylinders, Beakers, Dropper, Stirrer

Chemicals: Standard 0.02N sulphuric acid, Phenolphthalein indicator, Methyl orange indicator

Theory:
● Alkalinity is a measure of the capability of water to absorb H + ions without significant
change of pH. In other words, alkalinity is a measure of the acid buffering capacity of water.
● Alkalinity is primarily due to salts of weak acids, although weak or strong bases may also
contribute. Alkalinity of a sample of water is primarily due to the presence of OH–
(hydroxide ion), HCO3– (bicarbonate ion) and CO32– (carbonate ion) or the mixture of two
ions present in water. The possibility of OH– and HCO3 – ions together is not possible since
they combine together to form CO32– ions.
● It is measured volumetrically by titration with 0.02 N sulphuric acid and is reported in terms
of CaCO3 equivalent.
● For samples whose initial pH is above 8.3, the titration is conducted in two steps. In the first
step, the titration is conducted until the pH is lowered to 8.2, the point at which
phenolphthalein indicator turns from pink to colorless. This value corresponds to the points
for conversion of carbonate to bicarbonate ion.
● The second phase of titration is conducted until the pH is lowered to 4.5, corresponding to
methyl orange end point, which corresponds to the equivalence points for the conversion of
bicarbonate ion to carbonic acid.

Safety and necessary Precautions:

● Wear lab coat, safety glasses and gloves

● Avoid skin and eye contact with chemicals.
● In case of skin contact, rinse the area for several minutes. For eye contact, flush eyes with
water and seek immediate medical advice.
Procedure:

1. Pipette out 50 mL of sample into a clean Erlenmeyer flask (V).

2. Add one drop of sodium thiosulphate solution, if residual chlorine is present.
3. Add two drops of phenolphthalein indicator; if the pH is above 8.3, colour of solution
becomes pink.
4. Titrate against standard 0.02 N sulphuric acid in the burette, till the colour just disappears.
Note down the volume (V1).
5. Then add two drops of methyl orange indicator, the colour turns yellow.
6. Again titrate against acid, until the colour turns to orange yellow.
7. Note down the total volume (V2).
8. Put both the results in the table and compare the results.

Observations:

Sample Trial Burette Reading Volume of Burette Reading Volume

Name No. acid used of acid
or No. (Mean) used
(Mean)

Initial Final Diff. Initial Final Diff.

Calculation:

1. Phenolphthalein alkalinity (P) as mg/L CaCO3 = V1 x 1000

mL of sample
 2. Total alkalinity (T) as mg/L CaCO3 = V2 x 1000

mL of sample

The types of alkalinities present in the samples are calculated using the equations given in the
following table and the results are tabulated.

Result:

Sample Hydroxide Carbonate Bicarbonate Hydroxide Carbonate

Name or No. alkalinity as alkalinity as alkalinity as Carbonate Bicarbonate
CaCO3 (ppm) CaCO3 (ppm) CaCO3 (ppm) alkalinity as alkalinity as
CaCO3 (ppm) CaCO3 (ppm)

Quiz:

1. Which amongst the following indicators is pink in basic medium?

a) Methyl orange b) Starch c) Phenolphthalein d) Litmus

2. With respect to the constituents causing alkalinity in water, which of the following situation never
arises?
a) CO32- and HCO3– together
b) HCO3– and OH– together
c) OH– only
d) OH– and CO32- together

3. Alkalinity is not caused by…

a) carbonates b) bicarbonates c) chlorides d) all
4. The following cause alkalinity as well hardness in natural water:
a) Calcium carbonates c) Calcium bicarbonates
b) Magnesium carbonates d) All

5. Which of the following is not a water borne disease?

a) Typhoid b) Scabies c) Cholera d) Hepatitis

6. Why are two indicators used in determining alkalinity in a given water sample?

7. Alkalinity of water is an indication of ….

8. Why is alkalinity known as the buffering capacity of water?

9. What is the limit range of alkalinity according to WHO and BIS?

10. Enlist applications of alkalinity measurement.

Suggested Reference:
Laboratory Manual of Engineering Chemistry, by S K. Bhasin & Sudha Rani. Publisher: Dhanpat Rai
Publishing Company Ltd.

References used by the students: (Sufficient space to be provided)

Rubric wise marks obtained:

Rubrics 1 2 3 4 5 Total
Marks
 Experiment No: 4
To determine the amount of chloride present in the given water sample.
Date:

Competency and Practical Skills:

1. Able to Perform task with due consideration to safety rules

2. Able to do required calculation in volumetric analysis.
3. Have knowledge of chemistry of precipitation of chloride ion

4. Relevant CO’s : CO3: Describe the importance and relevance of chemistry in our everyday life.
CO4: Select the appropriate chemical material and utilization of it.

Objectives: (a) To describe different impurities in water.

(b) To show the disadvantages of chloride in water.
(c) To estimate the amount of chloride in a water sample.

Glassware/Instruments: Burette, Pipettes, Erlenmeyer flask, Measuring cylinder

Chemicals: Chloride free distilled water. Standard silver nitrate solution (0.0141N) Potassium
chromate indicator. Acid or alkali for adjusting pH.

