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Chemistry Lab Manual SPPU

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0% found this document useful (0 votes)
516 views108 pages

Chemistry Lab Manual SPPU

Uploaded by

yashdeshmukh711
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PDF, TXT or read online on Scribd
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Marathwada Mitramandal’s College of Engineering, Karvenagar, Pune - 52

First Year Engineering (2019 Pattern) Semester I / II Engineering Chemistry

Marathwada Mitramandal’s
College of Engineering
Permanently Affiliated to SPPU | Accredited with ‘A’ grade by NAAC |
Recipient of ‘Best College’ award by SPPU | Accredited by NBA (Electrical
and Mechanical Engg.) | Recognized under 2(f) and 12(B) of UGC Act 1956

Sr. No. 18, Plot No. 5/3, CTS.No. 205,


Behind Vandevi Temple,
Karvenagar, Pune-411052
Tel.: (020) 25473160 E-mail:
[email protected]
Website: www.mmcoe.edu.in
______________________________________________________________________________

DEPARTMENT OF ENGINEERING SCIENCES

First Year Engineering


Academic Year: 20 ___ - 20 ___
Semester:_____
Subject: Engineering Chemistry
Subject Code - 107009
Laboratory Manual and Workbook

Nameof Student:
_____________________________________________

Division: _____ Roll No.: ___________ Batch: __________

SPPU Exam Seat Number: __________________________________

FE 2019 Pattern
Marathwada Mitramandal’s College of Engineering, Karvenagar, Pune - 52
First Year Engineering (2019 Pattern) Semester I / II Engineering Chemistry

FE 2019 Pattern
Marathwada Mitramandal’s College of Engineering, Karvenagar, Pune - 52
First Year Engineering (2019 Pattern) Semester I / II Engineering Chemistry

INDEX
Sr. Title Date Remark Signature
No. of Faculty

1 Hardness of water sample

2 Alkalinity of water sample

3 Conductometry

4 pH metry

5 Preparation of polymer

6 Proximate Analysis

7 Colorimetry

8 Electroplating

Electroless plating (Content Beyond


9
Syllabus)

10 Phosphate content in Soft Drinks (V-Lab)

11 Soil Analysis – Kjeldahl’s Method (V-Lab)

CERTIFICATE

This is to certify that


Name of the student: ________________________________________________________________________________

Division: _______ Roll No.: ______________________ SPPU Exam Seat No.: __________________________________

of First Year Engineering has satisfactorily completed the term work in the subject of Engineering
Chemistry in the Department of Engineering Sciences of Marathwada Mitramandal’s College of
Engineering, Karvenagar, Pune - 52 as prescribed by Savitribai Phule Pune University.
Date:

Faculty In-Charge Head of Dept. Principal


MMCOE

FE 2019 Pattern
Marathwada Mitramandal’s College of Engineering, Karvenagar, Pune - 52
First Year Engineering (2019 Pattern) Semester I / II Engineering Chemistry

Marathwada Mitramandal’s College of Engineering


Vision: To aspire for the Welfare of Society through excellence in Science and
Technology.

Mission:
Our Mission is to
Mould young talent for higher endeavors.
Meet the challenges of globalization.
Commit for socially progress with values and ethics.
Orient faculty and students for research and development.
Emphasize excellence in all disciplines.

Department of Engineering Sciences


Vision: Empowering Engineering Aspirants with knowledge, skills and moral values

Mission: To provide broad theoretical and practical knowledge of Basic Science and
Engineering to the students that can be applied for betterment of Society.

OBJECTIVES:
1. To develop higher order thinking abilities by imparting basic and advanced
knowledge

2. To provide necessary platform for enhancing personal skills and talents

3. To create awareness and sensitivity about social issues

FE 2019 Pattern
Marathwada Mitramandal’s College of Engineering, Karvenagar, Pune - 52
First Year Engineering (2019 Pattern) Semester I / II Engineering Chemistry

First Engineering Structure for Semester I and Semester II


Teaching Scheme Examination Scheme and
Credits
(Hours/Week) Marks
Course Course
Code Name
Theory Practical Tutorial ISE ESE TW PR OR Total TH PR TUT Total

Engineering
107009 Chemistry 4 2 -- 30 70 -- 25 -- 125 4 1 -- 5

107002: Engineering Chemistry


Teaching Scheme: Credits: 05 Examination Scheme:
TH: 04 Hr/week In-Semester :30 Marks
PR: 02 Hr/week End-Semester :70 Marks
PR :25 Marks

Prerequisite Courses, if any:


Types of titrations, volumetric analysis, structure property relationship, types of crystals, periodic
table, classification and properties of polymers, electromagnetic radiation, electrochemical series

Companion Course, if any: Laboratory Practical

Course Objectives:
1. To understand technology involved in analysis and improving the quality of water as a
commodity.
2. To acquire the knowledge of electro-analytical techniques that facilitates rapid and precise
understanding of materials.
3. To understand structure, properties and applications of speciality polymers and nano material.
4. To study conventional and alternative fuels with respect to their properties and applications.
5. To study spectroscopic techniques for chemical analysis.
6. To understand corrosion mechanisms and preventive methods for corrosion control.

Course Outcomes:
On completion of the course, learner will be able to–
CO1: Apply the different methodologies for analysis of water and techniques involved in softening
of water as a commodity.
CO2: Select appropriate electro-technique and method of material analysis.
CO3: Demonstrate the knowledge of advanced engineering materials for various engineering
applications.

FE 2019 Pattern
Marathwada Mitramandal’s College of Engineering, Karvenagar, Pune - 52
First Year Engineering (2019 Pattern) Semester I / II Engineering Chemistry

CO4: Analyze fuel and suggest use of alternative fuels.


CO5: Identify chemical compounds based on their structure.
CO6: Explain causes of corrosion and methods for minimizing corrosion.

Course Contents

Unit I Water Technology (08 Hrs)

Impurities in water, hardness of water: Types, Units and Numericals. Determination of hardness (by
EDTA method using molarity concept) and alkalinity, numericals. Ill effects of hard water in boiler -
priming and foaming, boiler corrosion, caustic embrittlement, scale and sludge. Water treatment: i)
Zeolite method and numericals ii) Demineralization method. Purification of water: Reverse osmosis
and Electrodialysis.

Unit II Instrumental Methods of Analysis (08 Hrs)

Introduction: Types of reference electrode (calomel electrode), indicator electrode (glass electrode),
ion selective electrode: ion selective membranes such as solid membrane, enzyme based membrane
and gas sensing membrane.
[A] Conductometry: Introduction, conductivity cell, conductometric titrations of acid versus base
with titration curve.
[B] pHmetry: Introduction, standardization of pH meter, pH metric titration of strong acid versus
strong base with titration curve.

Unit III Engineering Materials (08 Hrs)

A] Speciality polymers: Introduction, preparation, properties and applications of the following


polymers:
1. Engineering Thermoplastic: Polycarbonate,
2. Biodegradable polymers: Poly (hydroxybutyrate-hydroxyvalerate),
3. Conducting Polymer: Polyacetylene,
4. Electroluminescent polymer: Polyphenylene Vinylene,
5. Polymer composites: Fiber reinforced plastic (FRP)- Glass reinforced and Carbon reinforced
polymer composite.
[B] Nanomaterials: Introduction, classification of nanomaterial based on dimensions (zero
dimensional, one-dimensional, two-dimensional and three-dimensional), structure, properties and
applications of graphene and carbon nanotubes, quantum dots (semiconductor nanoparticles).

Unit IV Fuels (08 Hrs)

Introduction (definition, classification of fuel based on chemical reactions and characteristics of an


ideal fuel), Calorific value (CV): Higher calorific value (HCV) and Lower calorific value (LCV),
Determination of Calorific value: Principle, construction and working of Bomb calorimeter and

FE 2019 Pattern
Marathwada Mitramandal’s College of Engineering, Karvenagar, Pune - 52
First Year Engineering (2019 Pattern) Semester I / II Engineering Chemistry

Boy’s gas calorimeter and numericals, Solid fuel: Coal: Analysis of Coal-Proximate and Ultimate
analysis, numericals, Liquid fuel: Petroleum: Refining of petroleum /crude oil and composition,
boiling range and uses of various fractions,
Gaseous fuel: Composition, properties and applications of CNG. Hydrogen gas as a future fuel
Alternative fuels: Power alcohol and biodiesel.

Unit V Spectroscopic Techniques (08 Hrs)

[A]UV-Visible Spectroscopy:
Introduction, interaction of electromagnetic radiation with matter, statement of Beer’s law and
Lambert’s law, absorption of UV radiation by organic molecule leading to different electronic
transitions, terms involved in UV-visible Spectroscopy- chromophore, auxochrome, bathochromic
shift, hypsochromic shift, hyperchromic shift and hypochromic shift, Instrumentation and basic
principle of single beam spectrophotometer, applications of UV-visible spectroscopy.
[B] Infra red Spectroscopy:
Introduction, Principle of IR Spectroscopy, types of vibrations: Stretching (symmetric and
asymmetric) and bending (scissoring, rocking, wagging and twisting), conditions of absorption of IR
radiations, vibration of diatomic and polyatomic molecules. Instrumentation with block diagram.
Parts of IR spectrum, fundamental group region, fingerprint region, applications of IR spectroscopy.

Unit VI Corrosion Science (08 Hrs)

Introduction, Types of corrosion – Dry and Wet corrosion, mechanism of dry corrosion, nature of
oxide films and Pilling-Bedworth’s rule, wet corrosion – mechanism: hydrogen evolution and
oxygen absorption, galvanic cell corrosion, concentration cell corrosion, Factors influencing rate of
corrosion. Methods of corrosion control and prevention: cathodic and anodic protection, metallic
coatings and its types, surface preparation, methods to apply metallic coatings-hot dipping,
cladding, electroplating, cementation.

Books & Other Resources:

Text Books:
1. Engineering Chemistry by O .G. Palanna, Tata Mcgraw Hill Education Pvt. Ltd.
2. Textbook of Engineering Chemistry by Dr. S. S. Dara, Dr. S. S. Umare, & Company Ltd.
3. Textbook of Engineering Chemistry by Dr. Sunita Rattan, S. K. Kataria & Sons Publisher

Reference Books:
1. Engineering Chemistry, Wiley India Pvt. Ltd.
2. Inorganic Chemistry, 5 ed by Shriver and Atkins, Oxford University Press
3. Basic Concept of Analytical Chemistry, 2ed , S. M. Khopkar, New Age-International Publisher
4. Instrumental Methods of Chemical Analysis, G. R. Chatwal, Himalaya Publishing House
5. Spectroscopy of organic compounds, 2 ed, P. S. Kalsi, New Age-International Ltd., Publisher
6. Polymer Science, V. R. Gowarikar, N. V. Viswanathan, jayadevSreedhar, Wiley Eastern Limited

FE 2019 Pattern
Marathwada Mitramandal’s College of Engineering, Karvenagar, Pune - 52
First Year Engineering (2019 Pattern) Semester I / II Engineering Chemistry

Instructions for Students


Before performing the experiment
1. Report to the laboratory in time. Keep your bags on the bag rack.
2. Keep your mobile phones switched off during the practicals.
3. Read and understand theory related experiment (from notes or books) and clear concepts
4. Carefully understand the explanation and demonstration of the experiment
5. Listen to the instructions carefully before performing the practical
6. Every experiment is to be performed in a batch. Take your own readings turn by turn.
7. Do not touch any unknown chemicals kept in the laboratory (to avoid any injury or accident).

During experiment
1. Clean the glasswares carefully and inform to lab assistant if any breakage
2. Make sure all the required glassware is kept on your practical table
3. Collect the solutions in beaker from solution bottle kept at one place
4. Make sure the burette/ apparatus are working properly.
5. Do not mix different solution except the experimental procedure
6. Plot the graph wherever required

After experiment
1. Return the solutions in the solution bottle after completion of the practical.
2. Clean the glass wares with water and keep on wooden rack
3. Do the calculations or draw the graph and show it to your instructor.

Instructions
1. Minimum eight experiments should be performed by every student in a semester
2. Few questions are given at the end of every experiment. These are to be written by students in
their own words after understanding the theory
3. Previous experiments should be checked before performing the next experiment.
4. The index page should get signed by the faculty after completion of checking of every
experiment.

FE 2019 Pattern
Marathwada Mitramandal’s College of Engineering, Karvenagar, Pune - 52
First Year Engineering (2019 Pattern) Semester I / II Engineering Chemistry

First Year Engineering (2095 pattern) (Common to All)


Semester I and II: Engineering Chemistry

Programme Outcomes:

1. Engineering knowledge: Apply the knowledge of mathematics, science, engineering fundamentals,


and an engineering specialization for the solution of complex engineering problems.
2. Problem analysis: Identify, formulate, research literature, and analyze complex engineering
problems reaching substantiated conclusions using first principles of mathematics, natural sciences, and
engineering sciences.
3. Design/development of solutions: Design solutions for complex engineering problems and design
system components or processes that meet the specified needs with appropriate consideration for public
health and safety, and cultural, societal, and environmental considerations.
4. Conduct investigations of complex problems: The problems that cannot be solved by
straightforward application of knowledge, theories and techniques applicable to the engineering
discipline.
5. Modern tool usage: Create, select, and apply appropriate techniques, resources, and modern
engineering and IT tools, including prediction and modeling to complex engineering activities, with an
understanding of the limitations.
6. The engineer and society: Apply reasoning informed by the contextual knowledge to assess
societal, health, safety, legal and cultural issues and the consequent responsibilities relevant to the
professional engineering practice.
7. Environment and sustainability: Understand the impact of the professional engineering solutions
in societal and environmental contexts, and demonstrate the knowledge of, and need for sustainable
development.
8. Ethics: Apply ethical principles and commit to professional ethics and responsibilities and norms of
the engineering practice.
9. Individual and team work: Function effectively as an individual, and as a member or leader in
diverse teams, and in multidisciplinary settings.
10. Communication: Communicate effectively on complex engineering activities with the engineering
community and with t h e society at large, such as, being able to comprehend and write effective reports
and design documentation, make effective presentations, and give and receive clear instructions.
11. Project management and finance: Demonstrate knowledge and understanding of t h e engineering
and management principles and apply these to one’s own work, as a member and leader in a team, to
manage projects and in multidisciplinary environments.
12. Life-long learning: Recognize the need for, and have the preparation and ability to engage in
independent and life-long learning in the broadest context of technological change.

FE 2019 Pattern
Marathwada Mitramandal’s College of Engineering, Karvenagar, Pune - 52
First Year Engineering (2019 Pattern) Semester I / II Engineering Chemistry

Engineering Chemistry
(107009)
Course Objectives:

1. To understand technology involved in analysis and improving quality of water as a


commodity.
2. To acquire the knowledge of electro-analytical techniques that facilitates rapid and
precise understanding of materials.
3. To understand structure, properties and applications of specialty polymers and nano
material.
4. To study conventional and alternative fuels with respect to their properties and
applications.
5. To study spectroscopic techniques for chemical analysis.
6. To understand corrosion mechanisms and preventive methods for corrosion control.

Course Outcomes:

On completion of this course the students are able to:

1) Apply the difference methodologies for analysis of water and techniques involved in
softening of water as commodity
2) Select appropriate electro-technique and method of material analysis
3) Demonstrate the knowledge of advanced engineering materials for various engineering
applications
4) Analyze fuel and suggest use of alternative fuels
5) Identify chemical compounds based on their structure
6) Explain causes of corrosion and methods for minimizing corrosion

FE 2019 Pattern
Marathwada Mitramandal’s College of Engineering, Karvenagar, Pune - 52
First Year Engineering (2019 Pattern) Semester I / II Engineering Chemistry

CO-PO Mapping Matrix

PO PO PO PO PO PO PO PO PO PO PO PO
SUBJECT
1 2 3 4 5 6 7 8 9 10 11 12

CO1 1 2 1 - - 1 - - - - - 1

CO2 1 - - - 2 - - - - - - 2

Engineering CO3 2 - 1 - - 1 - - - - - 2
Chemistry
CO4 2 2 - - - 1 2 - - - - 1

CO5 1 - - - 2 - - - - - - 2

CO6 1 - 1 - - 1 2 - - - - 1

Experiments – CO Mapping Matrix

SUBJECT Expt. No. CO1 CO2 CO3 CO4 CO5 CO6


1 √

2 √

3 √

4 √

5 √
Engineering 6 √
Chemistry
7 √

8 √

9 √

10 √

11 √

FE 2019 Pattern
Marathwada Mitramandal’s College of Engineering, Karvenagar, Pune - 52
First Year Engineering (2019 Pattern) Semester I / II Engineering Chemistry

Assessment Rubrics:
0 1 2 3 4 5

Attd Does not Performed as


Punctuality perform during per regular
regular schedule
schedule (2.5 - If late
reporting by 10
minutes or
more)

Preparation Does not Neither shows States the can only state Understands Understands
(2) perform during any objective very the objective objective but objective and
regular understanding vaguely but cannot place in can relate it to
schedule of the shows poor the context of an
objective nor understanding theory appropriate
can relate it to theory topic
theory

Participati Does not Does not Perform the Perform the Performs Performs
on in perform during participate in experiment only experiment experiment experiment on
Conductio regular experiment with the help only with the on his /her his /her own
n of Lab schedule from supervisor help own without without help
or others but the from help records records all the
work is untidy supervisor or all the readings
others but the readings, properly
work is neat untidy work

Post expt Does not Does not Completes Completes Completes Completes
completion / perform during complete the calculations / calculations / calculations / calculations /
Quiz/ regular calculations/ graph but graph and graph and graph and
certification schedule graph etc but incomplete write-up but write-up and write-up and
writes readings write-up does not partially answers FAQs
answer FAQ answers FAQs

FE 2019 Pattern
Marathwada Mitramandal’s College of Engineering, Karvenagar, Pune - 52
First Year Engineering (2019 Pattern) Semester I / II Engineering Chemistry

Experiment No: 1

Title:- Hardness of water

Date: __________ Signature of teacher: ________

1
Marathwada Mitramandal’s College of Engineering, Karvenagar, Pune - 52
First Year Engineering (2019 Pattern) Semester I / II Engineering Chemistry

Diagram:

Reactions:

Where M2+ = Ca or Mg from Hard water

2
Marathwada Mitramandal’s College of Engineering, Karvenagar, Pune - 52
First Year Engineering (2019 Pattern) Semester I / II Engineering Chemistry

Aim: Estimation of total hardness of given sample of water by


EDTA method.
Theory: Water sample which does not produce lather readily with soap is known as
‘hard water’. On heating, it leaves deposits of scales on the walls of the container. The
total hardness is due to the presence of dissolved bicarbonates, sulphate, chlorides and
nitrates of magnesium and calcium. The relation between the type of water sample and
degree of hardness can be given by the following table.

Hardness of water sample Hardness as ppm of CaCO3


Soft 0 - 75
Moderately Hard 75 - 150
Hard 150 - 300
Very Hard Above 300
The hardness which can be easily removed on heating is known as temporary hardness. It is due
to bicarbonates of calcium and magnesium which get decomposed on heating as insoluble
carbonates and hydroxides which can be removed by filtration.
Ca(HCO3)2 (on heating) → CaCO3↓ + H2O + CO2
Mg(HCO3)2 (on heating) → Mg(OH)2↓ + 2CO2↑
This hardness is also known as bicarbonate hardness. The hardness which cannot be removed
by heating is known as permanent hardness or noncarbonate hardness. The sum total of
temporary and permanent hardness is known as total hardness.
For determining suitability of water for domestic and industrial purposes, type of hardness and
hence magnitude of hardness is important. To determine total hardness of a given water sample,
disodium salt of ethylene diamine tetra acetic acid (EDTA) is used as it forms a strong 1:1
complex with divalent metal ions.
The EDTA forms a stable complex in the basic medium thus an alkaline buffer of NH4OH and
NH4Cl (pH 10) is used. In this complexometric titration Eriochrome black T (EBT) is used as
an indicator. This indicator forms a less stable wine red colored complex with metal ion (less
stable w.r.t. metal ion – EDTA complex) Which dissociates on titration with EDTA solution. On
dissociation a strong 1:1 metal ion – EDTA complex is formed and an indicator is set free
which gives its blue color to the solution .
Chemicals: - Ethylene Diamine Tetra-acetic acid (EDTA) 0.05M, buffer solution (pH = 10),
Eriochrome black T indicator (EBT) etc.
Apparatus: - Graduated Burette 25 ml, Glass beaker 100 ml, 250 ml, Volumetric flask 250 ml,
Conical Flask 100 ml, Glass measuring cylinder 100 ml

3
Marathwada Mitramandal’s College of Engineering, Karvenagar, Pune - 52
First Year Engineering (2019 Pattern) Semester I / II Engineering Chemistry

Procedure:
A) Total hardness of given water sample:-
1. Wash, rinse and fill burette -1 with standard EDTA solution.
2. Wash, rinse and fill burette -2 with a given hard water sample.
3. Take 10mL hard water sample from burette-2 into conical flask & add 10 mL buffer solution
& 2-3 drops of EBT solution into it. Color turns to wine red.
4. Titrate this solution against EDTA from burette -1 till color changes to blue. Note down this
burette reading as X1 mL.
5. Repeat the same procedure twice to obtain two readings as X2. X3, to find mean Xml.

Observations:

Burette 2: (LHS) Hard water solution

Burette 1: (RHS) Std. 0.01 M EDTA solution

Indicator: Eriochrome Black T

Buffer Solution: NH4Cl + NH4OH (pH 10)

End Point: Wine Red to Blue

Sr.
No. Readings Average

1 Burette 2 9 ml 10 ml 11 ml V = 10 ml

2 Burette 1 X1 = _____ ml X2 = ____ ml X3 = ____ ml X = _____ ml

Calculations:

1 mole EDTA = 1mole Ca2+ or 1mole Mg2+ = 1 mole CaCO3 equivalent


1ml 1 M EDTA≡ 100 mg CaCO3 equivalent

Part A:

Total Hardness = Volume of EDTA required x Molarity of EDTA x 100 x 1000


Volume of hard water
= X x 0.01 x 100 x 1000 = x 0.01 x 100 x 1000
V 10

= _____________ ppm or mg/lit

4
Marathwada Mitramandal’s College of Engineering, Karvenagar, Pune - 52
First Year Engineering (2019 Pattern) Semester I / II Engineering Chemistry

B) Permanent hardness of given water sample:


1. Take approx. 400 mL water in the beaker. Boil it for 20 min. Cool & filter it.
2. Transfer this water in 250 mL volumetric flask & dilute up to mark with distilled water.
Now we have to find out the hardness of this water.
3. Wash, rinse and fill burette -1 0.01M EDTA solution
4. Wash, rinse and fill burette -2 with boiled hard water sample
5. Take a 10 mL boiled hard water sample in a conical flask & add 10 mL buffer solution
& 2-3 drops of EBT solution into it. Color will turn to wine red.
6. Titrate this solution against EDTA from burette-1 till color changes to blue. Note down
reading as Y1 ml.
7. Repeat the same procedure for two more readings as Y2. Y3, to find mean Yml..
Observations:

Burette 2: (LHS) Boiled water solution

Burette 1: (RHS) Std. 0.01 M EDTA solution

Indicator: Eriochrome Black T

Buffer Solution: NH4Cl + NH4OH (pH 10)

End Point: Wine Red to Blue

Sr.
No. Readings Average

1 Burette 2 9 ml 10 ml 11 ml V = 10 ml

2 Burette 1 Y1 = _____ ml Y2 = ____ ml Y3 = ____ ml Y = _____ ml

Part B:
Permanent Hardness = Volume of EDTA required x Molarity of EDTA x 100 x 1000
Volume of hard water
= Y x 0.01 x 100 x 1000
V
= x 0.01 x 100 x 1000 = __________ppm or mg/lit
10
Part C:

Total hardness = Permanent hardness - Temporary hardness


Temporary hardness = Total Hardness - Permanent hardness

= =____________ ppm or mg/lit

5
Marathwada Mitramandal’s College of Engineering, Karvenagar, Pune - 52
First Year Engineering (2019 Pattern) Semester I / II Engineering Chemistry

Result:

1 Total Hardness of water __________ ppm


2 Permanent Hardness of water __________ ppm
3 Temporary Hardness of water __________ ppm

Questions:
1. Draw structure of Metal – EDTA Complex.
2. Define Hardness. Explain its types (Mention Reactions involved).
3. 50 ml water sample on titration with 0.01 M EDTA solution requires 10.5 ml for the end
point using buffer & EBT. Calculate hardness present in water per lit.?
4. 50 ml boiled water sample on titration with M/40 EDTA solution requires 9.7 ml for the
end point using buffer & EBT. Name the type & Calculate the hardness present in water
per lit.?
5. 100ml of water sample requires 18.7ml of M/50 disodium salt of EDTA for end point in
titration. 100ml same sample after boiling and filtration, takes 10.3ml of disodium
EDTA for end point. Calculate temporary and permanent hardness of water.

Answers:-

6
Marathwada Mitramandal’s College of Engineering, Karvenagar, Pune - 52
First Year Engineering (2019 Pattern) Semester I / II Engineering Chemistry

7
Marathwada Mitramandal’s College of Engineering, Karvenagar, Pune - 52
First Year Engineering (2019 Pattern) Semester I / II Engineering Chemistry

8
Marathwada Mitramandal’s College of Engineering, Karvenagar, Pune - 52
First Year Engineering (2019 Pattern) Semester I / II Engineering Chemistry

9
Marathwada Mitramandal’s College of Engineering, Karvenagar, Pune - 52
First Year Engineering (2019 Pattern) Semester I / II Engineering Chemistry

10
Marathwada Mitramandal’s College of Engineering, Karvenagar, Pune - 52
First Year Engineering (2019 Pattern) Semester I / II Engineering Chemistry

Experiment No: 2

Title :- Alkalinity of water

Date: __________ Signature of teacher: ________

11
Marathwada Mitramandal’s College of Engineering, Karvenagar, Pune - 52
First Year Engineering (2019 Pattern) Semester I / II Engineering Chemistry

Diagram:
Reactions:

P = Phenolphthalein
M = Methyl Orange

Standard reference table:

Types of alkalinities present in water samples-

Sr. Relation Relation Between Hydroxide Carbonate Bicarbonate


No. Between x & y P&M (OH-) in ppm (CO32--) in ppm (HCO3-) in
ppm

1 x=0 P=0 0 0 M
2 x=y P=M M 0 0
3 x=½y P=½M 0 2P 0
4 x>½y P>½M (2P - M) 2(M-P) 0
5 x<½y P<½M 0 2P (M-2P)

12
Marathwada Mitramandal’s College of Engineering, Karvenagar, Pune - 52
First Year Engineering (2019 Pattern) Semester I / II Engineering Chemistry

Aim: Determination of alkalinity of a given alkaline water sample.


Theory: Pure water is neutral. Its pH is exactly seven. But because of dissociation or
hydrolysis of different minerals present in water, it becomes alkaline. Alkalinity of water means
total content of OH-, HCO3-, CO32- in water.
In boilers for steam generation, water having high alkalinity leads to caustic
embrittlement, precipitation of sludges and deposition of scales. So it is essential to remove
them before taking this water in the boiler. To remove alkalinity of water, first it should be
measured. These alkalinities can be estimated volumetrically by titrating water samples against
standard acid using methyl orange and phenolphthalein indicators.
Chemicals: 0.02 N HCl, Alkaline water Sample – I, II, III, Phenolphthalein & Methyl Orange
Indicator
Procedure:
1. Take 10 ml of given water sample 1 (WS I) in a conical flask, titrate it against 0.02 N
HCl using phenolphthalein as an indicator, till pink color just vanishes. Let this reading
be x ml. This end point is called Phenolphthalein end point.
2. To the same solution, add 1 to 2 drops of methyl orange as indicator and continue the
titration till light yellow color change to orange. Let this reading be y ml. This is called
the Methyl Orange end point.
This procedure is repeated for different samples of water as WS II & WS III.
Observations:
Burette: 0.02 N HCl

Conical Flask: Water sample I / II / III


Indicator: 1) Phenolphthalein in the beginning
2) Methyl orange to the same solution after getting the first end point.

End Point: 1) Pink to colorless, 2) Yellow to orange

Calculations: Similar to hardness, chloride content etc., alkalinity is also expressed as parts
per million in terms of CaCO3. equivalents.
1000 ml 1 N HCl corresponds to 50 g of CaCO3 eq.
So V ml 0.02 N HC1 = V x 0.02 x 50 g. CaCO3 eq.
1000 x 1
3
= V x 0.02 x50 x 10 mg. CaCO3 eq. = V mg of CaCO3eq
1000 x 1
Since 10 ml water sample, 1000 ml water sample = 100 x ppm alkalinity

Hence, Phenolphthalein alkalinity ‘P’ = 100 x ppm


& Methyl orange alkalinity ‘M’ = 100 y ppm

13
Marathwada Mitramandal’s College of Engineering, Karvenagar, Pune - 52
First Year Engineering (2019 Pattern) Semester I / II Engineering Chemistry

Observation table: (Mention formulae and answer)

Water x ml y ml Relation P M Relation OH- CO32- HCO3-


Sample between between (Mention (Mention (Mention
x&y P&M formulae) formulae) formulae)

Water
Sample
-I

Water
Sample
- II

Water
Sample
- III

Result:
Water Sample OH- CO32- HCO3-
(Mention only answer) (Mention only answer) (Mention only answer)

Water Sample - I

Water Sample - II

Water Sample - III

Questions:
1. What is alkalinity? State the type of alkalinities.
2. Which type of alkalinities is not possible practically? Why?
3. 50 ml of an alkaline water sample requires 9.2ml of 0.02N HCl up to
phenolphthalein end point & total 13.1ml of the acid for complete neutralization.
Find the types & amounts of alkalinities.
4. A water sample was alkaline to both P.P. and M.O. 50 ml of water sample
required 10 ml N/50 H2SO4 for P.P. end point & another 15ml for complete
neutralization. Calculate type & amount of alkalinity.
5. A water sample is not alkaline to P.P. However, 100 ml of sample on titration
with N/40 HCl, required 16.9 ml to obtain the end point using M.O. as an
indicator. What are the types and amount of alkalinities present in the sample?

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Answers:-

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Experiment No: 3

Title :- Conductometry

Date: __________ Signature of teacher: ________

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Diagram:

Reaction:

Graph:

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Aim: To investigate the conductometric titration of


Strong acid against Strong base.
Theory:
When NaOH solution is added to HCl solution H+ ion in solution is replaced by
Na+ ion. The mobility or ion conductance of H+ ion is more than mobility or ion
conductance of Na+ ion. A high mobile cation is replaced by a less mobile cation and
conductance of the solution decreases. This decrease in conductance takes place with
every addition of NaOH solution till HCl solution or H+ ions are present in the solution.
HCl + NaOH Cl- + Na+ + H2O
When the neutralization is complete, that is all the H+ ions are replaced by Na+ ions,
further addition of NaOH increases conductance due to presence of excess OH - ions. If a
graph of volume of NaOH added against conductance is plotted, we get two straight
lines in V shape intersecting at equivalence point.
Apparatus: Conductometer, Conductivity cell, magnetic stirrer, etc.

Chemicals: Standard 0.02N NaOH, Approx. 0.02N HCl, KCl, Burette, glass rod

Procedure:-

1. Take 10 ml of 0.02N HCl in a small beaker, add about 20ml of conductivity water.
2. Dip a conductivity cell into the solution and ensure that the electrodes of the cell are
completely immersed into the solution. Put a magnetic needle into it and place the
electrode assembly on a magnetic stirrer. Stir the solution well.
3. Connect the electrodes to the conductivity bridge and measure conductance of 0.02N
HCl solution.
4. From the burette, add 0.5ml of 0.02 N NaOH into the HCl solution and stir the
solution. Measure the conductance of the solution.
5. In a similar way, add 0.5ml of 0.02N NaOH solution each time and every time
measure the conductance. Take conductance readings till the equivalence point
exceeds.
6. Plot a graph of conductance against ml of 0.02N NaOH added. From the graph find
neutralization point and hence find exact normality of HCl solution.

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Observation table:
Sr. ml of NaOH added Conductance of Sr. ml of NaOH added Conductance of
No. from burette solution No. from burette Solution
1 27

2 28

3 29

4 30

5 31

6 32

7 33

8 34

9 35

10 36

11 37

12 38

13 39

14 40

15 41

16 42

17 43

18 44

19 45

20 46

21 47

22 48

23 49

24 50

25 51

26 52

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Calculations:
(I) Exact Normality of of HCl solution: HCl ☰ NaOH
N1 V1 ☰ N2 V2
As N2 = 0.02 N, V1 = 25 ml, V2 = Consider this value from graph _______ml
∴ N1 =

∴ Normality of HCl = _________ N

(II) Strength of HCl = Normality of HCl x Equivalent weight of HCl


= x 36.5

∴ Strength of HCl = _________ g/lit

Result:
(I) Normality of HCl ___________ N
(II) Strength of HCl ___________ g/lit

Questions:
1. Define the following terms & also Give their units (a) Specific conductance, (b) Cell
constant, (c) Equivalent conductance, (d) Molar conductance.
2. Explain conductometric titration curve of Weak Acid – Weak Base
3. Explain construction of conductivity cell with labeled diagram.
4. