4300011_BCH Lab Manual

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Diploma Engineering

Laboratory Manual
BASIC CHEMISTRY
(4300011)
[ Semester : 1 – Chemical (05), Textile Processing Technology (28) ]
[ Semester : 2 – Textile Manufacturing Technology (29),
Printing Technology (58), Textile Designing (59)]

Enrollment No.
Name of the Student
Semester
Programme/Branch
Academic Term
Name of the Institute

Directorate Of Technical Education


Gandhinagar - Gujarat
BASIC CHEMISTRY (4300011)  Laboratory Manual

Certificate

This is to certify that Mr./Ms. ..................................………………………………………………………………….


Enrollment No. ..........................………….……………. of Semester ..……. of Diploma in
………………………………………………......................... Engineering of the Institute
………………………………………………………………………....................................... (GTU Code: ............... )
has satisfactorily completed the term-work in the course BASIC CHEMISTRY (4300011) for the
Academic Year : 202…… - 202…… Term: Odd/Even as prescribed in the GTU curriculum.

Place: …………………..

Date: …………………..

Signature of Course Faculty Head of the Department


BASIC CHEMISTRY (4300011)  Laboratory Manual

Preface

The primary aim of any laboratory/Practical/field work is enhancement of required skills as


well as creative ability amongst students to solve real time problems by developing relevant
competencies in psychomotor domain. Keeping in view, GTU has designed competency focused
outcome-based curriculum -2021 (COGC-2021) for Diploma engineering programmes. In this more
time is allotted to practical work than theory. It shows importance of enhancement of skills amongst
students and it pays attention to utilize every second of time allotted for practical amongst Students,
Instructors and Lecturers to achieve relevant outcomes by performing rather than writing practice in
study type. It is essential for effective implementation of competency focused outcome- based Green
curriculum-2021. Every practical has been keenly designed to serve as a tool to develop & enhance
relevant industry needed competency in each and every student. These psychomotor skills are very
difficult to develop through traditional chalk and board content delivery method in the classroom.
Accordingly, this lab manual has been designed to focus on the industry defined relevant outcomes,
rather than old practice of conducting practical to prove concept and theory.
By using this lab manual, students can read procedure one day in advance to actual
performance day of practical experiment which generates interest and also, they can have idea of
judgement of magnitude prior to performance. This in turn enhances predetermined outcomes amongst
students. Each and every Experiment /Practical in this manual begins by competency, industry relevant
skills, course outcomes as well as practical outcomes which serve as a key role for doing the practical.
The students will also have a clear idea of safety and necessary precautions to be taken while
performing experiment.
This manual also provides guidelines to lecturers to facilitate student-centered lab activities for
each practical/experiment by arranging and managing necessary resources in order that the students
follow the procedures with required safety and necessary precautions to achieve outcomes. It also
gives an idea that how students will be assessed by providing Rubrics.
The selection, characterization, and suitability assessment of natural raw materials essentially
requires principles and concepts of Basic Chemistry for technicians through the inclusion of various
practical exercises, creative activities, etc. Many global problems/issues and their in-depth
understanding is addressed through the inclusion of topics of relevance like solutions, titrations, pH,
electrochemistry, corrosion, water, lubricants, polymers, etc. in this lab manual of the course.
Although we have tried our level best to design this lab manual, but always there are chances
of improvement. We welcome any suggestions for improvement.

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BASIC CHEMISTRY (4300011)  Laboratory Manual

Practical No. 0

DTE’s 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.

DTE’s Mission:
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Institute’s Vision: (Student should write)
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Institute’s Mission: (Student should write)
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Department’s Vision: (Student should write)
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Department’s Mission: (Student should write)
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BASIC CHEMISTRY (4300011)  Laboratory Manual

Programme Outcomes (POs) : (as prescribed by National Board of Accreditation(NBA))

1. Basic and Discipline specific knowledge: Apply knowledge of basic mathematics, science
and engineering fundamentals and engineering specialization to solve the engineering
problems.

2. Problem analysis: Identify and analyse well-defined engineering problems using codified
standard methods.

3. Design/ development of solutions: Design solutions for engineering well-defined


technical problems and assist with the design of systems components or processes to
meet specified needs.

4. Engineering Tools, Experimentation and Testing: Apply modern engineering tools and
appropriate technique to conduct standard tests and measurements.

5. Engineering practices for society, sustainability and environment: Apply appropriate


technology in context of society, sustainability, environment and ethical practices.

6. Project Management: Use engineering management principles individually, as a team


member or a leader to manage projects and effectively communicate about well-
defined engineering activities.

7. Life-long learning: Ability to analyze individual needs and engage in updating in the
context of technological changes in field of engineering.

Programme Specific Outcomes (PSOs) : (Student should write)


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Programme Educational Objectives (PEOs) : (Student should write)


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BASIC CHEMISTRY (4300011)  Laboratory Manual

Practical Outcome - Course Outcome matrix


Course Outcomes (COs):
a. CO-1: Apply the principles of chemical bonding and solutions to solve various engineering problems.

b. CO-2: Solve engineering problems using the concepts of electrochemistry and corrosion.

c. CO-3: Use relevant water treatment methods to solve domestic and industrial problems.

d. CO-4: Classify organic compounds on the basis of their functional groups.

e. CO-5: Choose various types of engineering materials like lubricants, polymers, Elastomers
and Adhesives for domestic and industrial applications.

Sr. No. Practical Outcome/Title of the Experiment CO-1 CO-2 CO-3 CO-4 CO-5

Prepare a standard solution of oxalic acid or


1. - - - -
potassium permanganate. (A)

Determine the strength of the given sodium


hydroxide solution by titrating against
2. - - - -
standard oxalic acid solution using
phenolphthalein indicator. (A)

Standardize potassium permanganate


3. solution by standard oxalic acid solution and - - - -
estimate ferrous ions. (A)

Determine pH-Values of given samples of


4. Solution by using Universal Indicator and pH- - - - -
meter. (A)

Determine the rate of corrosion for different


5. - - - -
metals in the given solution. (A)

Determine the rate of corrosion for metal in


6. - - - -
the solution of different pH. (A)

Estimate total hardness of given water


7. - - - -
sample using standard EDTA solution. (A)

8. Estimate alkalinity of given water sample - - - -

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BASIC CHEMISTRY (4300011)  Laboratory Manual

using 0.01M sulphuric acid solution. (A)

Determine Total Dissolved Solid (TDS) and


9. Total Suspended Solid (TSS) in a given sample - - - -
of water. (A)

Determine the viscosity of the lubricating oil


10. - - - -
using a Redwood viscometer. (A)

Determine the Acid value of the given


11. - - - -
lubricating oil. (A)
Determine flash point and fire point of the
given lubricating oil using Pensky
12. - - - -
Martens/Cleveland open cup/Able’s
flashpoint apparatus. (A)

 (A) indicates ‘Application’ or Higher Cognitive Levels (Analyzing, Evaluating and


Creating) of Action verb/s used in Practical Outcome/Title of the Experiment
according to Revised Bloom’s Taxonomy.

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BASIC CHEMISTRY (4300011)  Laboratory Manual

 Industry Relevant Skills :


The following industry relevant skills are expected to be developed in the students by performance
of experiments of this course.

1. Use principles of Basic Chemistry to solve broadly defined engineering problems.


2. The practical exercises, the underpinning knowledge, and the relevant soft skills associated
with the competency are to be developed in the students to display the COs.

INSTRUCTIONS INCHEMISTRY LABORATORY

 Guidelines to Course Faculty :


1. Course faculty should demonstrate experiment with all necessary implementation strategies
described in curriculum.
2. Course faculty should explain industrial relevance before starting of each experiment.
3. Course faculty should involve & give opportunity to all students for hands on experience.
4. Course faculty should ensure mentioned skills are developed in the students by asking.
5. Utilize 2 hrs of lab hours effectively and ensure completion of write up with quiz also.
6. Encourage peer to peer learning by doing same experiment through fast learners.

 Instructions for Students :


1. Bring this Laboratory Manual regularly.
2. Before entering the lab, students should be aware of the fundamental prerequisites (concepts and
principles), etc., expected, to perform the practical.
3. Have some meal before you come in the chemistry laboratory i.e., don’t come with empty
stomach.
4. According to the timetable, students should regularly report to the Chemistry laboratory.
5. Study the list of Experiments/Practical Outcomes (PrOs) with their COs and Rubrics with Marks
distribution from 0 to 5 considering each of the PrOs Five Criteria for Five miscellaneous
Performance Indicators for Continuous Assessment (CA) of Practicals of the course from this
Laboratory Manual to make yourself well acquainted about it by which you can learn in a very
systematic and scientific way to score well with flying colours.
6. As you enter the lab, place your backpack, water bottle, and any other personal items in the
bookrack.
7. While working in a chemistry lab, always wear an Apron.
8. Each student should keep a record (log) book for any unscheduled writing that occurs when
receiving instructions, performing, being observed, doing calculations, getting results, etc.
9. Maintain a neat and orderly workplace. (Good housekeeping)
10. Always perform experiments in accordance only with correct procedures. Never choose the easy option.
11. Only perform experiments in the lab when you are watched over by a faculty member/s.

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BASIC CHEMISTRY (4300011)  Laboratory Manual

12. Do not be afraid to seek for help from your instructor in any situation. It might have to do with
safety, standard operating procedure, etc. Before moving ahead, make sure you properly
understand each of the instructions.
13. Organize the work in the group. Keep records on the practical observations and do the
calculations as needed, etc. Also complete the Interpretation of results, Conclusion and Answers of
the ‘Practical related quiz’.
14. After usage, store the reagents where they are. Do not change their positions.
15. Submit the lab manual, in time, as and when asked for Continuous Assessment (CA) by the
course faculty member.
16. Students should clean the equipment and glassware after the practical/experiment gets completed.
Store the unused chemicals. Dispose of the unwanted, useless chemicals carefully. Disconnect the
setup you've made and return all the instruments and components you've used after the practical
is completed.
17. Verify that your workspace is clean and dry before leaving the laboratory. Make sure that every water,
electricity, and gas valve is turned off completely.
18. When leaving the lab, fully wash your hands.
19. Student shall attempt to develop related hand-on skills and build confidence.
20. Student shall develop the habits of evolving more ideas, innovations, skills etc.
21. Students shall develop maintenance skills as expected by industries.
22. Student shall refer practical relevant videos, technical magazines, data books, etc.

Follow these DO’s & DON’T’S …to Protect yourself and others :
1. Use extreme caution and maintain good discipline in the laboratory.
2. Before igniting the bunsen burner, be sure that all combustible chemicals have been completely
kept away from it.
3. Any equipment damage should be reported to the lab supervisor if something occurs during
the experiment. While using the chemicals or handling the apparatus (equipment
and/or glassware and/or chemicals), you should use precautions.
4. Food and beverages are not permitted in the lab.
5. Never use pipette by mouth suction for taking out the concentrated solutions.
6. Never pour water directly into any concentrated acid.
7. Chemicals should never be placed directly on the balance pan. When weighing a chemical with a
balance, always use the appropriate weighing container.
8. Avoid using the washbasin to dispose of strong acids. Do not discard any used paper, litmus paper,
or other materials into the sink. Throw them in the dustbin. While not in use, keep the water and
gas knobs closed.

Following SHOULD BE DISPLAYED & ALL SHOULD KNOW TO FOLLOW … :


1. All Chemicals must be properly labeled and stored appropriately.
2. Display all twelve principles of Green Chemistry and all should be followed by everyone to the
maximum possible extent to follow Competency-focused Outcome-based Green Curriculum (COGC)
 2021 of GTU in Chemistry Laboratory also.
3. Display List of Experiments/Practical Outcomes (PrOs) with their COs & Cognitive Levels (R, U and
A) for the action verbs used, Rubrics for Continuous Assessment (CA) for Practicals in the Chemistry
Laboratory to make the students well acquainted about it.

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BASIC CHEMISTRY (4300011)  Laboratory Manual

4. Ventilation and/or Roof ventilation must be there in Chemistry laboratory.


5. When harmful or unpleasant vapours are produced, use the Fume hoods and/or Exhaust fan/s.
6. Standard Safety Signs and Symbols must be displayed in the laboratory.
7. Be familiar with emergency EXIT from the Chemistry Laboratoy.
8. Lab staff, students, and faculty members should be informed of the general Electrical Safety Regulations
that must be followed too.
9. All people should have easy access to Fire Extinguishers and also display its operating procedure
near to it in short.
10. Everyone should have easy access to a First-Aid kit.
11. Emergency Contact Numbers for Gas cylinder supplier / PNG should be displayed in the lab and
known to each one.
12. Everyone in the lab should be aware of and have access to the Important Common Emergency
Numbers.
13. If possible, CCTV cameras should be installed in Chemistry Laboratory for monitoring and safety
purposes.

ALL SHOULD BE WELL AWARE OF … :


1. To prevent accidents from occurring and to respond to them effectively and in a timely
manner, laboratory staff, students, laboratory assistant/s and faculty members should be
well-versed in common safety symbols, signage, emergency exit routes, general electrical
safety guidelines/rules, Important Common Emergency Numbers, etc. and operation of safety
gadgets, fire extinguishers, First-Aid kit, etc to avoid any accident to happen and to manage it
well in time.
2. Students, laboratory assistant/s and faculty members should be knowledgeable about
identifying chemical dangers, storing specific chemicals, using safety and emergency
equipment, and disposing of chemical waste properly.
3. Students, laboratory assistant/s and faculty members should be aware of the proper actions
to take in the event of laboratory accidents, such as chemical spills, fires, explosions,
injuries to the body, chemical burns, heat burns, injuries to the face, glass-related cuts,
inhaling dangerous gases, etc.

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BASIC CHEMISTRY (4300011)  Laboratory Manual

RUBRICS for all PrOs with marks distribution for Continuous Assessment (CA)
of Practicals of Basic Chemistry (4300011) for 25 Marks
PrOs PERFORMANCE INDICATORS for the PrOs Criteria OF STUDENTS in Practical Exercises
Sr. CRITERIA (Each of maximum 5 Marks)
No. (As per GTU Excellent Very Good Good Average Poor
Curriculum) 5 marks 4 marks 3 marks 2 marks 1 mark
⮞ “PROCESS” related skills
- Prepare - Prepare - Prepare - Prepare - Prepare - Prepare
Experimental setup Experimental Experimental Experimental Experimental Experimental
accurately setup accurately setup setup with some setup with the setup poorly
by own satisfactorily by help of faculty help of faculty
1. own member member
- Handling of - Very carefully - Carefully - Good Handling - Proper - Poor Handling of
apparatus/glasswar Handling of Handling of of Handling of apparatus/glassw
es for precise apparatus/glassw apparatus/glassw apparatus/glassw apparatus/glass ares
measurements ares ares ares wares
- Practice and - Practice and - Practice and - Practice and - Practice and - poorly Practice
adapt good and adapt standard adapt very good adapt good and adapt gladly and adapt weak
safe measuring and safe and safe safe measuring and safe and unsafe
techniques measuring measuring techniques measuring measuring
2.
techniques techniques techniques techniques
- Record - Record - Record - Record - Record - Record
observations observations observations observations observations observations
correctly correctly properly satisfactorily partially incorrectly
- Housekeeping - Regularly Keeps - Keeps - Keeps - Sometimes - Keeps
surrounding area surrounding area surrounding area Keeps surrounding area
neat and very very clean clean surrounding unclean
3. clean area clean
- Observance - Strictly Follow - Nicely follow - Follow safety - Sometimes - Rarely Follow
/Follow safety rules safety rules safety rules rules Follow safety safety rules
rules
⮞ “PRODUCT” related skills
- Does Calculations - Did correct - Did precise - Did good - Did - Did incorrect
Calculations with Calculations with Calculations with Calculations Calculations
unit unit unit satisfactorily without unit
without unit
- Interpret the - Interpret the - Interpret the - Interpret the - Interpret the - Interpret the
4.
Results and their Results and their Results and their Results and their Results and Results and their
Conclusion/s Conclusion/s with Conclusion/s with Conclusion/s with their Conclusion/s with
perfect very clear good explanation Conclusion/s unclear
explanation explanation with partial explanation
explanation
- Prepare report of - Perfectly - Properly - Moderately - Partially - Poorly Prepare
practical in Prepare report of Prepare report of Prepare report of Prepare report report of practical
prescribed format practical in practical in practical in of practical in in prescribed
prescribed format prescribed format prescribed format prescribed format
format
5.
- Viva-voce - Answer the - Answer the - Answer the - Able to - Only able to
questions questions with questions, but answer basic answer few basic
effectively with explanations and fails to elaborate questions questions
explanations and elaboration
elaboration
When above Performance Indicator/s for the PrOs Criteria is/are NOT fulfilled at all by the student/s then 0 Mark is to
IMP
given for that criteria.

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BASIC CHEMISTRY (4300011)  Laboratory Manual

Continuous Assessment (CA) Sheet of Practicals of Basic Chemistry (4300011)


Name of the Institute ................................................................................... (GTU Code ............ )
Diploma Engineering - Programme : ...................................................... (Programme Code ......... )
Academic Term : ..................................................... Enrollment No. : ...............................................
Semester : .......... Full Name of the Student : ....................................................................................
PrOs Criteria of Rubrics (refer previous page)
c-1 c-2 c-3 c-4 c-5
TOTAL

- Practice and adapt good and safe


- Handling of apparatus/glasswares
- Prepare Experimental setup

- Observance /Follow safety rules

- Prepare report of practical in


Marks

- Interpret the Results and their


- Record observations correctly
Obtain
Signature

for precise measurements


ed
of the

measuring techniques
Sr. Practical Outcomes (PrOs) / Page out of

- Does Calculations
course

prescribed format
No. Title of the Experiment No. Date 25

- Housekeeping
Faculty

Conclusion/s

- Viva-voce
Member
accurately

Marks Obtained Out Of


(based on Performance Indicator/s for the PrOs Criteria)
5 +5 +5 +5 +5 = 25
Prepare a standard solution
1. of oxalic acid or potassium 13 - -202
permanganate.
Determine the strength of
the given sodium hydroxide
2. solution by titrating against 22 - -202
standard oxalic acid solution
using phenolphthalein
indicator.
Standardize potassium
permanganate solution by 29 - -202
3. standard oxalic acid solution
and estimate ferrous ions.
Determine pH-Values of
4. given samples of Solution 37 - -202
by using Universal Indicator
and pH-meter.

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BASIC CHEMISTRY (4300011)  Laboratory Manual

Determine the rate of


5. corrosion for different 56 - -202
metals in the given solution.
Determine the rate of
6. corrosion for metal in the 63 - -202
solution of different pH.
Estimate total hardness of
7. given water sample using 71 - -202
standard EDTA solution.
Estimate alkalinity of given
8. water sample using 0.01M - -202
80
sulphuric acid solution.
Determine Total Dissolved
9. Solid (TDS) and Total 87 - -202
Suspended Solid (TSS) in a
given sample of water.
Determine the viscosity of
10. the lubricating oil using a - -202
95
Redwood viscometer.
Determine the Acid value of - -202
11. the given lubricating oil. 103

Determine flash point and


fire point of the given
lubricating oil using Pensky - -202
12. 115
Martens/Cleveland open
cup/Able’s flashpoint
apparatus.
128-
 APPENDICES (1 to 4)
135
 ACKNOWLEDGEMENTS 136

Total Marks obtained of all Practicals

Overall (Average) MARKS OBTAINED out of 25 Marks


(GTU Examination Scheme for Practical Marks of CA : 25 Marks (To Pass: 10 Marks))
 Important Note for the Course Faculty Member :
At the end of the term, after the submission of this Laboratory Manual by the student, the Course
Faculty Member should detach this Continuous Assessment (CA) Sheet to keep record for future
aspects.

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BASIC CHEMISTRY (4300011)  Laboratory Manual

Date: ...... - ...... - 202…..

Practical No. 1
Prepare a standard solution of oxalic acid or potassium permanganate.
( Preparation of Primary Standard solution )

A. Objective:
Varieties of solutions are made in chemistry laboratory. Preparing the solutions in
chemistry laboratory is an important and integral part of studying chemistry.

“A solution whose concentration/strength is known accurately is known as


Standard solution.”

There are two types of solutions: Primary standard solution and Secondary
standard solution.

“A solution that is prepared by accurately weighing a known quantity of the solute


followed by its dissolution in a solvent to get the definite volume of the solution is
termed as primary standard solution.”

For a solute, to be Primary standard, it must be stable and non-hygroscopic. Oxalic


acid and Potassium permanganate are known as high purity substances that can
be dissolved separately in a known volume of solvent to produce a primary
standard solution. Primary Standard solutions called titrands are used in chemistry
laboratory or in pharmaceutical field to determine the unknown concentrations of
dissolved substances in other solutions through quantitative determinations. e.g.,
titrations.

B. Expected Program Outcomes (POs):


1. Basic and Discipline specific knowledge
2. Problem analysis
3. Design/Development of solutions
4. Engineering Tools, Experimentation and Testing
5. Engineering practices for society, sustainability and environment
6. Project Management

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BASIC CHEMISTRY (4300011)  Laboratory Manual

C. Expected Skills to be developed based on competency:


The following industry relevant skills are expected to be developed in the students
by performance of this experiment of this course.
Use/Apply basic principles of Applied Chemistry in various engineering
applications to solve broadly defined engineering problems.

D. Expected Course Outcomes (COs):


Apply the principles of chemical bonding and solutions to solve various
engineering problems.

E. Practical Outcomes (PrOs):


1. Calculate the required amount of a given substance using prerequisites.
2. Weigh accurately the required amount of a given substance using electronic
weighing balance.
3. Prepare standard solution of a given substance of requisite molarity and
normality.

F. Expected Affective Domain Outcomes (ADOs):


The ADOs are best developed through laboratory/field-based exercises.
1. Work as a leader/a team member
2. Follow ethical practices
3. Observe safety measures
4. Good housekeeping
5. Time management
6. Practice environmentally friendly methods and processes for the sustainability
of the environment.
7. Handle tools/components/equipment carefully with necessary precautions

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BASIC CHEMISTRY (4300011)  Laboratory Manual

G. Prerequisite Theory:
Molarity :
“The number of gram mole weight of the solute dissolved in 1 litre (1000 mL) of the
solution is known as the molarity of the solution.”
🠚 Its unit is M or mole/L. (It is read as Molar.)
🠚 Molarity of solution = 1000  Weight of substance (g)
Molecular weight of substance  Volume of solution (mL)
1 M solution :
“The solution which contains 1 gram mole weight of the solute per litre (1000 mL)
of the solution is known as 1 molar solution.”
Normality :
“The number of gram equivalent of the solute dissolved in 1 litre (1000 mL) of the
solution is known as the normality of the solution.”
🠚 Its unit is N. (It is read as Normal.)
🠚 Normality of solution = 1000  Weight of substance (g)
Equivalent weight of substance  Volume of solution (mL)
1 N solution :
“The solution which contains 1 gram equivalent weight of the solute per litre (1000
mL) of the solution is known as 1 normal solution.”

H. Experimental set up:

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BASIC CHEMISTRY (4300011)  Laboratory Manual

I. Resources/Equipment Required:
Instrument/Equipment
Sr.
Quanti
/Components/Trainer Specification
No. ty
kit
• Watch glass 2
• Standard volumetric flask with stopper (100 2
1. Glassware (Borosil) mL) 2
• Funnel 2
• Beakers (250 mL, 500mL) 1
• Wash bottle
• Oxalic acid (hydrated) (H2C2O4.2H2O) 5 gm
2. Chemicals (AR Grade) • Potassium permanganate (KMnO4) 5 gm
• Distilled water 1000
mL
Type of Laboratory Balance: Analytical,
Electronic Weighing Sensitivity (mg): 1 mg, Maximum Capacity of
3. weighing (grams): 200 g, Shape of PAN: 1
Balance
Circular, Power Supply: Single Phase, Display:
LED.
J. Safety and necessary Precautions to be followed:
1. While working in the chemistry laboratory use Apron.
2. Handle all the glassware and chemicals/solutions very safely and
carefully.
3. Clean all the glassware thoroughly before using them.
4. Use the chemicals/solutions and distilled water judiciously.
5. Disposal of the used chemicals/solutions should be done through drainage or
by appropriate methods.
6. After completion of this experiment, store the unused solutions for further use
in future.

K. Procedure to be followed :
⮞ Preparation of ......... mL ....... M .............................. solution :
(1) Wash and clean thoroughly all apparatus with distilled water.
(2) Weigh the exact weight of clean and dried watch glass and record its weight in
book.
(3) Calculate the required amount of a given substance using prerequisites as
shown below in Calculations.

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BASIC CHEMISTRY (4300011)  Laboratory Manual

(4) Weigh accurately the required amount ........... g of a given substance


....................................... in a clean dry watch glass using electronic weighing
balance.
(5) Transfer weighed substance into a standard volumetric flask of 100 mL size
using funnel.
(6) Gradually add distilled water using wash bottle to the flask using funnel by
stirring it well to dissolve it and dilute it up to engraved mark i.e., 100 mL.
(7) Using glass stopper close the measuring flask and shake softly the solution 3
to 4 times to get a 100 mL homogeneous solution of requisite concentration
and volume.
(8) Write the observations and results. Also interpret and make conclusion from
it.
⮞ Preparation of ......... mL ....... N ............................... solution :
Follow the above mentioned steps (1) to (8) to prepare the required solution.

L. Calculations & Observations :


⮞ Calculations :
 MOLAR SOLUTIONS :
So based on prerequisites -
🢡 Preparation of 100 mL 0.1 M H2C2O4.2H2O (Oxalic acid (hydrated)) solution :
Molecular weight of H2C2O4.2H2O = 6(H) + 2(C) + 6(O)
= 6(1) + 2(12) + 6(16)
= 6 + 24 + 96

Molecular weight of H2C2O4.2H2O = 126 g/mol

Method : 1 : (‘’ sign indicates ‘equivalent’)


Now, according the definition of 1 M solution, as we know -

1000 mL 1M H2C2O4.2H2O solution  126 g H2C2O4.2H2O

 1000 mL 0.1M H2C2O4.2H2O solution  12.6 g H2C2O4.2H2O


 100 mL 0.1M H2C2O4.2H2O solution  1.26 g H2C2O4.2H2O
Method : 2 :
Weight of H2C2O4.2H2O required = Molarity  Molecular weight  Volume (L)

= 0.1  126  (100/1000)

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BASIC CHEMISTRY (4300011)  Laboratory Manual

 Weight of H2C2O4.2H2O required = 1.26 g


Thus, 1.26 g H2C2O4.2H2O is dissolved in distilled water in standard volumetric
flask upto 100 mL mark to form 100 mL 0.1M H2C2O4.2H2O solution.
Similarly,
🢡 Preparation of 100 mL 0.1 M KMnO4 (Potassium permanganate) solution :
Molecular weight of KMnO4 = 1(K) + 1(Mn) + 4(O)
= 1(39) + 1(55) + 4(16)
= 39 + 55 + 64

 Molecular weight of KMnO4 = 158 g/mol


Now, according the definition of 1 M solution, as we know -

1000 mL 1M KMnO4 solution  158 g KMnO4

 1000 mL 0.1M KMnO4 solution  15.8 g KMnO4


 100 mL 0.1M KMnO4 solution  1.58 g KMnO4

Thus, 1.58 g KMnO4 is dissolved in distilled water in standard volumetric flask upto
100 mL mark to form 100 mL 0.1M KMnO4 solution.

 NORMAL SOLUTIONS :
So based on prerequisites -
🢡 Preparation of 100 mL 0.1 N H2C2O4.2H2O (Oxalic acid (hydrated)) solution :
Equivalent weight of H2C2O4.2H2O = Molecular mass of H2C2O4.2H2O
Basicity of H2C2O4.2H2O

Here, Basicity of H2C2O4.2H2O = No. of replaceable H+ ions in H2C2O4.2H2O = 2

 Equivalent weight of H2C2O4.2H2O = 126


2
 Equivalent weight of H2C2O4.2H2O = 63 g/equivalent
Method : 1 : (‘’ sign indicates ‘equivalent’)
Now, according to the definition of 1 N solution, as we know -

1000 mL 1N H2C2O4.2H2O solution  63 g H2C2O4.2H2O


1000 mL 0.1N H2C2O4.2H2O solution  6.3 g H2C2O4.2H2O
100 mL 0.1N H2C2O4.2H2O solution  0.63 g H2C2O4.2H2O

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BASIC CHEMISTRY (4300011)  Laboratory Manual

Method : 2 :
Weight of H2C2O4.2H2O required = Normality  Equivalent weight  Volume (L)

= 0.1  63  (100/1000)

 Weight of H2C2O4.2H2O required = 0.63 g


Thus, 0.63 g H2C2O4.2H2O is dissolved in distilled water in standard volumetric
flask upto 100 mL mark to form 100 mL 0.1N H2C2O4.2H2O solution.

🢡 Preparation of 100 mL 0.1 N KMnO4 (Potassium permanganate) solution :


Equivalent weight of KMnO4 = Molecular mass of KMnO4
Change in oxidation no. of ‘Mn’
Here, Change in oxidation no. of ‘Mn’ = Difference in valency of ‘Mn’ = 5
 Equivalent weight of KMnO4 = 158
5
 Equivalent weight of KMnO4 = 31.6 g/equivalent
Now, according the definition of 1 N solu tion, as we know -

1000 mL 1N KMnO4 solution  31.6 g KMnO4

 1000 mL 0.1N KMnO4 solution  3.16 g KMnO4


 100 mL 0.1M KMnO4 solution  0.316 g KMnO4

Thus, 0.316 g KMnO4 is dissolved in distilled water in standard volumetric flask


upto 100 mL mark to form 100 mL 0.1N KMnO4 solution.

⮞ Observations :

1. For the preparation of ......... mL ......... M ............................. solution, the


weight of ............................. taken = ................... g.
2. For the preparation of ......... mL ......... N ............................... solution, the weight
of ............................. taken = ................... g.

M. Results :
(1) .................. g ............................. is dissolved in distilled water in standard
volumetric flask upto 100 mL mark to form ......... mL ............... M
............................. solution.
(2) .................. g ............................. is dissolved in distilled water in standard
volumetric flask upto 100 mL mark to form ......... mL ................ N
............................. solution.

N. Interpretation of Results :

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BASIC CHEMISTRY (4300011)  Laboratory Manual

…..................................................................................................................................
.............….....................................................................................................................
.....................................................................................................................................
.....................................................................................................................................
O. Conclusion :
…..................................................................................................................................
.............….....................................................................................................................

P. Practical related Quiz :


(1) What is concentration?
Ans. ..........................................................................................................................
...........................................................................................................................
(2) Define : Molarity.
Ans. ..........................................................................................................................
...........................................................................................................................
(3) Define : 1 Molar solution.
Ans. ..........................................................................................................................
...........................................................................................................................
(4) Define : Normality.

Ans. ..........................................................................................................................
...........................................................................................................................
(5) Define : 1 Normal solution.
Ans. ..........................................................................................................................
...........................................................................................................................
(6) Write the formulae to find the Molarity and Normality of solutions.
Ans. ...........................................................................................................................
...........................................................................................................................
...........................................................................................................................
...........................................................................................................................
...........................................................................................................................
...........................................................................................................................
...........................................................................................................................
(7) Calculate the amount of oxalic acid (hydrated) required to prepare 500 mL
0.02 M oxalic acid solution. [Ans. 1.26 g]

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BASIC CHEMISTRY (4300011)  Laboratory Manual

Ans. ..........................................................................................................................
...........................................................................................................................
...........................................................................................................................
...........................................................................................................................
...........................................................................................................................
...........................................................................................................................
...........................................................................................................................
...........................................................................................................................
...........................................................................................................................

(8) Calculate the amount of KMnO4 required to prepare 250 mL 0.02 N KMnO4
solution. [Ans. 0.158 g]
Ans. ..........................................................................................................................
...........................................................................................................................
...........................................................................................................................
...........................................................................................................................
...........................................................................................................................
...........................................................................................................................
...........................................................................................................................
...........................................................................................................................
...........................................................................................................................

Q. References / Suggestions :
https://youtu.be/OtiUJn1PZ9I
Students should search and write any one reference relevant to this experiment
................................................................................................................................

R. Assessment-Rubrics
As mentioned in (1) Rubrics (Pg. 10) and (2) Continuous Assessment (CA) (Pg. 11) is
to be done by the course faculty member.

 Remarks (if any) : .......................................................................................................

 Signature of the course Faculty Member with Date : ...............................................

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BASIC CHEMISTRY (4300011)  Laboratory Manual

Date: ...... - ...... - 202…..

Practical No. 2
Determine the strength of the given sodium hydroxide solution by titrating against
standard oxalic acid solution using phenolphthalein indicator.
( ACID-BASE TITRATION – Weak Acid and Strong Base )

A. Objective:

When acid and base react with each other - salt and water formation occurs. This
process is called Neutralization. Basis on this process we can determine unknown
concentration of acid or base solution. This method is known as Acid-Base
Titration. In the acid-base reaction at the end-point indicator shows colourchange.
So, we can judge the end-point. By this method we can calculate the amount of
acid or base present in its solution. Acid-base titrations are used in pharmaceutical
field to determine the concentration of solutions.

B. Expected Program Outcomes (POs):


1. Basic and Discipline specific knowledge
2. Problem analysis
3. Design/Development of solutions
4. Engineering Tools, Experimentation and Testing
5. Engineering practices for society, sustainability and environment
6. Project Management

C. Expected Skills to be developed based on competency:

This practical is expected to develop the following skills for the industry-
identified competency:
Use/Apply basic principles of Basic Chemistry in various engineering
applications.

D. Expected Course Outcomes (COs):


Apply the principles of chemical bonding and solutions to solve various engineering
problems.

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BASIC CHEMISTRY (4300011)  Laboratory Manual

E. Practical Outcomes (PrOs):


1. To demonstrate Titrimetric Analysis-Acidimetry experiment. i.e., Accurately
titrate the titrant/titrator (solution in conical flask) against titrand (solution in
burette) using indicator.
2. Calculate the unknown concentration of given acid or base using data recorded
from the experiment performed.

F. Expected Affective Domain Outcomes (ADOs):


1. Work as a leader/a team member
2. Follow ethical practices
3. Observe safety measures
4. Good housekeeping
5. Time management
6. Practice environmentally friendly methods and processes for the sustainability
of the environment.

G. Prerequisite Theory:
 Strong Acid: An acid which ionizes completely (almost 100%) in its aqueous
solution is called a strong acid. e.g., HCl, H2SO4, HNO3, etc.
 Weak Acid: An acid which ionizes partially/slightly (about 2 to 3 %) in its
aqueous solution is called a weak acid. e.g., H2C2O4, HCOOH, CH3COOH, etc.
 Strong Base: A base which ionizes completely (almost 100%) in its aqueous
solution is called a strong base. e.g., NaOH, KOH, Ba(OH)2, etc.
 Weak Base: A base which ionizes partially/slightly (about 2 to 3 %) in its
aqueous solution is called a weak base. e.g., NH4OH, Na2CO3, NaHCO3, etc.
 Titration: The solution of unknown concentration of definite volume is allowed
to react chemically with the other solution having known concentration. This
method of determining the exact volume of a solution having unknown
concentration is known as titration.
🠚 So, titration is the technique used to find the unknown concentration of a
chemical component present in a given sample.
🠚 Types of Titrations: (1) Acid-Base titration (2) Redox titration (3)
Precipitation titration (4) Complexometric titration
 Indicator: Indicator is a weak acid or a weak base which changes its own colour
at the end of titration (neutralization) indicating the completion of the
reaction.
🠚 e.g., Phenolphthalein, Methyl orange, Orange-Red, Methylene blue, Starch,
EBT (Erichrome Black-T) etc.

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BASIC CHEMISTRY (4300011)  Laboratory Manual

H. Experimental set up:

I. Resources/Equipment Required:
Sr. Instrument/Equipment Specification Quanti
No.
/Components/Trainer kit ty

• Funnel 1
• Burette (50mL) 1
• Burette stand 1
1. Glassware (Borosil) • White glazed tile 1
• Conical flask (100 mL) 1
• Pipette (10mL) 1
• Wash bottle
1
• Beakers (250 mL, 100mL)
1
• x M NaOH solution
• 0.1 M Oxalic acid (H2C2O4.2H2O) As per
2. Chemicals (AR Grade) the
solution (Standard solution)
• Phenolphthalein indicator need
• Distilled water

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BASIC CHEMISTRY (4300011)  Laboratory Manual

J. Safety and necessary Precautions followed:


a. While working in the chemistry laboratory use Apron.
b. Handle all the glassware and chemicals/solutions very safely and
carefully.
c. Clean all the glassware thoroughly before using them.
d. Use the chemicals/solutions and distilled water judiciously.
e. Disposal of the used chemicals/solutions should be done through drainage or
by appropriate methods.
f. After completion of this experiment, store the unused solutions for further use
in future.

K. Procedure to be followed:
1. Clean the burette properly with distilled water and finally rinse it with sodium
hydroxide (NaOH) solution. Clamp the burette vertically in a burette stand.
2. Fill the burette with sodium hydroxide (NaOH) solution through a funnel above
the zero mark.
3. Remove the air gap from the nozzle of the burette by running the solution
forcefully from it.
4. Don’t keep funnel on the burette while taking and noting the reading. Also, see
that no drop of the liquid is hanging at the nozzle of the burette.
5. Note the reading by keeping the eye exactly at the same level of the lower
meniscus of the filled solution. Now, set the burette level at zero mark.
6. Pipette out 10 mL of oxalic acid solution in a cleaned conical flask.
7. Add 2 drops of phenolphthalein indicator into the conical flask. And put the
flask on the glazed tile. Titrate the acid with sodium hydroxide solution with
constant stirring the solution till a very faint permanent pink colour is obtained.
8. Note the reading from the burette and record it as final reading.
9. Repeat the procedure until three concordant readings are obtained. Record
your readings in Observation Table.

L. Observations, Observation Table, Chemical Equation and Calculations:


⮞ Observations:
• Burette: x M sodium hydroxide solution (Titrand)
• Conical flask (using Pipette): 10 mL 0.1 M standard solution of oxalic acid
(Titrant / Titrator)
• Indicator: 2-3 drops of Phenolphthalein
• Colour change (at the end point): Colourless to a very faint permanent pink
colour

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BASIC CHEMISTRY (4300011)  Laboratory Manual

⮞ Observation Table:
Mean (Average)
Burette Pilot reading I II III
reading,
Reading (mL) (mL) (mL) (mL)
(mL) = (I + II + III)/3
mL
Final reading mL mL mL
(Whole No.)
Initial reading 0.0 mL mL mL mL V2 = ............mL
Difference mL
mL mL mL
= F.r.–I.r. (Whole No.)
Thus, 10 mL 0.1 M Oxalic acid (H2C2O4.2H2O) solution requires
V2 =............... mL of x M NaOH solution for neutralization.

⮞ Chemical Equation:
H2C2O4(aq) + 2NaOH(aq) 🠚 Na2C2O4(aq) + 2H2O(aq)
⮞ Calculations:
(1) Molarity of NaOH solution :
a1M1V1 = a2M2V2 ;where, a1 = basicity (replaceable H+) of oxalic acid=2
M1 = molarity of the oxalic acid solution = 0.1 M
V1 = volume of the oxalic acid solution = 10 mL
a2 = acidity (replaceable OH-) of sodium hydroxide = 1
M2 = molarity of the sodium hydroxide solution = xM
V2 = volume of the sodium hydroxide solution = ............mL

 M 2 = a1 M 1 V1
a2 V 2

 M2 = 2 × 0.1 × 10
1 × ………..

 M2 = ............ M NaOH solution

(2) Strength (g/L) of NaOH solution:


Strength (Concentration) of NaOH solution in g/L = Molarity of NaOH solution
× Molar mass of NaOH
= ..............× 40 g/L

 Strength of NaOH solution = .............. g/L

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BASIC CHEMISTRY (4300011)  Laboratory Manual

M. Results:
The strength (concentration) of the given NaOH solution is ............. g/L.

N. Interpretation of Results :
…..................................................................................................................................
.............….....................................................................................................................
.....................................................................................................................................

O. Conclusion :
…...................................................................................................................................
..............….............................................................................................................

P. Practical related Quiz :


1. Which is/are the strong base/s among the following?
a. NaOH
b. KOH
c. Na2CO3
d. NH4OH
Ans. .......................................................................................................................
2. Which is/are the strong acid/s among the following?
a. HCl
b. H2SO4
c. HNO3
d. (COOH)2
Ans. .......................................................................................................................
3. Define : Titration.
Ans. .......................................................................................................................
.......................................................................................................................
.......................................................................................................................
.......................................................................................................................
4. Write the names of types of titrations.

Ans. .......................................................................................................................
.......................................................................................................................

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BASIC CHEMISTRY (4300011)  Laboratory Manual

5. What is indicator?
Ans. .......................................................................................................................
.......................................................................................................................
.......................................................................................................................
6. Write three names of indicator.
Ans. .......................................................................................................................
.......................................................................................................................
7. What type of reaction is an acid-alkali titration?
Ans. .......................................................................................................................
8. Write chemical equation for this experiment.
Ans. .......................................................................................................................

Q. References / Suggestions:
1. Laboratory Manual Chemistry, NCERT Publication
2. https://en.wikipedia.org/wiki/Acid%E2%80%93base_titration
3. https://vlab.amrita.edu/?sub=2&brch=193&sim=352&cnt=4
4. Figure source: https://pediaa.com/difference-between-standardization-and-
titration/
5. https://www.youtube.com/watch?v=1J9ozb6nB48
Students should search and write any one reference relevant to this experiment
..........................................................................................................................

R. Assessment-Rubrics:
As mentioned in (1) Rubrics (Pg. 10) and (2) Continuous Assessment (CA) (Pg. 11) is
to be done by the course faculty member.

 Remarks (if any) : ...................................................................................................

 Signature of the course Faculty Member with Date : ..........................................

28 | Page
BASIC CHEMISTRY (4300011)  Laboratory Manual

Date: ...... - ...... - 202…..

Practical No. 3
Standardize potassium permanganate solution by standard oxalic acid solution and
estimate ferrous ions.
( REDOX TITRATION )

A. Objective:

The amount of ferrous (Fe2+) ions present in the given solution can be determined
by redox titration. In Redox titration oxidation and reduction takes place
simultaneously. Here KMnO4 acts as an oxidizing agent. This titration is carried out
in acidic medium & hot condition. Ferrous ions solution is titrated against KMnO4
solution. By this titration we can determine amount of Fe2+ ions. Here oxalic acid is
used to standardize KMnO4 solution.

B. Expected Program Outcomes (POs):


1. Basic and Discipline specific knowledge
2. Problem analysis
3. Design/Development of solutions
4. Engineering Tools, Experimentation and Testing
5. Engineering practices for society, sustainability and environment
6. Project Management

C. Expected Skills to be developed based on competency:


The following industry relevant skills are expected to be developed in the students
by performance of this experiment of this course.
Use/Apply basic principles of Basic Chemistry in various engineering applications
to solve broadly defined engineering problems.

D. Expected Course Outcomes (COs):


Solve engineering problems using the concepts of electrochemistry and corrosion.

E. Practical Outcome (PrOs):


1. Standardize KMnO4 solution by standard oxalic acid solution.
2. Estimate ferrous (Fe2+) ions in terms of normality, molarity and g/l.

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BASIC CHEMISTRY (4300011)  Laboratory Manual

F. Expected Affective Domain Outcomes (ADOs):


The ADOs are best developed through laboratory/field-based exercises.
1. Work as a leader/a team member
2. Follow ethical practices
3. Observe safety measures
4. Good housekeeping
5. Time management
6. Practice environmentally friendly methods and processes for the sustainability
of the environment.
7. Handle tools/components/equipment carefully with necessary precautions.

G. Prerequisite Theory:
Permanganate ion is a powerful oxidizing agent, especially in acidic solution,
which can be used to analyse solutions. In these titration reactions, the intensely
coloured permanganate ion (O.N. of Mn = +7) is reduced to form the colourless
manganese ion (O.N. of Mn = +2). An advantage to using this is that it is “self-
indicating”. As long as the reducing agent remains present in the sample, the
colour of permanganate quickly disappears as it is reduced. However, at the
endpoint, all the reducing agent has been used up so the next drop of
permanganate solution is sufficient to cause a visible colour change. So, at the
endpoint, we know the oxidizing agent and reducing agent have reacted exactly in
proportion to their stoichiometry in the balanced redox reaction. If we know how
much of the oxidizing agent we added, then we can figure out how much reducing
agent was present in the unknown.
“The reaction in which oxidation and reduction half-reactions take place
simultaneously is called a redox reaction.”

H. Experimental set up:

30 | Page
BASIC CHEMISTRY (4300011)  Laboratory Manual

I. Resources/Equipment Required:

Sr. Instrument/Equipment
Specification Quantity
No. /Components/Trainer kit
• Funnel 1
• Burette(50mL) 1
• Burette stand 1
• White glazed tile 1
1. Glassware (Borosil) • Conical flask (100 mL) 1
• Pipette (10 mL) 1
• Wash bottle 1
• Beakers (250 mL, 100 mL) 1
0.1 N H2C2O4.2H2O (hydrated As per
oxalic acid) solution requirem
KMnO4 solution ent
2. Chemicals (AR Grade)
x N FeSO4.7H2O solution
Dilute H2SO4 solution
Distilled Water

J. Safety and necessary Precautions followed:


1. While working in the chemistry laboratory use Apron.
2. Handle all the glassware and chemicals/solutions very safely and
carefully.
3. Clean all the glassware thoroughly before using them.
4. Use the chemicals/solutions and distilled water judiciously.
5. Disposal of the used chemicals/solutions should be done through drainage or
by appropriate methods.
6. After completion of this experiment, store the unused solutions for further use
in future.

K. Procedure to be followed:
PART – 1: To Standardize KMnO4 solution

1. Wash all glassware with water.


2. Clamp the burette in the burette stand.
3. Fill the burette with x N KMnO4 solution and set it upto zero mark.
4. Take 10ml 0.1 N oxalic acid solution by pipette and transfer into conical flask.
5. Add 1 to 1½ test-tube of dilute H2SO4 in the conical flask and heat it to 60o-
70oC. (Just vapours come out.)
6. Titrate this hot mixture by adding drop by drop KMnO4 solution from burette.

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BASIC CHEMISTRY (4300011)  Laboratory Manual

7. When permanent light pink colour is observed, stop the addition of KMnO4
solution from the burette.
8. First take pilot reading and note-down in observation table.
9. Then take three accurate readings by repeating above procedure.
10. By calculations find the strength of x N KMnO4 solution.

2+
PART – 2: To Estimate Fe ions present in FeSO4.7H2O solution

1. Wash all glassware with water.


2. Clamp the burette in the burette stand.
3. Fill the burette with ......... N KMnO4 solution and set it upto zero mark.
4. Take 10 ml x N FeSO4.7H2O solution by pipette and transfer into conical flask.
5. Add 1 to 1½ test-tube of dilute H2SO4 in the conical flask.
6. Titrate this mixture by adding drop by drop KMnO4 solution from burette.
7. When permanent light pink colour is observed, stop the addition of KMnO4
solution from the burette.
8. First take pilot reading and note down in observation table.
9. Then take three accurate readings by repeating above procedure.
10. By calculations find the strength of x N FeSO4.7H2O solution.

L. Observations, Observation Tables, Chemical Equations and Calculations:


For PART – 1 :

⮞ Observations:
 Burette: x N KMnO4 solution (Titrand)
 Conical flask (using Pipette): 10 ml 0.1N oxalic acid solution (Titrant/Titrator) +
1 to 1½ test-tube of dilute H2SO4 + HEAT
 Indicator: KMnO4 self-indicator
 Colour change (at the end point): Colourless to Light Pink
⮞ Observation Table:

Mean (Average)
Burette Pilot reading I II III
reading, (mL)
Reading (mL) (mL) (mL) (mL) V1 = (I + II + III)/3
mL
Final reading mL mL mL
(Whole No.)
Initial reading 0.0 mL mL mL mL V1 = ............ mL
Difference mL
mL mL mL
= F.r. – I.r. (Whole No.)
Thus, 10 mL 0.1N oxalic acid solution requires V1 = ……..ml of KMnO4 solution for its
complete oxidation.

32 | Page
BASIC CHEMISTRY (4300011)  Laboratory Manual

⮞ Chemical Equation:
2KMnO4(aq) + 3H2SO4(aq) + 5H2C2O4(aq) 🠚 2MnSO4(aq) + 8H2O(l) + 10CO2(g)
⮞ Calculations: (for PART-1)
To find Normality of KMnO4 solution (N1) :

N1  V1 = N2  V2 N1 = Normality of KMnO4 solution = x N = ?


V1 = Volume of KMnO4 solution = ……. ml
 N1  …….. = 0.1  10
N2 = Normality of oxalic acid solution = 0.1 N
 N1 = 0.1 x 10
V2 = Volume of oxalic acid solution = 10 ml
……..

 N1 = ................N KMnO4 solution

For PART – 2 :

⮞ Observations:
 Burette: ............. N KMnO4 solution (Titrand)
 Conical flask (using Pipette): 10 ml y N FeSO4.7H2O solution + 1 to 1½ test-
tube of dilute H2SO4 solution
 Indicator: KMnO4 self-indicator
 Colour change (at the end point): Colourless to Light Pink
⮞ Observation Table:

Pilot reading Mean (Average)


Burette I II III
(mL) reading, (mL)
Reading (mL) (mL) (mL) V2 = (I + II + III)/3
(Whole No.)
Final reading mL mL mL mL
Initial reading 0.0 mL mL mL mL V2 = ........... mL
Difference mL
mL mL mL
= F.r. – I.r. (Whole No.)
Thus, 10 ml of y N FeSO4.7H2O solution requires V2=……..ml of ......... N KMnO4 solution
for its complete oxidation.

⮞ Chemical Equation:
2KMnO4(aq) + 10FeSO4(aq) + 8H2SO4(aq) 🠚 K2SO4(aq) + 2MnSO4(aq) + 5Fe2(SO4)3(aq) + 8H2O(g)
⮞ Calculations: (for PART-2)

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BASIC CHEMISTRY (4300011)  Laboratory Manual

(1) To find Normality of FeSO4.7H2O solution (N2) :N1

 V1 = N 2  V2 N1 = Normality of FeSO4.7H2Osolution = y N = ?

 N1  10 = ……..  …….. V1 = Volume of FeSO4.7H2O solution = 10 ml

 N1 = ……..  …….. N2 = Normality of KMnO4 solution = ……. N

10 V2 = Volume of KMnO4 solution = ……. ml

 N1 = ............. N FeSO4.7H2Osolution

(2) Molecular mass of FeSO4.7H2O = 1(Fe) + 1(S) + 14(H) + 11(O)


= 1(56) + 1(32) + 14(1) + 11(16)
= 56 + 32 + 14 + 176

 Molecular mass of FeSO4.7H2O = 278 g/mol

(3) Equivalent mass of FeSO4.7H2O = Molecular mass of FeSO4.7H2O


Change in oxidation number of Fe
Here, Change in oxidation number of Fe = 1 (as Fe2+ changes to Fe3+)

= 278
1
 Equivalent mass of FeSO4.7H2O = 278 g/equivalent

(4) To find Molarity of FeSO4.7H2O solution (M) :

Molarity  Molecular mass = Normality  Equivalent mass

 Molarity  278 = ………  278

 Molarity = ........ M FeSO4.7H2Osolution

(5) To find strength of FeSO4.7H2O solution in g / l :

g / l = Normality of FeSO4.7H2Osolution  Equivalent mass of FeSO4.7H2O

 g / l = ……..  278

 g / l = ......... g / l of FeSO4.7H2O solution

34 | Page
BASIC CHEMISTRY (4300011)  Laboratory Manual

M. Results :
1. Normality of FeSO4.7H2O solution = ............... N.
2. Molarity of FeSO4.7H2O solution = ............... M
3. Strength of FeSO4.7H2O solution = ............... g/l

N. Interpretation of Results :
…..................................................................................................................................
.............….....................................................................................................................
.........................................................................................................................

O. Conclusion :
…...................................................................................................................................
..............….............................................................................................................

P. Practical related Quiz :


1. Define: Redox reaction.
Ans. .......................................................................................................................
.......................................................................................................................
.......................................................................................................................

2. Why sufficient quantity of dilute H2SO4 is added in this titration?


Ans. .......................................................................................................................
3. What is the oxidizing agent and the reducing agent in this experiment?
Ans. .......................................................................................................................
.......................................................................................................................
4. Write the names and chemical formula of any three oxidizing agents and
three reducing agents.
Ans. .......................................................................................................................
.......................................................................................................................
.......................................................................................................................
.......................................................................................................................
.......................................................................................................................
.......................................................................................................................

5. Which solution is used for the standardization of KMnO4 solution?

Page | 35
BASIC CHEMISTRY (4300011)  Laboratory Manual

Ans. .......................................................................................................................

6. Write redox equations for this experiment for part-I and part-II.
Ans. .......................................................................................................................
.......................................................................................................................

Q. References / Suggestions:
1. https://dbchhag.blogspot.com
2. https://www.youtube.com/watch?v=HDUd4KqBKa8&t=124s
3. https://www.youtube.com/watch?v=bHkFSavcU5I
4. https://www.youtube.com/watch?v=LA0wbCkczAE
5. Figure source:
https://pediaa.com/difference-between-standardization-and-titration/
6. https://www.youtube.com/watch?v=1J9ozb6nB48
Students should search and write any one reference relevant to this experiment
.........................................................................................................................

R. Assessment-Rubrics:
As mentioned in (1) Rubrics (Pg. 10) and (2) Continuous Assessment (CA) (Pg. 11) is
to be done by the course faculty member.

 Remarks (if any) : ...................................................................................................

 Signature of the course Faculty Member with Date : ..........................................

36 | Page
BASIC CHEMISTRY (4300011)  Laboratory Manual

Date: ...... - ...... - 202…..

Practical No. 4
Determine pH-Values of given samples of Solution by using Universal Indicator and
pH-meter.
( pH Measurement )

A. Objective:
Chemical, biochemical and bio-mineralization reactions are highly pH sensitive.
Water is the cheapest and most abundant chemical available on the earth. Many
industries consume water as a raw material and / or as a reagent in the
manufacture of drugs, detergents, cosmetics, cements, fertilizers, varnishes,
paints, lubricants, polymers, adhesives, elastomers, ceramics, etc. Hence proper
pH should be maintained throughout the reaction. Fertility of soil, waste water
and drinking water treatments, corrosion and electrolysis are also pH dependant.
Therefore, determination of pH of a given sample is important and should be
carried out precisely. So pH has high significance.

B. Expected Program Outcomes (POs)


1. Discipline knowledge: Apply knowledge of engineering chemistry to
solve various engineering problems.
2. Problem Analysis: Plan to perform experiments and practices to use the
results to solve engineeringproblems.
3. Design/ development of solutions: Use relevant lubricants for domestic
and industrial applications.

C. Expected Skills to be developed based on competency:


‘Use/Apply basic principles of Basic chemistry to solve broadly-defined
engineering problems.’
1. Determination of pH of a given sample.

2. Selection of proper method of pH measurement.

Page | 37
BASIC CHEMISTRY (4300011)  Laboratory Manual

D. Expected Course Outcomes(COs):


Solve engineering problems using the concepts of electrochemistry and corrosion.

E. Practical Outcomes (PrOs):


1. Calibration of pH meter.
2. Selection of proper method of pH measurement.
3. Determination of pH of a given sample.

F. Expected Affective domain Outcome (ADOs):


1. Work as a leader/a team member.
2. Follow safety measures.
3. Follow ethical practices.
4. Time management.
5. Practice good housekeeping.

G. Prerequisite Theory:
pH means potential / power (potenz German word) of Hydrogen ion in solution.
pH scale was introduced by Danish biochemist Sorensen in 1923. This scale is
applicable to only very dilute aqueous solutions and pure water (distilled water) to
+
magnify the lower concentration of H(aq) ions present in them. For non-aqueous
solutions this scale is not applicable.
“pH of an aqueous solution is the negative logarithm of molar (mol/litre)
concentration of hydronium (H3O+ (aq)
) (or hydrogen H+ (aq)
) ions present in an
aqueous solution to the base 10.”

pH =  log10[H3O+] =  log10[H+]
🠚 pH has no unit.
🠚 pH ranges from 0 to 14.
🠚 If pH is 0 to less than 7, the aqueous solution is acidic in nature.
🠚 If pH is equal to 0, the aqueous solution is neutral in nature.
🠚 If pH is more than 7 to 14, the aqueous solution is basic in nature.

38 | Page
BASIC CHEMISTRY (4300011)  Laboratory Manual

Similarly, pOH can be defined and can be mathematically expressed as

pOH =  log [OH-]


Also, pH + pOH = 14

🠚 Approximate pH value of the given dilute aqueous solutions can be obtained by


using Universal indicator and pH paper.
🠚 Absolute (Accurate) pH value of the given dilute aqueous solutions can be
obtained by using Digital pH-meter.

H. Experimental set up:

Digital pH meter

I. Resources/Equipment Required:

Sr. Instrument/Equipment Quan


No. Specification
/Components/Trainer kit tity
1. Digital pH meter Type: Microcontroller Based, Display: 1
LED / LCD / Touch Screen, 3 digits,
Calibration: up to 3 points with auto
buffer, pH Range (pH): 0.00 to 14.00,
+/- 0.05, Power Requirements: 230 V
+/- 10, 50 Hz AC, Modes: pH mV- C,
Temperature Compensation Type:
Automatic Temperature Compensation
Range (Degree C): 0 to 100,
Temperature Accuracy (Degree C): +/-
0.3, Resolution (pH): 0.01
2. Pipette (10 mL) Borosilicate glass 1

3. Measuring flask (100 mL) Borosilicate glass 1

Page | 39
BASIC CHEMISTRY (4300011)  Laboratory Manual

4 Beaker (25 mL) Borosilicate glass 6

5 Test tube stand Wooden or Plastic material 1

6 Test tubes Borosilicate glass 6


100mm *13mm *11mm
7 White glazed tile Ceramic material 1

8 Wash bottle (500 mL) Plastic material 1

9 Chemicals: Analytical grade reagents As


• dilute aqueous acid solutions per
• dilute aqueous alkali solutions need
• mineral water, distilled water,
tap water, deionized water
• buffer solutions of pH 7 and
pH 2
• Universal indicator

J. Safety and necessary Precautions followed:

1. Glassware should be cleaned and dried.


2. Keep the electrode in distilled water when not in use or cover with a sleeve
to save it from jerks.
3. The electrode should not touch the sides or the bottom of the beaker.
4. Allow the display to stabilize before taking your reading.

K. Procedure to be followed:
Part - I: pH measurement by Universal indicator.
1. Procure samples in separate beakers of 100 mL capacity each.
2. Transfer nearly 2 mL of the sample (20 drops) with the help of a separate
dropper for each sample in six different test tubes marked 1, 2, 3, 4, 5and
6 respectively.
3. Add two drops of the universal indicator in each test tube and mix the
content of each test tube thoroughly by shaking.
4. Match the colour appearing in each test tube with the standard pH chart.
5. Record your observations as in Observation Table
Part - II: pH measurement by pH meter.
1. Calibrate pH meter with pH 7 and pH 2 Buffers.
2. Select the pH Mode and set the temperature control knob to 25°C. Adjust
the cal 2 knob to read 100%.
3. Rinse the electrode with deionized water and blot dry using a piece of
tissue.

40 | Page
BASIC CHEMISTRY (4300011)  Laboratory Manual

4. Place the electrode in the solution of pH 7 buffer, allow the display to


stabilize and, then, set the display to read 7 by adjusting cal 1. Remove the
electrode from the buffer.
5. Rinse the electrode with deionized water and blot dry using a piece of
tissue.
6. Place the electrode in the solution of pH 2 buffer, allow the display to
stabilize and, then, set the display to read 2 by adjusting cal 2. Remove the
electrode from the buffer.
7. Rinse the electrode with deionized water and blot dry using a piece of
tissue.
8. Measure the pH value.
9. Make sure that the meter is set to the pH Mode and adjust the
temperature to 25°C.
10. Place the electrode in the sample to be tested.
11. The pH of the solution appears in the display.
NOTE: Allow the display to stabilize before taking your reading!
12. Record your readings as in Observation Table.
13. Rinse the electrode with deionized water and place it back in the storage
solution.
14. Compare the result obtained by using universal indicator and that
obtained by using pH meter.

L. Observation Tables:
Part - I: pH measurement by Universal indicator

Colour with Universal


Name of the sample pH Inference
indicator
Sr. No.

1 dilute HCl solution


2 dilute NaOH solution
3 Distilled water
4 Tap water
5 Soap solution
6 dilute NaHCO3 solution
7 Butter milk/Lemon solution

Page | 41
BASIC CHEMISTRY (4300011)  Laboratory Manual

Part - II: pH measurement by Digital pH meter

Sr.
Name of the sample pH Inference
No.

1. dilute HCl solution

2. dilute NaOH solution

3. Distilled water

4. Tap water

5. Soap solution

6. dilute NaHCO3 solution

7. Butter milk/Lemon solution

M. Results:
1. pH of acidic solution ranges from ...………… .
2. pH of neutral solution is ...………… .

3. pH of basic solution ranges from more than ...………… .

N. Interpretation of Results:
.....................................................................................................................................
.....................................................................................................................................
.........................................................................................................................

O. Conclusion:
.....................................................................................................................................
.....................................................................................................................................

42 | Page
BASIC CHEMISTRY (4300011)  Laboratory Manual

P. Practical related Quiz:


1. Define: pH.
Ans. ..............................................................................................................
.............................................................................................. ................
.............................................................................................. ................
2. List out five acidic materials.
Ans. ..............................................................................................................
..............................................................................................................
3. List out five basic materials.
Ans. ..............................................................................................................
..............................................................................................................
4. List out five neutral materials.
Ans. ..............................................................................................................
..............................................................................................................
5. For a given very dilute aqueous sample, pH + pOH = .............. .

Q. References / Suggestions:
1. Engineering Chemistry by Jain & Jain, Dhanpat Rai Publishing Co. (P) Ltd, New
Delhi, ISBN: 93-521-6000-2.
2. Engineering Chemistry by Shikha Agarwal, Cambridge Uni. Press, New Delhi,
2013, ISBN: 9788126543342.
3. A Textbook of Engineering Chemistry by Dr. S. S. Dara &Dr. S. S. Umare, S.
Chand & Co.(P) Ltd., New Delhi, 2014, ISBN:81-219-0359-9.
Students should search and write any one reference relevant to this experiment
.................................................................................................................................

R. Assessment-Rubrics:
As mentioned in (1) Rubrics (Pg. 10) and (2) Continuous Assessment (CA) (Pg. 11) is
to be done by the course faculty member.

 Remarks (if any) : .......................................................................................................

 Signature of the course Faculty Member with Date : ...............................................

Page | 43
BASIC CHEMISTRY (4300011)  Laboratory Manual

Date: ...... - ...... - 202…..

Practical No. 5
Determine the rate of corrosion of different metals in the given solution.
( Rate of corrosion of different metals in the solution)

A. Objective:
Corrosion is a well-known redox phenomenon. There is a weight loss due
to corrosion of metal. Different metal undergoes corrosion at different rate
in given solution. Measure the rate of corrosion of different metals in the
solution.

B. Expected Program Outcomes (POs):


1. Basic and Discipline specific knowledge
2. Problem analysis
3. Design/Development of solutions
4. Engineering Tools, Experimentation and Testing
5. Engineering practices for society, sustainability and environment
6. Project Management

C. Expected Skills to be developed based on competency:


This practical is expected to develop the following skills for the industry-
Use/Apply principles of Basic Chemistry to solve broadly-defined
engineering problems related to corrosion.

D. Expected Course Outcomes (COs):


Solve engineering problems using the concepts of electrochemistry and corrosion.

E. Practical Outcomes (PrOs):


1. Measure the rate of corrosion of different metals in the given solution.
2. Measurement Skill
3. Preparation of solution
4. Weighing skill

44 | Page
BASIC CHEMISTRY (4300011)  Laboratory Manual

F. Expected Affective Domain Outcomes (ADOs):


The ADOs are best developed through laboratory/field-based exercises.
1. Work as a leader/a team member
2. Follow ethical practices
3. Observe safety measures
4. Good housekeeping
5. Time management

G. Prerequisite Theory:

• Corrosion is a destruction of metals into metallic compounds/salts


(metal oxide, metal hydroxide, etc.) due to surroundings. When metal
comes in the contact with gases or liquid medium, it under goes decay.
• Corrosion may be Dry corrosion or Wet corrosion.
• There are many factors which affect the rate of corrosion of metals like
moisture, purity of metal, area of metal, surrounding medium,
temperature, etc.
• During wet corrosion the medium of the solution and pH of the solution
also affect the rate of corrosion.
• The rate of corrosion of different metals in the given solution is
different.

H. Experimental set up:

Page | 45
BASIC CHEMISTRY (4300011)  Laboratory Manual

I. Resources/Equipment Required:

Sr. Instrument/Equipment
Specification Quantity
No. /Components/Trainer kit

Sensitivity (mg): 1 mg, 1


1. Electronic weighing balance Maximum capacity of
weighing (grams): 200 g.
• Glass rod As per
• Beakers (250 mL), requirement
• Dryer
• Pair of tongs (Steel)
2. Glassware
• Glass funnel
• Measuring cylinder
(10 mL)
• Policeman
• conc. HCl As per
• Sodium Hydroxide requirement
3. Reagents
• Sodium chloride
• Distilled water
Policeman is a flexible rubber scraper attached to a glass rod, used in chemistry
laboratories for amalgamating, transferring solid residues in gravimetric analysis
and also to prevent scratching glass when removing crystals from a glass
container.

J. Safety and necessary Precautions followed:


1. All the glassware should be rinsed properly with the help of distilled water
before they are used.
2. Handle all the glassware and chemicals/solutions very safely and carefully.
3. Add acid to water very slowly with constant stirring.
4. Do not inhale the gas produced during corrosion.
5. Keep flame/fire away from beaker.

K. Procedure to be followed:
1. Clean all the metal pieces of Fe, Zn and Al.
2. Polish each metal piece properly using policeman and remove the loose
particles from it.
3. Measure the surface area of each metal piece and note it down.

46 | Page
BASIC CHEMISTRY (4300011)  Laboratory Manual

4. Also note down the weight of each metal piece before corrosion.
5. Take 0.5M 100ml solution of any one - Hydrochloric acid (Acidic medium),
Sodium Hydroxide (Basic medium), Sodium chloride or Water (Neutral
medium) in three different beakers.
6. Now immerse each piece of different metals in three beakers having same
solution.
7. After one hour remove the metal plate from the solution.
8. Clean each piece by using water & policeman, remove all the loose particles
and then dry it with the help of drier.
9. Take weight of each piece after drying them and note down their weights
after corrosion.
10. Calculate the rate of corrosion of different metals in the same solution.

L. Observations, Observation Table and Calculations:


⮞ Observations:
1. Total surface area of the Iron (Fe) piece = ................... dm2
2. Total surface area of the Zinc (Zn) piece = ................... dm2
3. Total surface area of the Aluminium (Al) piece = ....................dm2
4. Any one of the following media for corrosion:
Acidic medium: 0.5M Hydrochloric acid solution or
Basic medium: 0.5M Sodium hydroxide solution or
Neutral medium: 0.5M Sodium chloride solution/Water
⮞ Observation Table:

Rate of
Weight loss corrosion
Total surface
Weight of metal Weight of metal of metal due of the
Sr. area of the
before corrosion, after corrosion, to corrosion, metal
No. Metal metal piece,
W1 (mg) W2 (mg) (W2  W1) (mdd)
A (dm2)
(mg) (calculate
& write)
1. Iron (Fe)

2. Zinc (Zn)

3. Aluminium (Al)

Page | 47
BASIC CHEMISTRY (4300011)  Laboratory Manual

🠚 Rate of corrosion of metals (are described by their weight loss) has been most
commonly given unit as mdd = (mg/dm2) per day (milligrams per square
decimetre per day) of metal lost by corrosion.

⮞ Calculations:

Rate of corrosion of a metal in the solution (mdd)

= Weight loss (mg)  Total surface Area of metal piece (dm2)  24 (hours)

= (W2  W1) (mg)  A (dm2)  24 (hours)

In 0.5M .......................................................... solution,


🢡 For Iron (Fe):
Rate of corrosion of Iron (Fe)

= Weight loss (mg)  Total surface Area of metal piece (dm2)  24 (hours)

= (W2  W1) (mg)  A (dm2)  24 (hours)


= ..................  ..................  24
= .................... mdd

🢡 For Zinc (Zn):


Rate of corrosion of Zinc (Zn)

= Weight loss (mg)  Total surface Area of metal piece (dm2)  24 (hours)

= (W2  W1) (mg)  A (dm2)  24 (hours)


= ..................  ..................  24
= .................... mdd

48 | Page
BASIC CHEMISTRY (4300011)  Laboratory Manual

🢡 For Aluminium (Al):


Rate of corrosion of Aluminium (Al)

= Weight loss (mg)  Total surface Area of metal piece (dm2)  24 (hours)

= (W2  W1) (mg)  A (dm2)  24 (hours)


= ..................  ..................  24
= .................... mdd

M. Results :
In 0.5M ........................................................... solution,
1. The rate of corrosion of the Iron (Fe ) piece/plate = ................... mdd.
2. The rate of corrosion of the Zinc (Zn) piece/plate = ................... mdd.
3. The rate of corrosion of the Aluminium (Al) piece/plate =.................... mdd.

N. Interpretation of Results:
🠚 The rate of corrosion of the .................. metal is the highest and of the
.................. metal is the lowest in the given
................................................................ solution.

🠚 Order of metals is .................. > .................. >.................... for the decreasing rate
of corrosion in the given ................................................................. solution.

O. Conclusion:
…..................................................................................................................................
.............….....................................................................................................................

P. Practical related Quiz:


1. Define: Corrosion.
Ans. ..........................................................................................................................
...........................................................................................................................
...........................................................................................................................

Page | 49
BASIC CHEMISTRY (4300011)  Laboratory Manual

2. What is described by the weight loss of the metal?


Ans. ..........................................................................................................................
..........................................................................................................................
3. Write any five factors which affect the rate of corrosion.
Ans. ..........................................................................................................................
...........................................................................................................................
...........................................................................................................................
4. What is the unit of rate of corrosion.
Ans. ..........................................................................................................................
5. Write the full form of mdd.
Ans. ..........................................................................................................................

Q. References / Suggestions:
1. Engineering Chemistry by Jain & Jain, Dhanpat Rai Publishing Co. (P) Ltd, New
Delhi, ISBN: 93-521-6000-2.
2. Engineering Chemistry by Shikha Agarwal, Cambridge Uni. Press, New Delhi,
2013, ISBN: 9788126543342.
3. A Textbook of Engineering Chemistry by Dr. S. S. Dara &Dr. S. S. Umare, S.
Chand & Co.(P) Ltd., New Delhi, 2014, ISBN:81-219-0359-9.
Students should search and write any one reference relevant to this experiment
.....................................................................................................................................

R. Assessment-Rubrics:
As mentioned in (1) Rubrics (Pg. 10) and (2) Continuous Assessment (CA) (Pg. 12) is
to be done by the course faculty member.

 Remarks (if any) : .......................................................................................................

 Signature of the course Faculty Member with Date : ...............................................

50 | Page
BASIC CHEMISTRY (4300011)  Laboratory Manual

Date: ...... - ...... - 202…..

Practical No. 6
Determine the rates of corrosion of the metal in the solutions of different pH.
( Rates of corrosion of metal in solutions of different pH )

A. Objective:
Corrosion is a well-known redox phenomenon. There is weight loss due to
corrosion of metal. Different metal undergoes corrosion at different rate in
a given solution. Measure the rate of corrosion of the metal in the
solutions of different pH.

B. Expected Program Outcomes (POs):


1. Basic and Discipline specific knowledge
2. Problem analysis
3. Design/Development of solutions
4. Engineering Tools, Experimentation and Testing
5. Engineering practices for society, sustainability and environment
6. Project Management

C. Expected Skills to be developed based on competency:


This practical is expected to develop the following skills for the industry-
Use/Apply principles of Basic Chemistry to solve broadly-defined
engineering problems related to corrosion.

D. Expected Course Outcomes (COs):


Solve engineering problems using the concepts of electrochemistry and corrosion.

E. Practical Outcomes (PrOs):


1. Measure the rate of corrosion of metal in the solutions of different pH.
2. Measurement Skill
3. Preparation of solution
4. Weighing skill

Page | 51
BASIC CHEMISTRY (4300011)  Laboratory Manual

F. Expected Affective Domain Outcomes (ADOs):


The ADOs are best developed through laboratory/field-based exercises.
1. Work as a leader/a team member
2. Follow ethical practices
3. Observe safety measures
4. Good housekeeping
5. Time management

G. Prerequisite Theory:
• Corrosion is a destruction of metals into metallic compounds/salts
(metal oxide, metal hydroxide, etc.) due to surroundings. When metal
comes in the contact with gases or liquid medium, it under goes decay.
• Corrosion may be Dry corrosion or Wet corrosion.

• There are many factors which affect the rate of corrosion of metals like
moisture, purity of metal, area of metal, surrounding medium,
temperature, etc.
• During wet corrosion the medium of the solution and pH of the solution
also affect the rate of corrosion.

• The rates of corrosion of the metal in solutions of different pH are


different.

H. Experimental set up:

solutions

52 | Page
BASIC CHEMISTRY (4300011)  Laboratory Manual

I. Resources/Equipment Required:

Sr. Instrument/Equipment
Specification Quantity
No. /Components/Trainer kit

Sensitivity (mg): 1 mg, 1


1. Electronic weighing balance Maximum capacity of
weighing (grams): 200 g.
• Glass rod As per
• Beakers (250 mL), requirement
• Dryer
• Pair of tongs (Steel)
2. Glassware
• Glass funnel
• Measuring cylinder
(10 mL)
• Policeman
• conc. HCl As per
• Sodium Hydroxide requirement
3. Reagents • Sodium chloride
• Distilled water
• pH strips
Policeman is a flexible rubber scraper attached to a glass rod, used in chemistry
laboratories for amalgamating, transferring solid residues in gravimetric analysis
and also to prevent scratching glass when removing crystals from a glass
container.

J. Safety and necessary Precautions followed:


1. All the glassware should be rinsed properly with the help of distilled water
before they are used.
2. Handle all the glassware and chemicals/solutions very safely and carefully.
3. Add acid to water very slowly with constant stirring.
4. Do not inhale the gas produced during corrosion.
5. Keep flame/fire away from beaker.

Page | 53
BASIC CHEMISTRY (4300011)  Laboratory Manual

K. Procedure to be followed:
1. Clean the three pieces of same metal (any one Fe, Zn or Al).
2. Polish each metal piece properly using policeman and remove the loose
particles from it.
3. Measure the surface area of each metal piece and note it down.
4. Also note down the weight of each metal piece before corrosion.

5. Take 100ml for each - 0.5M Hydrochloric acid solution (Acidic medium), 0.5M
Sodium Hydroxide solution (Basic medium) and 0.5M Sodium chloride
solution or Water (Neutral medium) in three different beakers.
6. Measure the approximate pH of each solution using pH strip and note it
down.
7. Now immerse each piece of same metal in the beakers having different
solutions.
8. After one hour remove the metal plate from the solution.
9. Clean each piece by using water & policeman, remove all the loose particles
and then dry it with help of drier.
10. Take weight of each piece after drying them and note down their weights
after corrosion.
11. Calculate the rates of corrosion of the metal in the solutions of different
pH.

L. Observations, Observation Table and Calculations:


⮞ Observations:

1. Total surface area of the 2nd piece of .................. metal, A2 = ................... dm2
2. Total surface area of the 1st piece of .................. metal, A1 = ................... dm2
3. Total surface area of the 3rd piece of .................. metal, A3 =.................... dm2
4. All three following solutions having different pH (of different media) for
corrosion:
Acidic medium : 0.5M Hydrochloric acid solution,
Basic medium : 0.5M Sodium hydroxide solution and
Neutral medium : 0.5M Sodium chloride solution/Water

54 | Page
BASIC CHEMISTRY (4300011)  Laboratory Manual

⮞ Observation Table:

Rate of
Total surface Weight of Weight of Weight loss corrosion of
Sr. area of the metal piece metal piece of metal due the metal
pH to corrosion,
No. same metal before after
Solution of solution piece, corrosion, corrosion, (mdd)
(W2  W1)
A (dm2) W1 (mg) W2 (mg) (calculate &
(mg)
write)
1. 0.5M HCl A1 =

2. 0.5M NaOH A2 =

3. 0.5M NaCl/H2O A3 =

🠚 Rate of corrosion of metals (are described by their weight loss) has been most
commonly given unit as mdd = (mg/dm2) per day (milligrams per square
decimetre per day) of metal lost by corrosion.

⮞ Calculations:
Rate of corrosion of a metal in the solution (mdd)

= Weight loss (mg)  Total surface Area of metal piece (dm2)  24 (hours)

= (W2  W1) (mg)  A (dm2)  24 (hours)

For ......................... (...... ) metal,


🢡 In 0.5M HCl solution:
Rate of corrosion of the 1st piece of ......................... (. ...... ) metal in 0.5 M HCl
solution

= Weight loss (mg)  Total surface Area of metal piece (dm2)  24 (hours)

= (W2  W1) (mg)  A (dm2)  24 (hours)


= ..................  ..................  24
= .................... mdd

Page | 55
BASIC CHEMISTRY (4300011)  Laboratory Manual

🢡 In 0.5 NaOH solution:


Rate of corrosion of the 2nd piece of ......................... (. ......) metal in 0.5M NaOH
solution

= Weight loss (mg)  Total surface Area of metal piece (dm2)  24 (hours)

= (W2  W1) (mg)  A (dm2)  24 (hours)


= ..................  ..................  24
= .................... mdd

🢡 In 0.5M NaCl solution/H2O:


Rate of corrosion of the 3rd piece of ......................... (. ..... ) metal in 0.5M NaCl
solution/H2O

= Weight loss (mg)  Total surface Area of metal piece (dm2)  24 (hours)

= (W2  W1) (mg)  A (dm2)  24 (hours)


= ..................  ..................  24
= .................... mdd

M. Results :
1. The rate of corrosion of the ......................... (. ..... ) metal in 0.5 M HCl solution
(having pH = ............) = ................... mdd.
2. The rate of corrosion of the ......................... (.......) metal in 0.5 M NaOH
solution (having pH = ............) = ................... mdd.
3. The rate of corrosion of the ......................... (.......) metal in 0.5 M NaCl
solution/H2O (having pH = ............) = ................... mdd.

N. Interpretation of Results:

🠚 The rate of corrosion of the ......................... (.......) metal is the highest in


.................................. solution at ............ pH and is the lowest in
.................................. solution at ............. pH.
🠚 Order of pH is .................. > .................. > ................... of solutions for the
decreasing rates of corrosion of the ......................... (.......) metal in different
solutions.

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BASIC CHEMISTRY (4300011)  Laboratory Manual

O. Conclusion:
…..................................................................................................................................
.............….....................................................................................................................

P. Practical related Quiz. (Same as practical -8)

1. What does the weight loss of the metal give idea about?
Ans. ..........................................................................................................................
..........................................................................................................................

2. Write the names of two main types of corrosion.


Ans. ..........................................................................................................................
...........................................................................................................................
...........................................................................................................................
3. Write the names of any five methods to prevent corrosion of metals.
Ans. ..........................................................................................................................
...........................................................................................................................
...........................................................................................................................
4. Write the use of policeman in chemistry laboratory.
Ans. ..........................................................................................................................
5. Why 24 is given in multiplied form in the formula of rate of corrosion?
Ans. ..........................................................................................................................

Q. References / Suggestions:
1. Engineering Chemistry by Jain & Jain, Dhanpat Rai Publishing Co. (P) Ltd, New
Delhi, ISBN: 93-521-6000-2.
2. Engineering Chemistry by Shikha Agarwal, Cambridge Uni. Press, New Delhi,
2013, ISBN: 9788126543342.
3. A Textbook of Engineering Chemistry by Dr. S. S. Dara &Dr. S. S. Umare, S.
Chand & Co.(P) Ltd., New Delhi, 2014, ISBN:81-219-0359-9.
Students should search and write any one reference relevant to this experiment
.................................................................................................................................

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BASIC CHEMISTRY (4300011)  Laboratory Manual

R. Assessment-Rubrics:
As mentioned in (1) Rubrics (Pg. 10) and (2) Continuous Assessment (CA) (Pg. 12) is
to be done by the course faculty member.

 Remarks (if any) : .......................................................................................................

 Signature of the course Faculty Member with Date : ...............................................

58 | Page
BASIC CHEMISTRY (4300011)  Laboratory Manual

Date: ...... - ...... - 202…..

Practical No. 7
Estimate total hardness of given water sample using standard EDTA
solution.
( Total Hardness of water by EDTA )

A. Objective:
Hardness in water is due to the presence of dissolved salts of calcium and
magnesium. It is unfit for drinking, bathing, washing and it also forms
scales in boilers. Hence it is necessary to estimate the amount of hardness
producing substances present in the water sample. Once it is estimated,
the amount of chemicals required for the treatment of water can be
calculated. The estimation of hardness is based on complexometric
titration. Hardness of water is determined by titrating with a standard
solution of Ethylene Diamine Tetra Acetic acid (EDTA) which is a
complexing agent. Since EDTA is insoluble in water, the disodium salt of
EDTA is taken for this experiment. EDTA can form four or six coordination
bonds with a metal ion.

B. Expected Program Outcomes (POs):


1. Discipline knowledge.
2. Design/Development of solutions.
3. Experiments and Testing.
4. Engineering practices for environment.

C. Expected Skills to be developed based on competency:

Use/Apply principles of Basic Chemistry to solve broadly-defined


engineering problems.

D. Expected Course Outcomes (COs):


Use relevant water treatment methods to solve domestic and industrial
problems.

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BASIC CHEMISTRY (4300011)  Laboratory Manual

E. Practical Outcome (PrOs):

1. Differentiate hard water and soft water.


2. Estimate total hardness of given water sample using standard EDTA
solution.

F. Expected Affective domain Outcome (ADOs):


1. Work as a leader/a team member.
2. Follow ethical practices.
3. Observe safety measures.
4. Time management.
5. Good housekeeping
G. Prerequisite Theory:
Water can be classified as hard water and soft water:
 Soft water: It lathers with soap. Water which is obtained from the rain is
soft water. This water is suitable for household purposes. e.g., laundry
and cleaning.
 Hard water: It is known as hard water because of the presence of salts of
calcium and magnesium. Hard water does not lather with soap but
instead forms a precipitate. The presence of magnesium and calcium
bicarbonates in water makes it temporarily hard. In this case, the
temporary hardness in water can be removed by boiling the water.
e.g., If we boil water, then the soluble salts like Mg(HCO3)2 is converted
into Mg(OH)2 which is insoluble and hence gets precipitated and is
removed by filtration. After filtration, the water we get is soft water.
Similary, soluble salt Ca(HCO3)2 is also removed along with it.
 When the insoluble salts of magnesium and calcium are present in the
form of chlorides and sulphates in water, we call it permanent hardness
because this hardness cannot be removed by simple boiling process;
some special methods are used to remove permanent hardness.
 EDTA (Ethylene Diamine Tetra Acetic acid) forms colourless 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. Eriochrome Black - T (E.B.T.) is used as an indicator. The
sample of hard water must be treated with buffer solution and EBT
indicator which forms unstable, wine-red coloured complexes with Ca2+
and Mg2+ present in water.

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BASIC CHEMISTRY (4300011)  Laboratory Manual

H. Experimental set up:

I. Resources/Equipment Required:

Sr. Instrument/Equipment
Specification Quantity
No. /Components/Trainer kit
• Burette (50 mL)
• Pipette (10 mL)
• Conical flask (100 mL)
• Burette stand
1. Glassware (Borosil) • White glazed tile 1 for each
• Funnel
• Wash bottle
• Measuring flask (100 mL)
• Beakers (100mL)
1. Ammonia buffer solution As per
2. Eriochrome Black - T (indicator) requirements
3. disodium salt of EDTA
2. Reagents (AR) 4. magnesium chloride hexahydrate
5. CaCO3
6. conc. HCl
7. NaOH

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BASIC CHEMISTRY (4300011)  Laboratory Manual

J. Safety and necessary Precautions followed:

1. Properly wash all the glassware with the help of distilled water.
2. All the glassware should be rinsed properly before they are used.
3. Handle all the glassware and chemicals/solutions very safely and carefully.
4. Remove the air bubble if present in the nozzle of the burette before taking the
burette reading.
5. Use white glazed tile to accurately observe the colour change at the
endpoint reading during the experiment.
6. The conical flask should be continuously shaking well during the
addition of the solution from the burette.

K. Procedure to be followed:
Part – I : To standardize the solution of EDTA – disodium salt of ethylene
diamine tetraacetate:
⮞ Preparation of Standard calcium chloride i.e., CaCl2 solution:

1. Accurately weigh out 0.5 gm of dried, pure CaCO3 into a 250 mL beaker.
2. Add approximately 25 mL of distilled H2O, then add 1 mL of conc. HCl carefully,
cover with watch glass spaced with glass hooks until dissolved.

3. Note: If CaCO3 does not dissolve completely, add another 0.5 mL of conc. HCl.
Next, evaporate volume to about 2 mL maintaining watch glass on beaker to
expel carbon dioxide.
4. Rinse watch glass, transfer quantitatively into a 500 mL volumetric flask and
make up volumetrically to 500 mL.
⮞ Preparation of EDTA solution:
1. Weigh out approximately 2 gm of reagent grade disodium EDTA into a 250 mL
beaker.
2. Add 0.05 g magnesium chloride hexahydrate, three pellets of NaOH and add
about 200 mL of distilled water to dissolve.
3. The EDTA will dissolve slowly over a period of a half an hour. Magnesium
chloride is added to enhance the sharpness of the end point (It forms a more
stable complex with the indicator).
4. Filter the EDTA solution into a 0.5 or 1 L bottle, and then add approximately
250 mL of distilled water.

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BASIC CHEMISTRY (4300011)  Laboratory Manual

⮞ Standardization of EDTA:
1. Pipette out 20 mL of CaCl2 solution into a conical flask.
2. Add 5mL of buffer solution (pH 10) and few drops of Eriochrome Black-T.
3. The indicator, which is originally blue color, would acquire a wine-red color.

4. Titrate with EDTA solution taken in the burette, till the wine-red color changes
to blue which is the end point. Repeat the titration till three concordant
readings are obtained. Record the readings as shown in Observation Table and
calculate the molarity of EDTA solution (standard EDTA solution should be
~0.01 M).
Part – II : To determine the total hardness of water:
1. Repeat the part - I titration method for sample hard water instead of standard
CaCl2 solution.
2. Repeat the titration till three concordant readings are obtained.
3. Record the readings as shown in Observation Table and calculate the total
hardness of given water sample in ppm.

L. Observations, Observation Table, Chemical Equations and Calculations:


Part – I : To standardize the solution of EDTA:

⮞ Observations:
• Burette: xM EDTA solution

• Pipette: 20mL CaCl2 solution + 5mL buffer solution (NH4OH + NH4Cl, pH = 10)
• Indicator: 2-3 drops of Eriochrome Black-T (EBT)
• Colour change: Wine red to Blue

⮞ Observation Table:
Mean (Average)
Burette Pilot reading I II III
reading,
Reading (mL) (mL) (mL) (mL)
(mL) = (I + II + III)/3
mL
Final reading mL mL mL
(Whole No.)
Initial reading 0.0 mL mL mL mL V1 = .......... mL
Difference mL
mL mL mL
= F.r.–I.r. (Whole No.)

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BASIC CHEMISTRY (4300011)  Laboratory Manual

⮞ Chemical Equations :
CaCO3(s) + 2HCl(aq) 🠚 Ca2+(aq) + 2Cl1-(aq) + H2O(l) + CO2(g)

Ca2+/Mg2+ + Eriochrome Black-T 🠚 Ca2+/Mg2+ -Eriochrome Black-T- complex


(Colourless) (Blue) (Wine red-unstable Complex)

Ca2+/Mg2+ -Eriochrome Black-T- complex + EDTA 🠚 Ca/Mg-EDTA complex + Eriochrome Black-T


(Wine red-unstable complex) (Colourless) (Colourless-stable complex) (Blue)

Part – II : To determine the total hardness of water:


⮞ Observations:
• Burette: Standardized EDTA solution
• Pipette: 20mL hard water sample + 5mL buffer solution (NH4OH + NH4Cl,
pH = 10)
• Indicator: Eriochrome Black-T (EBT)
• Colour change: Wine red to Blue

⮞ Observation Table:
Mean (Average)
Burette Pilot reading I II III
reading,
Reading (mL) (mL) (mL) (mL)
(mL) = (I + II + III)/3
mL
Final reading mL mL mL
(Whole No.)
Initial reading 0.0 mL mL mL mL V1 = .......... mL
Difference mL
mL mL mL
= F.r.–I.r. (Whole No.)
⮞ Chemical Equations :
Ca2+/Mg2+ + Eriochrome Black-T 🠚 Ca2+/Mg2+ -Eriochrome Black-T- complex
(Colourless) (Blue) (Wine red-unstable Complex)

Ca2+/Mg2+ -Eriochrome Black-T- complex + EDTA 🠚 Ca/Mg-EDTA complex + Eriochrome Black-T


(Wine red-unstable complex) (Colourless) (Colourless-stable complex) (Blue)

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BASIC CHEMISTRY (4300011)  Laboratory Manual

⮞ Calculations:
For Part – I : To standardize the solution of EDTA:
(1) Molarity of EDTA solution:
M 1V 1 = M 2V 2 ;where, M1= Molarity of EDTA solution = x M
V1 = Volume of EDTA solution = ............ mL (from Part-I)
M2 = Molarity of Ca2+solution
= 0.5/(100.09  0.500) = 0.009991M
V2 = Volume of Ca2+solution = 20 mL
 M1 = M2V2
V1
 M1 = 0.009991  20
...........

 M1 = ...........

For Part – II : To determine the total hardness of water:


(2) Total hardness of water in molarity (M) unit:
M 1V 1 = M 2V 2 ;where, M1= Molarity of EDTA solution = ............ M
V1 = Volume of EDTA solution = ............ mL (from Part-II)
M2 = Molarity of hard water = y M
V2 = Volume of hard water = 20 mL
 M2 = M1V1
V2
 M2 = ............  ...........
20

 M2 = ...........

(3) Total hardness of water in ppm unit:


Total hardness of water in ppm in terms of CaCO3
= Molarity of hard water (M2)  105 ppm in terms of CaCO3
= ...........  105
= ............. ppm

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BASIC CHEMISTRY (4300011)  Laboratory Manual

M. Results:
Total hardness of given water sample = ............ ppm in terms of CaCO3.

N. Interpretation of Results:
.....................................................................................................................................
.....................................................................................................................................
.....................................................................................................................................
.....................................................................................................................................

O. Conclusion:
.....................................................................................................................................
.....................................................................................................................................

P. Practical related Quiz:


1. Hardness of water is conventionally expressed in terms of equivalent amount
of .................... .
a. H2CO3
b. MgCO3
c. Na2CO3
d. CaCO3
2. What is hard water?
..............................................................................................................................
..............................................................................................................................
3. Write the types of hardness of hard water.
..............................................................................................................................
..............................................................................................................................
4. Write the names of four salts responsible for permanent hardness of water.
..............................................................................................................................
..............................................................................................................................
5. Write the full name of EDTA.
..............................................................................................................................
6. ppm stands for ..............................................……………. .
a. Parts per millions
b. Parts per mole
c. Percentage per millions
d. Percentage per mole

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BASIC CHEMISTRY (4300011)  Laboratory Manual

Q. References / Suggestions:
1. AWWA, WEF, APHA, 1998, Standard Methods for the Examination of
Water and Wastewater (Methods: 2340 C. EDTA Titrimetric Method
Sawyer, C.N., McCarty, P.L., and Parkin, G.F. 2000. Chemistry for
Environmental Engineering 4 th Edition. Tata McGraw-Hill Publishing
Company Limited.
2. IS 10500:2012- Drinking Water- Specification, Second Revision.
3. Engineering Chemistry by Shikha Agarwal, Cambridge Uni. Press, New Delhi,
2013, ISBN: 9788126543342.
4. Virtual lab link:
https://ee1-nitk.vlabs.ac.in/exp/determination-of-hardness/index.html
Students should search and write any one reference relevant to this experiment
................................................................................................................................

R. Assessment-Rubrics:
As mentioned in (1) Rubrics (Pg. 10) and (2) Continuous Assessment (CA) (Pg. 12) is
to be done by the course faculty member.

 Remarks (if any) : ...................................................................................................

 Signature of the course Faculty Member with Date : ..........................................

Page | 67
BASIC CHEMISTRY (4300011)  Laboratory Manual

Date: ...... - ...... - 202…..

Practical No. 8
Estimate alkalinity of given water sample using 0.02N sulphuric acid
solution.
( Alkalinity of water sample )

A. Objective:
Alkalinity is important for a variety of natural water and wastewater
treatments and uses. Alkalinity is thought to be a sign of these elements as
well because many surface waters contain carbonates, bicarbonates, and
hydroxides. An important factor in assessing whether water is suitable for
irrigation is alkalinity that is greater than alkaline earth metal
concentrations. Measurements of alkalinity are used to evaluate and
manage water and wastewater treatment procedures.

B. Expected Program Outcomes (POs)


1. Basic Discipline knowledge
2. Problem analysis
3. Design/Development of solutions
4. Experiments and Testing

C. Expected Skills to be developed based on competency:


This practical is expected to develop the following skills for the industry-
identified competency:
‘Use/Apply basic principles of Basic Chemisty in various engineering
applications.’

D. Expected Course Outcomes (COs)


Use relevant water treatment methods to solve domestic and industrial
problems.

68 | Page
BASIC CHEMISTRY (4300011)  Laboratory Manual

E. Practical Outcome (PrOs):


1. Differentiate hard water and soft water.
2. Determination of alkalinity level in a water sample.
3. Calculation of acid requirement for a water sample.

F. Expected Affective Domain Outcomes (ADOs):

1. Work as a leader/a team member.


2. Follow ethical practices.
3. Observe safety measures.
4. Time management.
5. Good housekeeping

G. Prerequisite Theory:
 Alkalinity: The alkalinity of the water is a measure of its capacity to neutralize
acids. The alkalinity of natural waters is due primarily to the salts of week acids,
although weak or strong bases may also contribute.

 Alkalinity is usually imparted by bicarbonate, carbonate and hydroxide. 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 phase, the titration is conducted until the pH is lowered to
8.2, the point at which phenolphthalein indicator turns from pink to colourless,
corresponds to Phenolphthalein End point (PE). 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,


corresponds to Methyl orange End point (ME), which corresponds to the
equivalence points for the conversion of bicarbonate ion to carbonic acid.

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BASIC CHEMISTRY (4300011)  Laboratory Manual

H. Experimental set up:

I. Resources/Equipment Required:
Sr. Instrument/Equipment
Specification Quantity
No. /Components/Trainer kit
• Burette (50 mL)
• Pipette (25 mL)
• Conical flask (250 mL)
• Burette stand
1. Glassware (Borosil) 1
• Funnel
• White glazed tile
• Measuring flask (500 mL)
• Wash bottle
• 0.02N H2SO4(aq)
As per
• Water sample
2 Reagents (AR) requirements
• Phenolphthalein indicator
• Methyl orange indicator

J. Safety and necessary Precautions followed:


1. Properly wash all the glassware with the help of distilled water.
2. All the glassware should be rinsed properly before they are used.
3. Handle all the glassware and chemicals/solutions very safely and carefully.
4. Remove the air bubble if present in the nozzle of the burette before taking the

70 | Page
BASIC CHEMISTRY (4300011)  Laboratory Manual

burette reading.
5. Use white glazed tile to accurately observe the colour change at the
endpoint reading during the experiment.
6. The conical flask should be continuously shaking well during the
addition of the solution from the burette.

K. Procedure to be followed:

 Sample collection and preparation: Collect a representative sample of the


water to be analysed in a clean container. Mix the sample thoroughly and filter
it if necessary to remove any suspended particles.

 Titration setup: Rinse a burette with the 0.02N sulphuric acid solution, and fill
it with the solution. Add 50 mL of the water sample to the flask. Add a few
drops of phenolphthalein indicator to the sample in the conical flask.

 Titration: Titrate the sample by slowly adding the 0.02N sulphuric acid solution
from the burette into the conical flask while swirling the flask. Continue adding
titrate the sample with the 0.02N sulphuric acid till a faint pink colour persists.

 Record titre value as a Phenolphthalein End point - PE and add 2-3 drops of
methyl orange indicator to the same solution and the titration is continued
until the colour turns to orange yellow. The titre value from the beginning of
the titration is recorded as the Methyl orange End point - ME.

 Repeat the titration until three concordant readings are obtained. Record your
readings in Observation Table and calculate the total alkalinity of the water
sample.

L. Observations, Observation Tables and Calculations:


⮞ Observations:
• Burette: 0.02N H2SO4 solution
• Pipette: 50mL water sample
• Indicators: (1) Phenolphthalein (2) Methyl orange
• Colour change: (1) Faint Pink to Colourless
(2) Light Yellow to pinkish Red or Orange red

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BASIC CHEMISTRY (4300011)  Laboratory Manual

⮞ Observation Table:
Mean (Average)
I II III
reading,
(mL) (mL) (mL)
Burette (mL) = (I + II + III)/3
Reading
PE ME PE ME PE ME PE ME

Final reading mL mL mL mL mL mL
Initial reading 0.0 mL 0.0 mL 0.0 mL 0.0 mL 0.0 mL 0.0 mL V2 = V2 =
......... mL ......... mL
Difference
mL mL mL mL mL mL
= F.r.–I.r.

⮞ Chemical equations:
OH– + H+ 🠚 H2O
CO32– + H+ 🠚 HCO3–
HCO3– + H+ 🠚 H2O + CO2

⮞ Calculations: For the given water sample,


(1) Hydroxide alkalinity i.e., Phenolphthalein alkalinity (P):
N × V2
P = 2 × Eq. weight of CaCO × 103 ppm
3
V1
;where,
N2×V2
N1 = normality of OH-1 ions = = .................. N
V1

V1 = volume of water sample = 50mL


N2 = normality of acid solution = 0.02N
V2 = volume of acid solution = ................. mL (Average PE)
Equivalent weight of CaCO3 = 50 g/equivalent

 P = 0.02  .............  50  103


50

 P = ...............ppm

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BASIC CHEMISTRY (4300011)  Laboratory Manual

(2) Total alkalinity i.e., Methyl orange alkalinity (M):


N2 × V2
M = × Eq. weight of CaCO 3 × 103 ppm
V1
;where,
N2×V2
N1 = normality of all alkaline ions = = .................. N
V1

V1 = volume of water sample = 50mL


N2 = normality of acid solution = 0.02N
V2 = volume of acid solution = ................. mL (Average ME)
Equivalent weight of CaCO3 = 50 g/equivalent

 M = 0.02  .............  50  103


50
 M = ............... ppm

M. Results:
(1) Hydroxide alkalinity of the given water sample, P =............... ppm.
(2) Total alkalinity of the given water sample, M = ..............ppm.

N. Interpretation of Results:

...................................................................................................................................
...................................................................................................................................
...................................................................................................................................
...................................................................................................................................

O. Conclusion:
.....................................................................................................................................
.....................................................................................................................................

P. Practical related Quiz:


1. What is ppm?
a. Parts per meter square
b. Parts per meter
c. Parts per million
d. Parts per millimetre
Ans. .......................................................................................................................

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BASIC CHEMISTRY (4300011)  Laboratory Manual

2. Alkalinity of water is an indication of


a. Base neutralizing capacity
b. Acid neutralizing capacity
c. Quantity of base present
d. Quality of base present
Ans. .......................................................................................................................
3. Define : Alkalinity of water.
Ans. .......................................................................................................................
...........................................................................................................................
................................................................................................................
4. What does PE and ME indicate?
Ans. .......................................................................................................................
...........................................................................................................................
...........................................................................................................................
............................................................................................................
5. Which two indicators are used for this experiment?
Ans. .......................................................................................................................
.......................................................................................................................

Q. References / Suggestions:
1. IS 3025-23 (Part 23) - 1986: Methods of Sampling and Test (physical
and chemical) for Water and Wastewater, Alkalinity, First Revision.
2. AWWA, WEF, APHA, 1998, Standard Methods for the Examination of
Water and Wastewater (Methods: 4500 B. Electrometric Method; 2320
B. Titration Method)
3. Virtual lab link: https://ee1-nitk.vlabs.ac.in/exp/determination-of-alkalinity/
Students should search and write any one reference relevant to this experiment
................................................................................................................................

R. Assessment-Rubrics:
As mentioned in (1) Rubrics (Pg. 10) and (2) Continuous Assessment (CA) (Pg. 12) is
to be done by the course faculty member.

 Remarks (if any) : ...................................................................................................

 Signature of the course Faculty Member with Date : ..........................................

74 | Page
BASIC CHEMISTRY (4300011)  Laboratory Manual

Date: ...... - ...... - 202…..

Practical No. 9
Determine Total Dissolved Solid (TDS) and Total Suspended Solid (TSS) in a given
sample of water.

( TDS & TSS of water sample )

A. Objective:
It is helpful to estimate the total dissolved solids to assess whether the
water is acceptable for drinking, industrial, or agricultural usage. The
examination of polluted waterways benefits greatly from the identification
of suspended solids. Light is blocked by suspended particles, which slows
the growth of plants that produce oxygen.

B. Expected Program Outcomes (POs):


1. Basic and Discipline specific knowledge
2. Development of solutions
3. Experimentation and Testing
4. Engineering practices for society, sustainability and environment

C. Expected Skills to be developed based on competency:


This practical is expected to develop the following skills for the industry-
identified competency:
‘Use/Apply basic principles of Basic Chemistry in various engineering
applications.’

D. Expected Course Outcomes (COs):


Use relevant water treatment methods to solve domestic and industrial
problems.

E. Practical Outcome (PrOs):


1. Water Quality Assessment.
2. TDS and TSS regulations and their determination.
3. Awareness about potable (drinking) water and health safety.

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BASIC CHEMISTRY (4300011)  Laboratory Manual

F. Expected Affective Domain Outcome (ADOs):


1. Work as a leader/’ a team member.
2. Follow ethical practices.
3. Observe safety measures.
4. Time management.
5. Good housekeeping

G. Prerequisite Theory:
• TSS and TDS measure the amount of particulate matter (tiny pieces of
things) floating in water.
• These particles, or ‘solids’, can be divided into two types by passing the
water through a filter. The particles that are large enough to be held
back by the filter are called total suspended solids (TSS), while the
particles that pass through the filter are called total dissolved
solids (TDS).
• Total suspended solids (TSS) values are often related to the turbidity
(cloudiness) of water. If TSS is high and the water is murky then light
from the sun will not travel well through the water, making it difficult
for plants and algae to grow.
• Total dissolved solids (TDS) include dissolved minerals and salts in the
water. As a result, TDS is often closely related to conductivity, salinity,
alkalinity, and hardness measures. Most freshwater fish and bugs
cannot tolerate high TDS because they are not adapted to saline (salty)
water, like marine fish are.

H. Experimental set up:

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BASIC CHEMISTRY (4300011)  Laboratory Manual

I. Resources/Equipment Required:
Sr. Instrument/Equipment
Specification Quantity
No. /Components/Trainer kit
Temperature is controlled by
digital temperature indicator
1. Hot air oven 1
cum controller from ambient to
250°C with ± 0.1°C Accuracy.
Sensitivity (mg): 1 mg,
2. Analytical Balance Maximum Capacity of 1
weighing (grams): 200 g.
Evaporating Dish As per
3. Glassware Graduated Cylinders require
Gooch Crucibles ment
As per
Dish Tongs and Crucible
4. Heat resistant metal tongs require
tongs
ment
As per
5. Filter papers Whatman require
ment
Glass flask equipped with a
side arm for vacuum pump
connection and a rubber
Vacuum Pumps with stopper to provide seal with
6. 1
glass filter funnel. The flask is used to
collect the filtered process
water that passes through the
filter.
As per
7. Forceps Metal or plastic based require
ment
sealable enclosures containing
8. Desiccator desiccants used for preserving 1
moisture

J. Safety and necessary Precautions followed


1. Properly wash all the glassware with the help of distilled water.
2. All the glassware should be rinsed properly before they are used.
3. Handle all the glassware and chemicals/solutions very safely and carefully.
4. If the sample cooled in a moist environment, the sample would increase in
weight because of the addition of water vapor from the air.
5. Do not touch container with bare hands.

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BASIC CHEMISTRY (4300011)  Laboratory Manual

K. Procedure to be followed:

🢡 TESTING OF SAMPLE FOR TOTAL DISSOLVED SOLIDS (TDS) :


1. Take a clean porcelain dish which has been washed and dried in a hot air
oven at 180oC for one hour.
2. Weigh the empty evaporating dish in analytical balance. Note the weight as
W1.
3. Mix sample well and pour into a funnel with filter paper. Filter
approximately 80 -100 mL of sample.
4. Using pipette transfer 75mL of unfiltered sample in the porcelain dish.
5. Switch on the oven and allowed to reach 105°C.
6. Place it in the hot air oven and care should be taken to prevent splattering
of sample during evaporation or boiling.
7. Dry the sample to get constant mass. Drying for long duration usually 1 to 2
hours is done to eliminate necessity of checking for constant mass.
8. Cool the container in a desiccator.
9. Weigh the dish as soon as it has cooled to avoid absorption of moisture.
Note the weight with residue as W2.

🢡 TESTING OF SAMPLE FOR TOTAL SUSPENDED SOLIDS (TDS) :

1. Place filtration apparatus with weighed filter paper in filter flask.


2. Mix sample well and pour into a graduated cylinder to the selected
volume.
3. Apply suction to filter paper flask and set filter paper with a small amount
of distilled water.
4. Pour selected volume into filtration apparatus.
5. Draw sample through filter paper into filter flask.
6. Rinse graduated cylinder into filtration apparatus with three successive 10
mL portions of distilled water, allowing complete drainage between each
rinsing.
7. Continue suction for three minutes after filtration of final rinse is
completed.
8. Dry filter paper in an oven at 103-105°C for at least 1 hour.
9. Cool filter paper in desiccator to room temperature.
10. When cool, weigh the filter paper.

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BASIC CHEMISTRY (4300011)  Laboratory Manual

L. Observation Table and Calculations:


Observation Table - 1: for Total Dissolved Solids (TDS)

Description Symbols Weight (gm)

Weight of the clean porcelain


W1 …………… gm
evaporating dish (gm)

Weight of the dish and the residue


W2 …………… gm
(gm) (after corrosion)

Weight of residue (gm) (weight of


W = W2  W1 …………… gm
water sample)

Volume of the water Sample (mL) V 50 mL

…………… mg/L
Total Dissolved Solids (mg/L) TDS
(calculate & write)

⮞ Calculations : ( for Total Dissolved Solids (TDS) )


Weight of residue, W (gm) = W2 – W1
= ………….. – ……………
= ..............gm

Weight of residue, W (mg) = ………….. × 1000


= .............. mg

Total Dissolved Solids (mg/L) = Weight of residue (mg) ÷ V mL


= W (mg) ÷ 50 (mL)

= ………….. mg ÷ [50  10-3 L]


= ………….. mg ÷ 0.05 L
= .............. mg/L

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BASIC CHEMISTRY (4300011)  Laboratory Manual

Observation Table 2: for Total Suspended Solids (TSS)

Description Symbols Weight(gm)

Weight of the clean filter paper (gm) W1 …………… gm

Weight of the filter paper and the


W2 …………… gm
residue (gm)

Wt. of residue (gm) W = W2  W1 …………… gm

Volume of the water Sample (mL) V 50 mL

…………… mg/L
Total Suspended Solids(mg/L) TSS
(calculate & write)

⮞ Calculations : ( for Total Suspended Solids (TSS) )


Weight of residue, W (gm) = W2 – W1
= ………….. – ……………
= ............. gm

Weight of residue, W (mg) = ………….. × 1000


= .............. mg

Total Suspended Solids (mg/L) = Weight of residue (mg) ÷ V mL


= W (mg) ÷ 50 (mL)

= ………….. mg ÷ [50  10-3 L]


= ………….. mg ÷ 0.05 L
= .............. mg/L

M. Results:
In a given water sample,
(1) Total Dissolved Solids (TDS) = ................... mg/L
(2) Total Suspended Solids (TSS) = ...................mg/L

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BASIC CHEMISTRY (4300011)  Laboratory Manual

N. Interpretation of Results:
.....................................................................................................................................
.....................................................................................................................................
.....................................................................................................................................
..........................................................................................................................

O. Conclusion:
.....................................................................................................................................
.....................................................................................................................................
...........................................................................................................................

P. Practical related Quiz:


1. High total dissolved solids indicate lower level of hardness.
a. True
b. False
Ans. …………………………………………………………………………………………………………….
2. Total Suspended Solids are mostly responsible for
a. Turbidity.
b. Colour
c. Odour
d. Taste
Ans. …………………………………………………………………………………………………………….
3. Write the full form of TDS.
Ans. …………………………………………………………………………………………………………….
4. What is the preferable TDS value for potable (drinking) water?
Ans. …………………………………………………………………………………………………………….
5. What is the full form of TSS?
Ans. …………………………………………………………………………………………………………….

Q. References / Suggestions
1. Link for virtual lab:
https://ee1-nitk.vlabs.ac.in/exp/determination-of-ts/procedure.html
2. Reference: www.researchgate.com
3. IS 3025 (Part 15)- 1984: Method of Sampling and Test (Physical and Chemical)
for Water and Wastewater: Total Residue (total Solids, Dissolved and
Suspended, First Revision.

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BASIC CHEMISTRY (4300011)  Laboratory Manual

4. A Textbook of Engineering Chemistry by Dr. S. S. Dara &Dr. S. S. Umare, S.


Chand & Co.(P) Ltd., New Delhi, 2014, ISBN:81-219-0359-9
5. Image source: (Source: https://www.researchgate.net/profile/Isam-Eldin-
Elgailani/post/How-can-I-determine-the-TSS-and-TDS-value-of-a-liquid-herbal-
extract/attachment/59d6590f79197b80779aeb74/AS%3A540930433794048%
401505979273757/download/How+to+measure+dissolved+suspended+total+s
olids.pdf)
Students should search and write any one reference relevant to this experiment
.................................................................................................................................

R. Assessment-Rubrics:
As mentioned in (1) Rubrics (Pg. 10) and (2) Continuous Assessment (CA) (Pg. 12) is
to be done by the course faculty member.

 Remarks (if any) : ...................................................................................................

 Signature of the course Faculty Member with Date : ...........................................

82 | Page
BASIC CHEMISTRY (4300011)  Laboratory Manual

Date: ...... - ...... - 202…..

Practical No. 10
Determine the viscosity of the lubricating oil using a Redwood viscometer.
( Viscosity using Redwood viscometer )

A. Objective:
Viscosity is the most significant property of any lubricating oil because it
determines the strength of the lubricant’s film in preventing friction between two
moving or sliding parts. If the viscosity of the oil is low for the operating
conditions, a liquid oil film cannot be maintained between two moving or sliding
parts; the machine must work harder and then generate more heat, so this will
create wear and tear on the machine. On the other hand, if the viscosity of the oil
is too high, the film may not be thick enough to prevent friction so this will create
wear and tear on the machine. Redwood viscometer - 1 or 2 is used in oil
manufacturing industries to determine the viscosity of lubricating oil. Lubricants
are used to reduce friction in various machineries that works at different
temperatures. The selection of lubricating oil for various machineries becomes
difficult because the viscosity of lubricating oils changes with temperature.
Determining the temperature effect on the viscosity of various lubricating oils will
help in selecting the relevant lubricants for different machines at different
temperatures.

B. Expected Program Outcomes (POs):


1. Basic and Discipline specific knowledge
2. Problem analysis
3. Design/Development of solutions
4. Engineering Tools, Experimentation and Testing
5. Engineering practices for society, sustainability and environment
6. Project Management
7. Life –Long learning

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BASIC CHEMISTRY (4300011)  Laboratory Manual

C. Expected Skills to be developed based on competency:


‘Use principles of Engineering Chemistry to solve broadly-defined engineering
problems.’
1. Determination of the viscosity of liquid lubricants using Redwood viscometer
No. 1
2. Selection of liquid lubricants for different types of Machinery.

D. Expected Course Outcomes (COs):


Use relevant fuels and lubricants for domestic and industrial applications.

E. Practical Outcomes (PrOs):


1. Determine the viscosity of given lubricating oil at different temperature using
Redwood Viscometer No. 1.
2. Selection of proper liquid lubricants in engineering based on their physical
properties like viscosity.

F. Expected Affective Domain Outcomes (ADOs):


The ADOs are best developed through laboratory/field-based exercises.
1. Work as a leader/a team member
2. Follow ethical practices
3. Observe safety measures
4. Good housekeeping
5. Time management
6. Practice environmentally friendly methods and processes for the sustainability
of the environment.
7. Handle tools/components/equipment carefully with necessary precautions

84 | Page
BASIC CHEMISTRY (4300011)  Laboratory Manual

G. Experimental set up/ Program Logic-Flow chart (CE & IT 1st and 2nd semester
software subjects only):

Redwood Viscometer No. 1

H. Prerequisite Theory:
Redwood viscometer is used to measure viscosity of lubricating oil. Redwood
viscometers are of two types based on their orifice size. Redwood viscometer No.
1 is commonly used for measuring viscosity of low viscous lubricating oils and it
has a jet of bore diameter 1.62 mm and length 10 mm. Redwood viscometer no.2
is used for measuring viscosity of highly viscous lubricating oil. It has a jet of bore
diameter 3.8 mm and length 15 mm. The unit of viscosity co-efficient is poise and
centipoise. It works on the principle of allowing a fixed volume of lubricating oil to
flow from a standard orifice at a fixed height and measuring the time of flow in
seconds. The viscosity of water at 20 ℃ is one centipoise and when the viscosity of
liquid measured with respect to water, it is call relative viscosity.

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BASIC CHEMISTRY (4300011)  Laboratory Manual

I. Resources/Equipment Required:
Instrument /
Sr. Equipment
Specification Quantity
No. / Components / Trainer
kit
Flow Range in second: 20-2000,
Redwood viscometer Redwood Viscometer Model No.: 01,
1. 03
No.1 Material: Stainless Steel,
Bath Capacity (Approx.): 7 litres
2. Kohlrausch flask Material: Glass, capacity: 50 mL 03
Timing capacity: Max. 23:59:59
(hours: minutes: seconds),
3. Stop watch Accuracy/Display Resolution: 0.1 03
second, operational keys: Start, Stop
& Reset, Water Resistance
4. Thermometer Temperature range: As per requirement 06
As per
5. Lubricating oil ................................................................
requirement
As per
6. Filter paper ................................................................
requirement

J. Safety and necessary Precautions to be followed:


1. Properly wash the oil cup with the help of suitable solvent.
2. Kohlrausch flask should be placed in exactly below the jet.
3. Accurately level the viscometer with the help of levelling screws.
4. Precisely observe the time of efflux for 50 mL fluid.

K. Procedure to be followed :
1. Clean the apparatus with the help of water.
2. The viscometer is levelled with the help of levelling screws.
3. The water bath is filled with water and a thermometer is placed in the water
bath.
4. Clean the oil cup and place the ball-valve rod on the agate jet to close it.
5. Place empty cleaned Kohlrausch flask below the jet.
6. Pour the experimental oil sample into the oil cup up to the tip of pointer.
7. Put the thermometer in the oil cup to read the temperature of oil sample and
cover it with a lid.

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BASIC CHEMISTRY (4300011)  Laboratory Manual

8. The water bath is heated slowly up to certain temperature with constant


stirring the water.
9. When the oil is at the desired temperature the heating is stopped and the ball
valve is lifted and the thermometer is suspended from the jacket.
10. The time of efflux for 50 mL of the oil to collect in the Kohlrausch flask is noted
and then the ball valve is immediately closed, to prevent any overflow of the
oil.
11. Repeat the experiment for different temperatures and note the respective
times of efflux of lubricating oil and water sample.

L. Calculations & Observations :


⮞ Observations:
1. Viscosity of given lubricating oil, ɳ1 = poise (calculate & write)
2. Viscosity of water, ɳ2 = 0.010019 poise (given)
3. Density of given lubricating oil, d1 = g/cm3 (given)
4. Density of water, d2 = 1 g/cm3
5. Time of flow of given lubricating oil, t1 = second
6. Time of flow of water, t2 = second

⮞ Observation Table:
Measurement of time of efflux for water and lubricating oil sample:
Relative viscosity
Time of flow Time of flow
Sr. Temperature of lubricating oil,
of Water, of lubricating oil,
No. (℃ ) ɳ1 (poise)
t1 (sec) t2 (sec)
(Calculate & Write)
Room
1.
Temperature
2. 40
3. 50
4. 60
5. 70

⮞ Calculations:

The following relative viscosity is obtained when the viscosity of a fluid is related
to the viscosity of water.
ɳ1 d1t1
=
n2 d2t2

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BASIC CHEMISTRY (4300011)  Laboratory Manual

d1t1
∴ ɳ1 = ɳ2
d2t2

;where, ɳ1 = viscosity of given lubricating oil (poise) (calculate)


ɳ2 = viscosity of water = 0.010019 poise (given)
d1 = Density of given lubricating oil (gm/cm3) = .................. gm/cm3 (given)
d2 = Density of water = 1 gm/cm3 (given)
t1 = Time of flow of given lubricating oil (sec) (from observation table)
t2 = Time of flow in of water (sec) (from observation table)

(1) At room temperature:

d1t1
∴ ɳ1 = ɳ2
d2t2

∴ ɳ1 = 0.010019  ..............  ..............


1  ................

∴ ɳ1 = ................ poise
Similarly find ɳ1 for all other four observations.

(2) At 40o C temperature:

d1t1
∴ ɳ1 = ɳ2
d2t2

∴ ɳ1 = 0.010019  ..............  ..............


1  ................

∴ ɳ1 = ................ poise

(3) At 50o C temperature:

d1t1
∴ ɳ1 = ɳ2
d2t2

∴ ɳ1 = 0.010019  ..............  ..............


1  ................

∴ ɳ1 = ................ poise

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BASIC CHEMISTRY (4300011)  Laboratory Manual

(4) At 60o C temperature:

d1t1
∴ ɳ1 = ɳ2
d2t2

∴ ɳ1 = 0.010019  ..............  ..............


1  ................

∴ ɳ1 = ................ poise

(5) At 70o C temperature:

d1t1
∴ ɳ1 = ɳ2
d2t2

∴ ɳ1 = 0.010019  ..............  ..............


1  ................

∴ ɳ1 = ................ poise

M. Results :
1. The viscosity of given lubricating oil at room temperature is poise.
2. The viscosity of lubricating oil at 40℃ is ............... poise.
3. The viscosity of lubricating oil at 50℃ is ............... poise.
4. The viscosity of lubricating oil at 60℃ is ............... poise.
5. The viscosity of lubricating oil at 70℃ is ............... poise.

N. Interpretation of Results :
…..................................................................................................................................
.............….....................................................................................................................
.....................................................................................................................................
.....................................................................................................................................

O. Conclusion :
…..................................................................................................................................
.............….....................................................................................................................

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BASIC CHEMISTRY (4300011)  Laboratory Manual

P. Practical related Quiz :


(1) Define : Viscosity of lubricating oil. Give its unit.
Ans. ..........................................................................................................................
...........................................................................................................................
...........................................................................................................................
(2) State the temperature effect on the viscosity of lubricating oils.
Ans. ..........................................................................................................................
...........................................................................................................................
(3) Write the differences between Redwood Viscometer No. 1 and 2.
Ans. ..........................................................................................................................
...........................................................................................................................
...........................................................................................................................
...........................................................................................................................
...........................................................................................................................
(4) Write precautions that should be taken during performing the experiment.
Ans. ..........................................................................................................................
...........................................................................................................................
...........................................................................................................................
...........................................................................................................................
(5) The volume capacity of the Kohlrausch flask is .................. .
Ans. ..........................................................................................................................

Q. References / Suggestions:
1. Engineering Chemistry by Jain & Jain, Dhanpat Rai Publishing Co. (P) Ltd, New
Delhi, ISBN: 93-521-6000-2.
2. Engineering Chemistry by Shikha Agarwal, Cambridge Uni. Press, New Delhi,
2013, ISBN: 9788126543342.
3. A Textbook of Engineering Chemistry by Dr. S. S. Dara & Dr. S. S. Umare, S.
Chand & Co.(P) Ltd., New Delhi, 2014, ISBN:81-219-0359-9.
Students should search and write any one reference relevant to this experiment
...................................................................................................................................

R. Assessment-Rubrics
As mentioned in (1) Rubrics (Pg. 10) and (2) Continuous Assessment (CA) (Pg. 12) is
to be done by the course faculty member.

 Remarks (if any) : ...................................................................................................

 Signature of the course Faculty Member with Date : ..........................................

102 | Page
BASIC CHEMISTRY (4300011)  Laboratory Manual

Date: ...... - ...... - 202…..

Practical No. 11
Determine the Acid value of the given lubricating oil.
( Acid value of Lubricating oil )

A. Objective:
Determination of acidity is more common and is expressed in terms of Acid
number or Acid value. Lubricating oil should have acid value less than 0.1. A value
above 0.1 indicates that the oil is oxidized. Some lubricating oils contain some
acidic components which are harmful as they can lead to corrosion. If the lubricant
undergoes oxidizing action during the lubricating action, the acidity or acid
number increases. A good lubricant is one which does not possess acidity and is
not liable to be oxidized to an acid. Properly refined lubricants are generally non-
acidic and therefore do not cause corrosion, but most petroleum-based lubricating
oils naturally contain various organic compounds that have some acidic properties.

B. Expected Program Outcomes (POs):


1. Basic and Discipline specific knowledge
2. Problem analysis
3. Design/Development of solutions
4. Engineering Tools, Experimentation and Testing
5. Engineering practices for society, sustainability and environment
6. Project Management
7. Life –Long learning

C. Expected Skills to be developed based on competency:


‘Use principles of Engineering Chemistry to solve broadly-defined engineering
problems.’
1. Determination of the acid value of liquid lubricants using titration method.
2. Selection of liquid lubricants for different types of Machinery.

D. Expected Course Outcomes (COs):


Use relevant fuels and lubricants for domestic and industrial applications.

Page | 103
BASIC CHEMISTRY (4300011)  Laboratory Manual

E. Practical Outcomes (PrOs):


1. Determine the acid value of given lubricating oil using titration method.
2. Selection of proper liquid lubricants for engineering use based on their
chemical properties like acid value.

F. Expected Affective Domain Outcomes (ADOs):


The ADOs are best developed through laboratory/field-based exercises.
1. Work as a leader/a team member
2. Follow ethical practices
3. Observe safety measures
4. Good housekeeping
5. Time management
6. Practice environmentally friendly methods and processes for the sustainability
of the environment.
7. Handle tools/components/equipment carefully with necessary precautions

G. Experimental set up/ Program Logic-Flow chart (CE & IT 1st and 2nd semester
software subjects only):

Titration Method

104 | Page
BASIC CHEMISTRY (4300011)  Laboratory Manual

H. Prerequisite Theory:
The acid number is an indication of the acidic or basic constituents of lubricating
oils. Neutralisation number, Acid number or Acid value of lubricating oil can be
defined as “The number of milligrams of KOH required to neutralize the free
acids present in 1 gram of the oil.” A known weight of lubricating oil is dissolved
in a neutral alcohol and titrated against 0.1 N KOH solution using phenolphthalein
as the indicator. The following formula can be made to calculate the acid value.
Volume of 0.1 N KOH required (X mL)  Normality of KOH  56.1
Acid Value = Weight of lubricating oil taken,W (gm)

I. Resources/Equipment Required:
Sr. Instrument/Equipment
No. /Components/Trainer kit Specification Quantity

1. Burette Borosilicate glass, 50 mL One per group

2. Conical flask Borosilicate glass, 250 mL One per group

3. Measuring cylinder Borosilicate glass, 250 mL One per group

4. Beaker Borosilicate glass, 100 mL One per group

5. Burette stand Iron or plastic material One per group


Chemicals:
Lubricating oil, 0.1 N KOH, As per
6. Laboratory Reagent grade
Alcohol, Phenolphthalein requirement
(As an Indicator)
Type of laboratory balance:
analytical, Sensitivity (mg): 1
Laboratory weighing mg, Maximum capacity of
7. weighing (grams): 200 g, 01
balance Shape of PAN: circular,
Display: LED

J. Safety and necessary Precautions to be followed:


1. Properly wash all the glassware with the help of distilled water.
2. All the glassware should be rinsed properly before it is used.
3. Handle all the glassware and chemicals/solutions very safely and carefully.
4. Remove the air bubble if present in the nozzle of the burette before taking
the burette reading.

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BASIC CHEMISTRY (4300011)  Laboratory Manual

5. Use white glazed tile to accurately observe the colour change at the
endpoint reading during the experiment.
6. The conical flask should be continuously shaking well during the addition
of the solution from the burette.
K. Procedure to be followed :
1. Clean the apparatus with the help of distilled water.
2. Fill 0.1 N KOH solution into the burette through a funnel upto the zero mark.
3. Weigh 1 to 2 g of the lubricating oil into 250 mL conical flask.
4. Add 100 mL of the mixture of alcohol and water (1:1) to dissolve the
lubricating oil.
5. Add 1-2 drops of phenolphthalein indicator to the conical flask.
6. The contents of the conical flask are titrated against 0.1 N KOH solution, till the
faint pink colour is obtained.
7. Take the initial and final reading of the burette to record in the observation
table.
8. Repeat the procedure until three concordant readings are obtained and it is
recorded in the observation table.

L. Calculations & Observations :


⮞ Observations:
1. Weight of given lubricating oil, W = g
2. Burette: 0.1 N KOH solution
3. Conical flask: 1 to 2 gm of lubricating oil + 100 mL of the mixture of alcohol
and water (1:1)
4. Indicator: 1-2 drops of Phenolphthalein solution
5. Colour change: Colourless to Pink
⮞ Observation Table:

Mean (Average)
Burette Pilot reading I II III
reading,
Reading (mL) (mL) (mL) (mL)
(mL) = (I + II + III)/3
mL
Final reading mL mL mL Volume of 0.1 N
(Whole No.)
KOH solution
Initial reading 0.0 mL mL mL mL
required,
Difference mL X = ........... mL
mL mL mL
= F.r.–I.r. (Whole No.)

⮞ Calculations:

106 | Page
BASIC CHEMISTRY (4300011)  Laboratory Manual

Acid value of the given lubricating oil can be calculated by


Volume of 0.1 N KOH required (X mL)  Normality of KOH  56.1
Acid value = Weight of lubricating oil taken,W (g)

 Acid value = ...............  0.1  56.1


................

 Acid value = ...............

M. Results :
Acid value of the given lubricating oil = ...................... .

N. Interpretation of Results :
…..................................................................................................................................
.............….....................................................................................................................
.....................................................................................................................................
.....................................................................................................................................

O. Conclusion :
…..................................................................................................................................
.............….....................................................................................................................

P. Practical related Quiz :


(1) Define: Acid value of lubricating oil.
Ans. ..........................................................................................................................
...........................................................................................................................
(2) State the effect of using lubricating oil which has an acid value greater than
1 in machinery.
Ans. ..........................................................................................................................
...........................................................................................................................
(3) Calculate the molecular mass of potassium hydroxide (KOH).
Ans. ..........................................................................................................................
...........................................................................................................................

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BASIC CHEMISTRY (4300011)  Laboratory Manual

(4) Write precautions that should be taken during performing the experiment.
Ans. ..........................................................................................................................
...........................................................................................................................
...........................................................................................................................
(5) Give the formula to calculate the acid value of lubricating oil.
Ans. ..........................................................................................................................
...........................................................................................................................
...........................................................................................................................

Q. References / Suggestions:
1. Engineering Chemistry by Jain & Jain, Dhanpat Rai Publishing Co. (P) Ltd, New
Delhi, ISBN: 93-521-6000-2.
2. Engineering Chemistry by Shikha Agarwal, Cambridge Uni. Press, New Delhi,
2013, ISBN: 9788126543342.
3. A Textbook of Engineering Chemistry by Dr. S. S. Dara & Dr. S. S. Umare, S. Chand &
Co.(P) Ltd., New Delhi, 2014, ISBN:81-219-0359-9.
Students should search and write any one reference relevant to this experiment
.....................................................................................................................................

R. Assessment-Rubrics
As mentioned in (1) Rubrics (Pg. 10) and (2) Continuous Assessment (CA) (Pg. 12) is
to be done by the course faculty member.

 Remarks (if any) : ......................................................................................................

 Signature of the course Faculty Member with Date : ...............................................

108 | Page
BASIC CHEMISTRY (4300011)  Laboratory Manual

Date: ...... - ...... - 202…..

Practical No. 12
Determine flash point and fire point of the given lubricating oil using Pensky-
Martens/Cleveland open cup/Abel’s flashpoint apparatus.
( Flash point & Fire point of Lubricating oil )

A. Objective:
Flash points and fire points of lubricating oils are required when the lubricating oils
are used at higher temperatures. So, the determination of flash points and fire
points is immensely important for lubricating oils. This method helps to detect
highly volatile constituents of the lubricating oils. If they are highly volatile at
normal temperatures, their escaping vapours can cause fire hazards. Hence, it
ensures safety against fire hazards during storage, transportation and use of
lubricating oil. A good lubricant should have flash point at least above the
temperature at which it is to be used.

B. Expected Program Outcomes (POs):


1. Basic and Discipline specific knowledge
2. Problem analysis
3. Design/Development of solutions
4. Engineering Tools, Experimentation and Testing
5. Engineering practices for society, sustainability and environment
6. Project Management
7. Life –Long learning

C. Expected Skills to be developed based on competency:


‘Use principles of Engineering Chemistry to solve broadly-defined engineering
problems.’
1. Determination of the flash point and fire point of liquid lubricants using
Pensky-Marten’s apparatus/ Cleveland open cup/Abel’s flashpoint apparatus.
2. Selection of liquid lubricants for machinery operating at different
temperatures.

Page | 109
BASIC CHEMISTRY (4300011)  Laboratory Manual

D. Expected Course Outcomes (COs):


Use relevant fuels and lubricants for domestic and industrial applications.

E. Practical Outcomes (PrOs):


1. Determine the flash point and fire point of given lubricating oil using Pensky-
Marten’s apparatus/ Cleveland open cup/Abel’s flashpoint apparatus.
2. Selection of proper liquid lubricants for engineering use based on their
physical properties like flash point and fire point.

F. Expected Affective Domain Outcomes (ADOs):


The ADOs are best developed through laboratory/field-based exercises.
1. Work as a leader/a team member
2. Follow ethical practices
3. Observe safety measures
4. Good housekeeping
5. Time management
6. Practice environmentally friendly methods and processes for the sustainability
of the environment
7. Handle tools/components/equipment carefully with necessary precautions

G. Experimental set up:

Pensky-Marten’s apparatus

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BASIC CHEMISTRY (4300011)  Laboratory Manual

H. Prerequisite Theory:
“Flash point is the lowest temperature at which the liquid lubricant gives
momentary flash of light when a flame is applied to it, but it does not continue to
burn. “Fire point is the lowest temperature at which the vapours of the liquid
lubricant catch fire and burns continuously for at least 5 seconds when the small
flame is applied near to it.” The fire points of liquid lubricants are 5 to 40 ℃ higher
than the flash points. So that the fire point of a lubricating oil is always greater
than its flash point. The flash points and fire points of lubricating oil are
determined using Pensky-Marten’s apparatus/Cleveland open cup/Abel’s
flashpoint apparatus.
I. Resources/Equipment Required:
Instrument /
Sr. Equipment
No. / Components / Specification Quantity
Trainer kit
Pensky-Marten’s apparatus:
Ignition source: Electric, Measuring Range:
Pensky- Ambient to 370℃ or more, Heat rate: 0.5 °C
Marten’s to 12 °C per minute. Sample Stirrer: manual or
apparatus automatic, Accessories: Brass Test Cup with
Handle, Thermometer Holder, Cover Assembly
OR etc. Voltage: 220-240V.
OR
Cleveland open Cleveland open cup apparatus:
cup Temperature range: Ambient to 370℃ or
1. 03
more, Temp. measurement PT100 temp.
OR sensor, Temp. scale resolution 0.1℃, Ignition
source: Electric, cooling forced air cooling,
Abel’s heating coil, heating 888W,220V, AC.
flashpoint OR
apparatus. Abel’s flashpoint apparatus:
Material: Stainless Steel, Power Source:
Electric, Voltage: 115V/220- 240V, 50-60 Hz,
Temperature Range: up to 110℃, Temp. scale
Resolution: 0.1 ℃
2. Thermometer Temperature range: As per requirement 03
As per
3. Lubricating oil ................................................................................. requireme
nt

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J. Safety and necessary Precautions to be followed:


1. The oil cup should be dried and cleaned.
2. Breathing over the surface of the lubricating oil should be avoided.
3. The stirring of the lubricating oil should be stopped at the time of applying
the test flame.
K. Procedure to be followed :
1. The lubricating oil under is filled up to the mark in the oil cup.
2. Set the thermometer vertically in the oil cup with the help of clamp.
3. The stirrer is rotated at about 1 to 2 revolutions per second and switch on the
electrical heating device.
4. The lubricating oil is heated so that the oil temperature is raised by about 5 ℃
per minute.
5. The test flame is immersed in oil vapour for about 1 second at a rate of 1 ℃
rise in temperature by operating the shutter.
6. Note the temperature at which a distinct flash is observed inside the cup.
7. The heating is continued further and record the temperature at which the
lubricating oil ignites and continues to burn for at least 5 seconds.
8. Note the temperature reading as the fire point of the lubricating oil.

L. Observation Table and Calculations:


⮞ Observation Table:

Observation of
Sr. Flash point (oC)
Temperature (oC)
No. and Fire point (oC)
(during heating)
o o
1. t1 = C Flash point = C
o o
2. t2 = C Flash point = C
o o
3. t3 = C Flash point = C
o o
4. t4 = C Fire point = C
o o
5. t5 = C Fire point = C
o o
6. t6 = C Fire point = C

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BASIC CHEMISTRY (4300011)  Laboratory Manual

⮞ Calculations:
1. Average value of flash point of the given lubricating oil
= (t1 + t2 + t3)/3
= (.............. + .............. + .............. ) / 3
= .............. / 3
= .............. ℃.

2. Average value of the fire point of given lubricating oil = (t4 + t5 + t6)/3
= (t1 + t2 + t3)/3
= (.............. + .............. + .............. ) / 3
= .............. / 3
= .............. ℃.

M. Results:
1. The flash point of the given lubricating oil = .............. ℃.
2. The fire point of the given lubricating oil =...............℃.

N. Interpretation of Results:
…..................................................................................................................................
.............….....................................................................................................................
.....................................................................................................................................
.....................................................................................................................................

O. Conclusion:
…..................................................................................................................................
.............….....................................................................................................................

P. Practical related Quiz:


(1) Define: Flash point, Fire point.
Ans. ..........................................................................................................................
...........................................................................................................................
...........................................................................................................................
...........................................................................................................................
...........................................................................................................................
...........................................................................................................................

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BASIC CHEMISTRY (4300011)  Laboratory Manual

(2) The fire point of the given lubricating oil is .................. higher than
the flash point.
Ans. ..........................................................................................................................
...........................................................................................................................
(3) Write precautions that should be taken while performing the
experiment.
Ans. ..........................................................................................................................
...........................................................................................................................
...........................................................................................................................
...........................................................................................................................
(4) Which apparatus can be used to find out the flash point and fire point
of the lubricating oil?
Ans. ...........................................................................................................................
...........................................................................................................................
...........................................................................................................................
...........................................................................................................................
(5) The fire point is the lowest temperature at which the vapour of
lubricating oil catches the fire and burns continuously for at least
......................... when a small flame is brought near to it.
Ans. ...........................................................................................................................

Q. References / Suggestions:
1. Engineering Chemistry by Jain & Jain, Dhanpat Rai Publishing Co. (P) Ltd, New
Delhi, ISBN: 93-521-6000-2.
2. Engineering Chemistry by Shikha Agarwal, Cambridge Uni. Press, New Delhi,
2013, ISBN: 9788126543342.
3. A Textbook of Engineering Chemistry by Dr. S. S. Dara & Dr. S. S. Umare, S. Chand &
Co.(P) Ltd., New Delhi, 2014, ISBN:81-219-0359-9.
Students should search and write any one reference relevant to this experiment
.....................................................................................................................................

R. Assessment-Rubrics:
As mentioned in (1) Rubrics (Pg. 10) and (2) Continuous Assessment (CA) (Pg. 12) is
to be done by the course faculty member.

Remarks (if any): .......................................................................................................

Signature of the course Faculty Member with Date: ................................................


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BASIC CHEMISTRY (4300011)  Laboratory Manual

APPENDICES

APPENDIX No. Information Page No.


APP AR ATUS

1. EQUIPMENTS / INSTRUMENTS 129

GLASSWARE /PLASTICWARE / WOODEN /


2. 131
METAL LABWARE

CHEM IC ALS
3.
INORGANIC Side Reagents -
133
Compounds/Solutions

4.
ORGANIC Side Reagents -
135
Compounds/Solutions

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APPENDIX

APP AR ATUS

1. EQUIPMENTS / INSTRUMENTS

Equipments / Practical
No. Specifications
Instruments No.
Electronic Type of Laboratory Balance: Analytical,
Weighing Balance / Sensitivity (mg): 1 mg, Maximum Capacity
1, 6, 7, 8, 11,
1 Digital Weighing of weighing (grams): 200 g, Shape of PAN:
13, 14, 16
Balance (OR Circular, Power Supply: Single Phase,
Analytical Balance) Display: LED.
Number of stirring Positions:1, Calibration:
Automatic Calibration, Magnetic stirrer
Hot plate with with a hot plate, Speed Control Accuracy of
2 3
Magnetic stirrer set speed (+/-) (RPM): 5, Maximum Stirring
capacity per position: 3000 ml,Top plate
Material: Stainless steel
Type: Microcontroller Based, Display:
LED / LCD / Touch Screen, 3 digits,
Calibration: up to 3 points with auto
buffer, pH Range (pH): 0.00 to 14.00,
+/- 0.05, Power Requirements: 230 V
3 Digital pH meter +/- 10, 50 Hz AC, Modes: pH mV- C, 4, 8
Temperature Compensation Type:
Automatic Temperature Compensation
Range (Degree C): 0 to 100,
Temperature Accuracy (Degree C): +/-
0.3, Resolution (pH): 0.01
The input range is from ± 1 V to ± 1000 V.
Accuracy: The accuracy is about ± 1 percent
4 Voltmeter 5
for a 3-digit digital voltmeter and ± 0.0002
percent for a 6-digit digital voltmeter.
5 6 V Battery As per requirement 6

6 Ammeter As per requirement 6

7 Rheostat As per requirement 6

8 Dryer As per requirement 7, 8


Temperature is controlled by digital
9 Hot air oven 11
temperature indicator cum controller from

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BASIC CHEMISTRY (4300011)  Laboratory Manual

ambient to 250°C with ± 0.1°C Accuracy.


Power supply: 220/230V, 50Hz single
phase, Capacity (Approx.): 50 – 100 liter,
Type of Shelves: 03, Material of Inner
Chambers: SS 304, Material of Outer
Chamber: MS with powder coated paint,
Material of Shelves: SS wire mesh.
Glass flask equipped with a side arm for
vacuum pump connection and a rubber
Vacuum Pumps
10 stopper to provide seal with funnel. The 11
with glass filter
flask is used to collect the filtered process
water that passes through the filter.
Flow Range in second: 20-2000,
Redwood Redwood Viscometer Model No.: 01,
11 12
viscometer No.1 Material: Stainless Steel,
Bath Capacity (Approx.): 7 litres
Timing capacity: Max. 23:59:59 (hours:
minutes: seconds), Accuracy/Display
12 Stop watch Resolution: 0.1 second, operational 12
keys: Start, Stop & Reset, Water
Resistance
Pensky-Marten’s apparatus:
Ignition source: Electric, Measuring
Range: Ambient to 370℃ or more, Heat
rate: 0.5 °C to 12 °C per minute. Sample
Stirrer: manual or automatic,
Pensky-Marten’s Accessories: Brass Test Cup with
apparatus Handle, Thermometer Holder, Cover
Assembly etc. Voltage: 220-240V.
OR OR
Cleveland open cup apparatus:
Cleveland open Temperature range: Ambient to 370℃
13 15
cup or more, Temp. measurement PT100
temp. sensor, Temp. scale resolution
OR 0.1℃, Ignition source: Electric, cooling
forced air cooling, heating coil, heating
Abel’s flashpoint 888W,220V, AC.
apparatus OR
Abel’s flashpoint apparatus:
Material: Stainless Steel, Power Source:
Electric, Voltage: 115V/220- 240V, 50-
60 Hz, Temperature Range: up to
110℃, Temp. scale Resolution: 0.1 ℃

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APPENDIX

2. GLASSWARE / PLASTICWARE / WOODEN / METAL LABWARE

Specifications
No. Apparatus Practical No.
(G/P/W/ML)
1 Watch glass G 1
Standard volumetric flask
2 G 1
with stopper (100 mL)
3 Funnel G/P 1, 2, 3, 7, 8, 9, 10, 16

4 Beakers (250 mL, 500mL) G/P 1

5 Beakers (250 mL, 100mL) G/P 2, 3, 9, 16

6 Beaker (25 mL) G/P 4


Beakers (250 mL) : 3.9" tall,
and has an inner diameter of
7 G/P 6, 7, 8, 14
65.8mm and an outer
diameter of 68mm.
8 Beakers (250 mL, 150mL) G/P 16

9 Wash bottle (500 mL) P 1, 2, 3, 4, 9, 10,

10 Burette (50 mL) G 2, 3, 9, 10, 13, 14

11 Burette stand ML/P 2, 3, 9, 10, 13, 14

12 White glazed tile Ceramic Material 2, 3, 4, 9, 10

13 Conical flask (100 mL) G 2, 3, 9

14 Conical flask (250 mL) G 10, 13, 14

15 Pipette (10 mL) G 2, 3, 4, 9, 10, 13, 14

16 Measuring flask (100 mL) G 4, 9

17 Measuring flask (500 mL) G 10

18 Test tube stand P/W 4, 16


Test tubes (100 mm  13
19 G 4, 16
mm  11 mm)
Insulated metallic
20 Connecting Wires 5
wires

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21 Salt-bridge G 5

22 Glass rod G 7, 8, 16

23 Pair of tongs Steel 7, 8

24 Measuring cylinder (10 mL) G 7, 8, 16

25 Measuring cylinder (250 mL) G 13, 14

26 Graduated Cylinders G 11

27 Policeman Rubber & Steel 7, 8

28 Evaporating Dish G 11

29 Gooch Crucibles Porcelain 11

30 Dish Tongs Heat resistant metal 11

31 Crucible Tongs Heat resistant metal 11

32 Forceps P/ML 11
G
sealable enclosures
33 Desiccator containing desiccants 11
used for preserving
moisture
34 Kohlrausch flask G 12
Temperature range: As
35 Thermometer 12, 15
per requirement
36 Round Bottom Flask (RBF) G 14

37 Reflux condenser G 14
ML - Water bath
Chamber Capacity:
38 Boiling water bath 14
Approx. 8 to 10
litres.
39 Dropper G 16

 IMPORTANT :
 Handle the Glassware very carefully.
 Return back all the Apparatus after their use.

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APPENDIX

CHEM IC ALS

3. INORGANIC Side Reagents


Compounds/Solutions

No. Reagents Concentration Practical No.


1 Distilled water - 1, 2, 3, 4, 7, 8, 16
2 Potassium permanganate (KMnO4) Solid 1
3 dil. NaOH solution 0.1 M 2, 4,
4 KMnO4 solution 0.1 M 3
5 dil. FeSO4.7H2O solution 0.1 M 3
6 dilute H2SO4 solution 3
7 Buffer solution (pH 2) 4
8 Buffer solution (pH 2) 4
9 dil. HCl solution 0.1 M 4
10 dilute NaHCO3 solution 4
11 Tap water 4
12 Soap solution 4
13 Butter milk/Lemon solution 4
1 M, different x
14 Zinc sulphate (ZnSO4) 5,
M
1 M, different y
15 Copper sulphate (CuSO4) 5, 6
M
16 Copper sulphate (CuSO4) 0.2 N 5,
17 KCl solution 5
18 Iron (Fe) pieces 7, 8
19 Zinc (Zn) pieces 7, 8
20 Aluminium (Al) pieces 7, 8
21 conc. HCl 7, 8, 9
22 Sodium hydroxide (NaOH) 7, 8, 9
23 Sodium chloride (NaCl) 7, 8

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BASIC CHEMISTRY (4300011)  Laboratory Manual

24 Magnesium chloride hexahydrate 9


25 Calcium carbonate (CaCO3) 9
26 Ammonia buffer solution 9
27 0.1 N KOH solution 13
28 Alcoholic 0.5 N KOH solution 14
29 0.5 N HCl solution 14
30 conc. Sulphuric acid (H2SO4) 16
31 pH strips (pH papers) 8
32 Whatman Filter paper 11
33 Filter paper 12, 16
Blue litmus paper
Red litmus paper
Starch paper
Turmeric paper
Porcelain pieces
Copper (Cu )foil

 IMPORTANT :
 Use the Chemicals Judiciously.
 Put the reagent bottles at their own places after their use.
 Don’t waste the chemicals.

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APPENDIX

4. ORGANIC Side Reagents


Compounds/Solutions

No. Reagents Practical No.


1 Oxalic acid (hydrated) (H2C2O4.2H2O) 1, 2, 3
Oxalic acid (hydrated) (H2C2O4.2H2O)
2 2, 3
solution (Standard solution) (0.1 M)
3 Universal indicator solution 4
4 Lubricating oil 12, 13, 15
5 Methanol 13, 14
6 Ethanol 13, 14
7 Glacial acetic acid 16
8 40% formaldehyde solution 16
9 Phenol 16
10 Phenolphthalein indicator (0.5%) 2, 10, 13, 14
11 Methyl orange indicator (0.05%) 10
12 Eriochrome Black-T (EBT) indicator 9
13 Disodium salt of EDTA 9

 IMPORTANT :
 Don’t waste the chemicals.
 Put the Side reagent bottles at their own places after their use.

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