Theory:
● Chloride in the form of chloride (Cl- ) ion is one of the major inorganic anions in water and
wastewater.
● The chloride concentration is higher in wastewater than in raw water because sodium
chloride is a common article of diet and passes unchanged through the digestive system.
● The measured chloride ions can be used to know salinity of different water sources. For
brackish water (or sea water or industrial brine solution), it is an important parameter and
indicates the extent of desalting of apparatus required.
● It also interferes with COD determination and thus it requires a correction to be made on the
basis of the amount present or else a complexing agent, such as HgSO4 can be added.
● Further, chloride ions are used as tracer ions in column studies to model fate of different
contaminants in soil and liquid media
● If water containing chlorides is titrated with silver nitrate solution, chlorides are precipitated
as white silver chloride.
● Potassium chromate is used as an indicator, which supplies chromate ions.
● As the concentration of chloride ions approaches extinction, silver ion concentration
increases to a level at which reddish brown precipitate of silver chromate is formed
indicating the end point.

Safety and necessary Precautions:

● Wear lab coat, safety glasses and gloves.

● Avoid skin and eye contact with chemicals.
● In case of skin contact, rinse the area for several minutes. For eye contact, flush eyes with
water and seek immediate medical advice.
Procedure:

1. Take 50mL of sample (V) and dilute to 100mL.

2. If the sample is coloured add 3mL of aluminum hydroxide, shake well; allow settling, filtering,
washing and collecting filtrate.

3. Sample is brought to pH 7–8 by adding acid or alkali as required.

4. Add 1mL of indicator (Potassium chromate).

5. Titrate the solution against standard silver nitrate solution until a reddish brown precipitate is
obtained.

6. Note down the volume (V1).Repeat the procedure for blank and note down the volume (V2).

Observations:

Burette:

Flask:

Indicator:

End Point:

Volume of sample taken for each trial =______ml

Calculation:

Result:

The amount of chloride contents in the given sample is = …………

Quiz:

1. What percentage of sodium chloride is approximately present in sea water? 1.40 % b) 2.40
% c) 3. 40 % d) 4.40 %

2. Step of sewage water treatment in which effluent from sewage plant is treated with chlorine is
called

a) Primary sewage treatment b) Secondary sewage treatment

c) Activated sludge treatment d) Chlorination

3. Process in which water is treated with slaked lime and alum is called

a) Sedimentation b) Coagulation c) Filtration d) Chlorination

4. Which of the following represents the physical characteristics of water?

a) Chloride content b) BOD c) Turbidity d) COD

5. At what pH, chlorine exists as molecular chlorine?

a) >10 b) 5 c) <5 d) >5

6. What is the role of chromate ions in chloride determination?

7. Why pH range is important in chloride determination?

 8. How chlorides gain access to natural waters?

9. What is the limit range of chloride in potable water according to WHO and BIS?

10. Enlist applications of chloride measurement in water

Suggested Reference:
Laboratory Manual of Engineering Chemistry, by S K. Bhasin & Sudha Rani. Publisher: Dhanpat Rai
Publishing Company Ltd. (as per GTU Syllabus)

References used by the students: (Sufficient space to be provided)

Rubric wise marks obtained:

Rubrics 1 2 3 4 5 Total
Marks
 Experiment No: 5
To Determine Saponification Value of an oil sample.
Date:

Competency and Practical Skills:

1. Able to Perform task with due consideration to safety rules

2. Able to do required calculation in volumetric analysis.
3. Have basic knowledge of organic functional groups and their chemistry

Relevant CO’s: CO3: Describe the importance and relevance of chemistry in our everyday life.
CO4: Select the appropriate chemical material and utilization of it.
CO5: Interpret the methods of science as a logical means of problem solving

Objectives: (a) To describe types of oils used to make soap.

(b) To show the difference between soap and detergent.
(c) To show the process of soap making.
(b) To show the role of estimation of saponification value in oil refining.

Glassware/Instruments: Boiling water bath/Burner, Reflux condenser, Burettes, Reflux

condenser, Burettes, Conical flasks, measuring cylinder
Chemicals: Fats and oils, Fat solvent, Alcoholic KOH, Phenolphthalein, Hydrochloric acid.

Theory:
● Fats and oils are the principle stored forms of energy in many organisms. These are
composed of triglyceride molecules (Ester of glycerol and three fatty acids).
● On refluxing with alkali, triacylglycerols (fatty acid esters) are hydrolyzed to give
glycerol and potassium salts of fatty acids (soap).Such process is known as
Saponification. The saponification equation is shown below:

● Saponification literally means soap making. It is important for the industrial user to know
the amount of free fatty acid present, since the presence of free fatty acid in the refined oil
is detrimental to the quality of refined oil as soap is obtained as a contaminant.
The amount of free fatty acid is estimated by determining the quantity of alkali that must be
added to the fat to render it neutral.
● The saponification value is the number of milligrams of KOH required to neutralize the fatty
acids resulting from the complete hydrolysis of 1g of fat.
● The saponification value gives an indication of the nature of the fatty acids constituent of
fat and depends on the average molecular weight of the fatty acids constituent of fat. Greater
the molecular weight (the longer the carbon chain), smaller is the number of fatty acids
liberated per gram of fat hydrolyzed and therefore, smaller the saponification number and
 vice versa.

Safety and necessary Precautions:

● Wear lab coat, safety glasses and gloves.
● Avoid skin and eye contact with chemicals.
● In case of skin contact, rinse the area for several minutes. For eye contact, flush eyes with
water and seek immediate medical advice.
● Ensure the secure connections of reflux condensers in experimental set up.

Procedure:

1. In a small beaker accurately weight 1g of fat and dissolve it in about 3ml of the fat solvent
(equal volumes of 95% ethanol and ether).
2. Transfer the contents of the beaker to a 250 ml conical flask by rinsing the beaker three
times with further milliliters of solvent.
3. Add 25ml of alcoholic KOH and attach to a reflux condenser.
4. Set another reflux condenser as blank with everything present except the fat.
5. In a small beaker Accurately weight 1g of fat and dissolve it in about 3ml of the fat solvent
(equal volumes of 95% ethanol and ether)
6. Transfer the contents of the beaker to a 250 ml conical flask by rinsing the beaker three
times with further milliliters of solvent.
7. Add 25ml of alcoholic KOH and attach to a reflux condenser.
8. Set another reflux condenser as blank with everything present except the fat.
9. Heat both flasks in a boiling water bath for 30 min.
10. Leave to cool to room temperature and titrate with 0.5 mol/liter HCl and use phenolphthalein
as indicator. Until the pink color disappears.
11. Record your readings as T ml for test and B ml for blank.

Observations:

Concentration of alcoholic KOH solution=_______N

Concentration of HCl solution =_______N

Concentration of HCl solution =_______N

Burette solution:

Flask solution: Alcoholic KOH (with and without oil)

Indicator;

End Point:

Refluxing temperature:
Weight of the sample:____________g

Observation table

Sr. No. Name of Weight of Blank (B) Test(T) Saponificati

Oil Oil on value (S)
mg KOH/g
1.
2.
3.

Calculation: Saponification Value = (Titre value of blank in ml – Titre

Value of sample in ml)

x N KOH x Equivalent wt of KOH

Result:

The Saponification value of the given oil sample is = …………

Quiz:

1. It is __________ of fatty oils which leads to formation of soaps.

a) Alkaline hydrolysis b) Alkaline electrolysis c) Hydrolysis d) Electrolysis

2. The saponification value of the vegetable oil is ______

a) Very high b) Very low c) moderate d) can’t be determined

3. Which of the following term describe saponification?

a) Cleavage of ester molecules into glycerol and sodium salt of fatty acid
 b) Dehydration process
c) Hydrolysis of a salt by adding a weak acid
d) Etherification process

4. If a fat has low saponification value, what can be inferred about the chain length of the fatty
acid?
a) Short chain length
b) Long chain length
c) Moderate chain length
d) Not possible to make any inference

5. Which of the following compound is an industrial product by saponification?

a) Glycerol b) NaOH c)KOH d)KCl

6. How is the saponification number determined?

7. What is meant by saponification index?

8. Why do we add NaCl sometimes during saponification?

9. Enlist five different types of oils with their saponification value.

10. Enlist three applications of estimation of saponification value

Suggested Reference:
Laboratory Manual of Engineering Chemistry, by S K. Bhasin & Sudha Rani. Publisher: Dhanpat Rai
Publishing Company Ltd. (as per GTU Syllabus)

References used by the students: (Sufficient space to be provided)

Rubric wise marks obtained:

Rubrics 1 2 3 4 5 Total
Marks
 Experiment No: 6
To Determine the unknown concentration of given solution spectrophotometrically.
Date:

Competency and Practical Skills:

1. Able to perform task with due consideration to safety rules

2. Can follow operating procedure to operate spectrophotometer for chemical analysis.
3. Have knowledge of electronic level, molecular orbitals, bonding and EM spectra.

Relevant CO’s:
CO2: Analyze microscopic chemistry in terms of atomic and molecular orbital’s and
intermolecular forces.
CO6: Distinguish the ranges of the electromagnetic spectrum used for exciting different molecular
energy levels in various spectroscopic techniques.

Objectives: (a) To describe spectra, spectral lines, wavelength range of various EM waves
(b) To show Interaction between EM radiation and matter.
(c) To show the working of UV-VIS spectrophotometer
(b) To Determine concentration of given solution using a spectrophotometer.

Glassware/Instruments: Spectrophotometer, Cuvette, wash bottle, filter paper, beaker. test tube,
weighing balance, volumetric flask

Chemicals: Cobalt nitrate, distilled water

Theory:
● When a beam of monochromatic light falls upon a substance, the fraction of the light absorb
in a function of the concentration of the substance and the path length. The ratio of intensity
of transmitted light I to the incident ‘Io’ defined as TRANSMITTANCE ‘T’. Thus,

T= I/Io …… (1)

Mathematically, it is found that

ln Io – ln I = Kb …….. (2)

Where,

K= a proportionality constant, characteristic of the absorbing solute.

b = path length.

The above expression, known as Lambert law, states that for a given solute the intensity of
the transmitted light decreases logarithmically as the path length increases arithmetically.

● Here greater interest is the dependence of the transmitted light on the concentration of
absorbing solute. Beer found that increasing the concentration of the absorber had the same
 effect as increasing the path length ‘b’. Thus the proportionality constant ‘k’ is in turn
proportional to the concentration ‘C’ of absorbing solute, or

k=AC ……. (3)

log(Io/I)=abC …… (4)

Where ‘a’ is another constant, it also takes care of expressing the equation with base of log10.
Equation (4) is Lambert- Beer’s Law.

Substituting equation (1) in equation (4), we get

Log I/T= abC

This gives a relationship between Transmittance ‘T’ and Concentration ‘C’.

● However, the relationship between the concentration ‘C’ and the log of the inverse of ‘T’ is
inconvenient in quantitative analysis. Therefore, another quantity introduced, called
ABSORBANCE ‘A’ as,

A = log I/T -------(5)

Thus, A = abC -------(6)

● The above law is of fundamental importance to spectrophotometer analysis. This facilities

measurement of concentration of different samples of some absorbing solutes (with
reference to a known standard value) by measurement of absorbance ‘A’ for each sample.

Safety and necessary Precautions:

● Wear lab coat and safety glasses and gloves.
● Avoid skin and eye contact with chemicals.
● In case of skin contact, rinse the area for several minutes. For eye contact, flush eyes with
water and seek immediate medical advice.
● Liquid should not overflow from the cuvette
● Calibrate the instrument regularly..

Procedure:
1. Prepare a stock solution of 0.2M cobalt nitrate(5.82 g. in 100ml. Dist.H2O). Dilute this
solution quantitatively so as to get 0.04M, 0.08M, 0.12M and 0.16M solution in 100 ml.
2. Strictly follow the instructions given on the instrument.
3. Measure the one of the above Co
++
solutions against a water ‘blank’ using each of the filter
in turn given with the instrument. The filter giving the maximum absorbance (510 nm) will
be most suitable for measuring the absorbance (A).
4. Determine the absorbance (from % Transmittance) of a test solution against water blank.
Carry out replicate measurements so as to get the corresponding readings.
++
5. Repeat the experiment for unknown Co concentration.
6. Plot absorbance (A) against concentration. A linear curve must be obtained if Beer-
Lambert's law is valid. Find the concentration of the unknown Co++ solution from this curve
from its absorbance.
 7. Tabulate the observation as follows.

Observations:

Observation Table

S. No. Concentration of % Transmittance %Absorbance (100-

Solution (T%) T%)

5 Unknown Co++
solution

Plot a graph Concentration (M) vs Absorbance (100-T %)

Calculation:

Calculate the unknown concentration using the straight line of the plotted graph

Result:

The Concentration given Coblat nitrate solution is = …………

Quiz:
1. In a surface spectrometer, which of the following beam is analysed?
a) Reflected beam b) Absorbed beam c) Refracted beam d) Incident beam

2. Beer Lambert’s law gives the relation between which of the following?
a) Reflected radiation and concentration b) Scattered radiation and concentration
c) Energy absorption and concentration d)Energy absorption and reflected radiation
3. In which of the following ways, absorption is related to transmittance?
a) Absorption is the logarithm of transmittance
b)Absorption is the reciprocal of transmittance
c) Absorption is the negative logarithm of transmittance
d) Absorption is a multiple of transmittance
4. Beer’s law states that the intensity of light decreases with respect to _____________
a) Concentration b) composition c) distance d) Volume

5. Which of the following is not true about Absorption spectroscopy?

a) It involves transmission
b) Scattering is kept minimum
c) A. Reflection is kept maximum
d) Intensity of radiation leaving the substance is an indication of concentration

6. which of the following is a source used in spectroscopy?

a) LASER b) Tube light c) Sodium vapour lamp d)Tungsten lamp

7. Which of the following wavelength ranges is associated with UV spectroscopy?

a) 400 – 100 nm b) 380-750 nm c) 0.01– 10 nm d) 0.8 – 500 µm

8. In photometers, the readings of the specimen are initially obtained in the form of which of the
following parameters?
a) Transmittance b) Absorption c) Wavenumber d) Wavelength

9. UV-VIS spectroscopy is also known as_____________.spectroscopy.

a) Electronic b) Vibrational c) Rotational d) magnetic

10. Write the principle of UV visible spectroscopy?

Suggested Reference:
Laboratory Manual of Engineering Chemistry, by S K. Bhasin & Sudha Rani. Publisher: Dhanpat Rai
Publishing Company Ltd. (as per GTU Syllabus)

References used by the students: (Sufficient space to be provided)

Rubric wise marks obtained:

Rubrics 1 2 3 4 5 Total
Marks
 Experiment No: 7
To determine the percentage of iron in the given steel sample.
Date:

Competency and Practical Skills:

1. Able to perform the test with accuracy and safety rules
2. Able to do titration and use secondary standard solutions.
3. Able to calculate the composition of steel samples.

Relevant CO’s : CO4: Select the appropriate chemical material and utilization of it.
CO5: Interpret the methods of science as a logical means of problem solving

Objectives: (a) To describe types of steel and constituents.

(b) To show the difference between stainless steel and normal steel.
(c) To estimate the iron content of a given steel sample.

Glassware/Instruments: Burette, Pipettes rent, Erlenmeyer flasks, measuring cylinder

Chemicals: Standard oxalic acid solution (N/10)
Potassium permanganate solution (N/10)
Dilute sulphuric acid
Theory:

● Steel is essentially an alloy of iron and carbon. Plain steel contains a certain amount C, Si,
S, P and Mn apart from iron. For special purposes varying amounts of other metals such as
Cr, V, Mo, W, Ti, Ni, Co, Zr and Cu are added.
● Transition metals mixed freely with each other in the molten state and on cooling a solution
of different metals results in the form of alloys.
● For examples, Cr dissolves in Ni to form Cr-Ni alloy. Mn dissolves in iron to form
manganese steels.
● The iron, cobalt, Nickel based alloys are called super alloys. They are highly resistant to
oxidation at high temperature and mainly used for blades and rotors of jet engines. For
example, Mnemonic alloys and Hast alloys.
● In the steel sample it contains iron and manganese (2+) ions. Addition of acid solutions with
the permanganate ions undergoes reduction reaction to Mn2+ ions. Since the permanganate
ions are violet in color and Mn2+ ions colorless, the end point in the titration reaction will
give a permanent pink color.
● For determining the amount of iron in steel, The steel sample is dissolved in dil H2SO4,
when the Fe present as FeSO4 and H2 gas is evolved

Fe + H2SO4 -------> FeSO4 + H2

● The amount of Fe+2 ion in the solution can be determined by a redox titration with standard
KMnO4 or K2Cr2O7 solution. The ionic equations with acidified KMnO4 are given below:

MnO4-+8H+ -----> Mn2+ +4 H2O+ 5e-

[Fe2++e------> Fe3+]*5

MnO4- + 5 Fe2++8H+ ---->Mn2++8H2O +5Fe3+

Safety and necessary Precautions:

● Wear lab coat, safety glasses and glows.

● Avoid skin and eye contact with chemicals.
● In case of skin contact, rinse the area for several minutes. For eye contact, flush eyes with
water and seek immediate medical advice.
● Do not add water in conc. acids.

Procedure:
Part-A: Standardization of KMnO4 solution
1. Prepare 100ml standard (N/10) oxalic acid solution.
2. Prepare 250 ml approx. (N/10) KMnO4 solution.
3. Pipette out 20 ml of the standard (N/10) oxalic acid solution into a 100 ml conical flask.
4. Add 10 ml of dilute H2SO4 and heat the solution to about 70oC.
5. Then, titrate this solution slowly against the KMnO4 solution from the burette until a faint
but permanent pink color persists in the solution.
6. Repeat the titration until concordant results of titrate value are obtained and calculate the
normality of the KMnO4 solution.
Part-B: Determination of iron in the steel sample
1. Accurately weigh 0.25 g of the cleaned steel sample onto a watch glass and carefully transfer
it to a 250 ml round bottom flask.
2. Add about 50 ml of dil. H2SO4 into the flask and gently heat it in a water bath. The steel
goes into solution with a brisk evolution of hydrogen gas.
3. Take care to see that droplets of the solution do not spurt out of the flask. This can be done
by covering the flask with a funnel or by providing a loose cotton wool plug at the mouth
of the flask.
4. When the steel is almost dissolved, add a piece of granulated zinc. The zinc reacts with
H2SO4 giving hydrogen gas which prevents the oxidation of ferrous ions and also reduces
the ferric ions present, of any.
5. Make up the volume of 250 ml with distilled water and shake the solution thoroughly.
6. Pipette out of 20 ml of the solution into a conical flask, add 10 ml of dilute H2SO4 and titrate
against KMnO4 solution taken in the burette.
7. The appearance of a faint but permanent pink color marks the end-point.
8. Repeat the titrations with fresh 20 ml portions of the solution until concordant readings are
obtained

Observations:
Part-A:
Oxalic Acid solid used =____________g
KMnO4 solid used=_______________g
Flask:
Indicator:
Temp. Aprrox=_____oC
End point:

Tabulation :
Calculation: Part-A

From first titration let us calculate the exact normality of KMnO4 solution

N1V1 = N2V2

N1 =0.1N oxalic acid

V1= Volume of N/10 Oxalic acid Taken(20ml)

N2= KMnO4 Solution approx. (N/10)

V2= Volume of KMnO4 Solution approx. (N/10) used

Observations:
Part-B:

1. Weight of empty watch glass = _______W1g

2. Weight of watch glass along with steel piece = _______W2g
3. Weight of the steel sample taken = (W2-W1)g = _______Wg
4. Wg of the sample after dissolving in H2SO4 acid was made up to 250 ml, 20 ml of this solution on
titration against KMnO4 (of normality N2) required = ____V ml

Calculation: Part-B

Calculate the amount of iron present in the entire 250 ml of the solution (prepared from 0.25 g of the steel
sample) using the relation.

1 ml of N/10 KMnO4 = 5.585 mg of Fe

The amount of Fe thus calculated on multiplication with 100 gives the percentage of Fe present the given
sample of the plain carbon steel. Thus,

% Fe in the steel sample = V×12.5×5.585×N2×10×100

250 × W

= (12.5 V × 5.585 × N2) %.

[Where 12.5 V is the volume of N2 normal KMnO4 equivalent to the iron present in the entire 250 ml of the
solution prepared from Wg of the steel.]

Result: After the experimental analysis the % Fe in the given steel sample is =_________

Quiz:
1. Which is closest to the purest form of the iron?
a) Cast Iron b) Wrought Iron c) Pig Iron d) Steel

2. Steel can be hardened quickly by the process of

a) Induction hardening b) Nitriding c) Cyaniding d) Carburizing

3. What happens when Manganese is added to steel?

a) Decreases strength and hardness of steel b) improves corrosion resistance

c) Decreases ductility d) improves strength and hardness of steel

4. Which of the following is added to steel to increase resistance to corrosion?

a) Carbon b) Manganese c) Sulfur d) Copper

5. Steel is mainly an alloy of

a) Iron and Carbon b) Sulphur and Zinc c) Zinc and tin d) Phosphorous and Tin

6: How else could you determine the end points in dichromate and permanganate titrations?
7: A solid is known to contain iron(III). Outline how you could determine the iron content using a redox
titration.

8: Calculate the mass of Fe In 21.6 g Fe2O3,

9: Enlist different types of steel with % of carbon in them.

10: Enlist three applications of redox titration.

Suggested Reference:
Laboratory Manual of Engineering Chemistry, by S K. Bhasin & Sudha Rani. Publisher: Dhanpat Rai
Publishing Company Ltd. (as per GTU Syllabus)
Inorganic quantitative analysis, Vogel

References used by the students: (Sufficient space to be provided)

Rubric wise marks obtained:

Rubrics 1 2 3 4 5 Total
Marks
 Experiment No: 8
To determine the amount of copper in a given brass sample.
Date:

Competency and Practical Skills:

1. Able to perform the test with accuracy and safety rules

2. Able to do titration and use standard solutions.
3. Able to calculate the composition of brass samples.

Relevant CO’s : CO4: Select the appropriate chemical material and utilization of it.
CO5: Interpret the methods of science as a logical means of problem solving
Objectives: (a) To describe types of brass alloys and constituents.
(b) To show the difference between brass and bronze alloys.
(c) To demonstrate the brass analysis work in the laboratory.
(b) To estimate copper content of brass sample

Glassware/Instruments: Burette, Pipettes rent, Erlenmeyer flasks, Measuring cylinder, burner

Chemicals: Brass sample, KI, NH4OH, acetic acid, Nitric acid, freshly prepared starch solution

Theory:
● Brass is mainly used for making statues, utensils, conducting wire etc. Different types of
alloy contain different compositions of its constituents. The main constituent of brass alloy
is 50 – 90 % copper and 20 – 40 % zinc, small quantities of tin, lead and iron etc.
● A solution of brass is made by dissolving the sample in a minimum amount of nitric acid.
● The dissolved oxides of nitrogen in the solution are expelled by boiling with urea. aftre it
the solution is neutralized by NH4OH and made into a slight acidic medium with HAc.
● KI is added and the cupric ion present in the brass solution oxidizes KI to iodine. The iodine
liberated is titrated against sodium thiosulphate using starch as indicator.
● The volume of sodium thiosulphate consumed is the measure of the amount of copper
present in the solution and sodium thiosulphate is commonly known as hypo.

Reactions:

Safety and necessary Precautions:

● Wear lab coat, safety glasses and gloves.
● Avoid skin and eye contact with chemicals.
● In case of skin contact, rinse the area for several minutes. For eye contact, flush eyes with
water and seek immediate medical advice.

Procedure:
PART-A : Preparation of brass solution (Sample Solution)
1. Carefully weigh about 0.5 g of the given brass pieces accurately using an electronic balance
 and transfer it into a clean conical flask.
2. Add two test tubes of 1:1 nitric acid and cover the mouth of the flask with a glass funnel.
3. Gently warm the solution to dissolve the brass piece completely and add two test tubes of
distilled water.
4. Add about two grams of urea and continue the heating until the reddish brown fumes of
oxides of nitrogen are expelled completely.
5. Cool the solution to room temperature and transfer the solution of brass into a clean 250 ml
standard measuring flask (SMF).
6. Make up the solution to the mark by adding distilled water and mix well for uniform
concentration.

Observations:
Part-A:
Weight of brass foils / pieces taken = W = ________ g
Time taken for dissolution of the brass sample = ________ min
Procedure:
PART-B: Estimation of copper (titration)

1. Pipette out 25 ml of brass solution into a clean conical flask and add dilute ammonium hydroxide
drop by drop until bluish white precipitate is formed.
2. Dissolve the ppt. by adding dilute acetic acid drop by drop and then add ¼ test tubes of acetic acid
in excess.
3. Add one test tube of 10% potassium iodide solution and shake well.
4. Titrate the liberated iodine against standard sodium thiosulphate solution taken in a burette using
starch as indicator towards the end point. (Add starch indicator when the brown solution changes to
whitish yellow).
5. Observe the color change in the flask carefully, disappearance of the blue color is the end point.
6. Note down the volume of hypo added and repeat the experiment for concordant values.
7. Calculate the percentage of copper in the given sample of brass.

Observations:
Part-B:
Burette: ____________________________
Conical flask: _______________________________________________________
_______________________________________________________
_______________________________________________________
Indicator: _______________________________
End point: _______________________________
Normality of hypo = ………….. (a) N
One gram equivalent weight of copper = 63.54
 Tabulation for reading of titration

Sr. No. Burette readings (ml) Concordant

V ml
Initial Final Difference

From the table: Volume of hypo required = V= _ _ _ _ _ _ ml

Calculation:
1000 ml of 1 N of hypo = one gm. equivalent weight of copper ( 63.54 )

V ml of (a) N hypo = X = Vx(a)Nx63.54 / 1000

X = _________ g of copper

Weight of copper present in 25 ml of brass solution = X = ________ g

Weight of copper present in 250 ml of brass solution = Y = (X x 250) / 25

= X x 10
= ________ g

Percentage of copper in the given brass sample = (Y x 100) / Weight of brass taken (W)

= ________ %

Result:

Percentage of copper in the given brass sample is = ________ %

Quiz:

1. Which of the following attributes explain why pure metals are not frequently used in engineering
applications?
a) Softness b) Hardness c) Brittleness d) Luster

2. What is the name of the alloy of copper called which contains a composition of 30-35% of zinc?
a) Bronze b) Duralumin c) Magnalium d) Brass
 3. Which among the following is an ore of copper?
a) Hematite b) Magnetite c) Chalcopyrite d) Siderite

4. Give the role of starch in this experiment.

5. Why is it also known as iodometric titration?

6. Why is potassium iodide solution during the analysis work?

7. Why should the endpoint be observed carefully?

8. Give importance to reddish brown fumes in this experiment.

9. Is it compulsory to warm the solution to dissolve the brass piece completely?

10. What is the role of acetic acid here in this experiment?

Suggested Reference:
Laboratory Manual of Engineering Chemistry, by S K. Bhasin & Sudha Rani. Publisher: Dhanpat Rai
Publishing Company Ltd.
. Practical Engineering Chemistry by K. Mukkanti, etal, B.S. Publications, Hyderabad.

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 Experiment No: 9
To study the rate of corrosion by weight loss method.
Date:

Competency and Practical Skills:

1. Explain the physical properties of metals

2. Distinguish between metals and nonmetals
3. Able to explain corrosion
4. Able to perform the test with accuracy and safety rules

Relevant CO’s : CO3: Describe the importance and relevance of chemistry in our everyday life.
CO4: Select the appropriate chemical material and utilization of it.

Objectives: (a) To show the losses incurred by corrosion.

(b) To show difference in corrosion rate for metal and alloys
(c) To describe various corrosion protection methods
(b) To estimate corrosion rate of given sample.

Glassware/Instruments: beaker, corrosion coupon//sample, tripod stand, thread, weighing

balance,

Chemicals: Hydrochloric acid/ corrosion media

Theory:
● When metals come into contact with certain substances in the air or water, they undergo a
chemical change that causes destruction of the metal. This process is called corrosion.
● When a metal corrodes or deteriorates, it cannot hold the same loads as it did before
corrosion began. At a certain point, corrosion can lead to dangerous conditions.
● The metals used in bridges, railroad tracks, and buildings are all subject to corrosion.
Because of this, it is important to monitor and manage corrosion to avoid structural collapse.
● The rate of corrosion is the speed at which any given metal deteriorates in a specific
environment. It is dependent upon environmental conditions as well as the type and
condition of the metal.
● Corrosion rates are normally calculated using mils per year. In other words, the corrosion
rate is based on the number of millimeters penetrated each year.
● We need to calculate following information to determine rate of corrosion:

- Weight loss (the decrease in metal weight during the reference time period)
- Density (density of the metal)
- Area (total initial surface area of the metal piece)
- Time (the length of the reference time period)

● Weight loss method: The simplest method of estimating corrosion losses in plants is weight
loss analysis. A weighted sample (also known as coupon) of the metal or alloy under
consideration is introduced into the corrosive medium and later removed after a reasonable
time interval. The coupon is then cleaned of all corrosion products and is reweighed. The
weight loss is converted to a corrosion rate (CR) or a metal loss (ML), as follows:
Safety and necessary Precautions:
● Wear lab coat and safety glasses and gloves.
● Avoid skin and eye contact with chemicals.
● In case of skin contact, rinse the area for several minutes. For eye contact, flush eyes with
water and seek immediate medical advice.

Procedure:

1. Mild steel strip specimen/alloy (corrosion coupon) of size 4 x2.5 x 0.1cm is prepared and
cleaned thoroughly.
2. The specimen or corrosion coupons are weighed and the weight is noted as W1.
3. In a beaker, 100 ml of 1 m HCl was taken and the MS strip was then immersed in the beaker
with the help of a tripod stand and thread.
4. After 24 hours, the test strip was withdrawn from the test solution, washed in double
distilled water and dried with acetone and re-weighed. The weight is noted as W2.
5. The weight loss is measured in gm from the difference of weight prior immersion in HCl
and after immersion.
6. From the weight loss the corrosion rate in MPY is calculated using the formula mentioned
above.

Observations:

-In beaker taken solution:

-Density of Mild steel strip/corrosion coupon =

-Mild steel strip/Coupen surface area =

S.No Type Time of Weight prior Weight after Difference

contact immersion(W1) immersion (W1-W2)
(W2)
Calculation:

Result:

The rate of corrosion of the given sample is = …………

Quiz:

1.During corrosion, metals always undergo___________

a) Oxidation b) Reduction c) Disproportionation d) evaporation

2. Coating of Zinc on iron is known as:

a) Galvanizing b) Metal cladding c) Tinning d) Tempering

3. Chemically, the rust is

a) Fe2O3
b) FeO · Fe2O3
c) Fe2O3 · xH2O
d) FeO · xH2O

4. The metal which is protected by a layer of its own oxide:

a) Cu b)Fe c) Au d) Al

5. The corrosion caused by the direct chemical action of environmental gases or anhydrous liquids on the
metal surfaces is called________Corrosion:
a) Dry b) Wet c) Pitting d) Electrochemical

6. Why are buried pipelines connected to Mg through a wire?

7. Which type of Corrosion occurs when zinc metal contains an impurity of copper?

8. State Pilling bed worth rule.

9. What is meant by Tinning?

10 Mention the factors affecting rate of corrosion.

Suggested Reference:
Laboratory Manual of Engineering Chemistry, by S K. Bhasin & Sudha Rani. Publisher: Dhanpat Rai
Publishing Company Ltd.

References used by the students: (Sufficient space to be provided)

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 Experiment No: 10
To Estimate the amount of MnO2 in the given sample of Pyrolusite ore.
.
Date:

Competency and Practical Skills:

1. Possess knowledge about ores and minerals

2. Have knowledge of redox reaction, oxidizing and reducing agents..
3. Able to prepare standard solutions.
4. Able to do required calculations.

Relevant CO’s: CO3: Describe the importance and relevance of chemistry in our everyday life.
CO4: Select the appropriate chemical material and utilization of it.

Objectives: (a) To describe analysis of ores and minerals

(b) To show difference between mineral and ore
(c) To explain redox titration
(b) To estimate amount of MnO2 in the given ore

Glassware/Instruments: pipette, burette, conical flask, beaker, funnel weighing balance

Chemicals: Pyrolusite, oxalic acid, dilute H2SO4, KMnO4

Theory:
● Pyrolusite ore contains a large amount of manganese in the form of manganese dioxide,
MnO2, and little silica. It is a black mineral. Its manganese content is between 60 to 63 %
and silica content is between l0 to l5% .
● MnO2 occurs in nature in the form of pyrolusite. Pyrolusite is not only used as a source of
manganese but also as an oxidizing agent in many industrial processes. For such purposes,
ore is graded on the basis of its available oxygen content rather than on its percentage of
manganese.
● The percentage of MnO2 is usually determined by treatment with an excess of acidified
solution of a reducing agent, such as sodium oxalate. The excess of the reducing agent is
determined by titration with standard KMnO4 where KMnO4 acts as a self indicator with
pale pink color at the end point.

Safety and necessary Precautions:

● Wear lab coat, safety glasses and gloves.

● Avoid skin and eye contact with chemicals.
● In case of skin contact, rinse the area for several minutes. For eye contact, flush eyes with
water and seek immediate medical advice.

Procedure:

1. Weigh out accurately about 0.1g of finely powdered dry Pyrolusite into a conical flask and
 add 25mL of standard N/10 oxalic acid.
2. Add 25mL of 10% H2SO4 and place a short funnel over the conical flask.
3. Boil the contents of the flask gently until no black particles are visible in the flask.
4. Allow it to cool to about 60-70 oC and titrate the excess oxalate with standard N/10 KMnO4.
5. Repeat the above process with 2 other samples of similar weight.
6. Calculate the amount of oxalic acid consumed in the reaction and calculate the percentage
of MnO2 in the Pyrolusite ore.

Observations:

S. No. Volume of Oxalic Burette Reading Volume of

acid used in ml KMnO4
consumed in ml
Initial Final

Calculation:

Weight of ore taken = _____________gm

Volume of N/10 Oxalic acid used =____________mL

Normality of KMnO4 = ___________N

Volume of KMnO4 consumed = _____x_____mL

1mL of KMnO4 = 0.004346g of MnO2

x mL of KMnO4= x*0.004346=____________g of MnO2

Percentage of MnO2 in 100g of ore = Wt of MnO2 obtained *100

Wt. of ore taken

Result:

The % of MnO2 in the given sample of Pyrolusite ore is =................

Quiz:

1. How many moles of KMnO4 will react with 180 gm H2C2O4 according to the given reaction?
 KMnO4 + H2C2O4 → 2CO2 + Mn2+
a) 4/5 b)2/5 c) 1/5 d) 1/3

2. Mn is present in which form in pyrolusite ore;

a) MnO b) MnO2 c)MnSO4 d)MnCl2

3. Pyrolusite is ……….
a) An oxide ore b) A sulfide ore c) Carbonate ore d) Sulphates ore

4. Which of the following indicators is required in the titration of oxalic acid and potassium permanganate?
a) Phenolphthalein b) Methyl red c) Methyl orange d) none

5. The oxidizing agent in the following reaction is:

a) MnO2 b) Oxalic acid c) MnSO4 d) CO2

6. Enlist physical properties of metals?

7. Mn is present in which form in Pyrolusite ore?

8. What is the equivalent weight of KMnO4 in acidic medium?

9. What is the principle of redox titration?

10. MnO2 is used as an oxidizing agent in industries. Give some example in support of this statement

Suggested Reference:
Laboratory Manual of Engineering Chemistry, by S K. Bhasin & Sudha Rani. Publisher: Dhanpat Rai
Publishing Company Ltd.

References used by the students: (Sufficient space to be provided)

Rubric wise marks obtained:

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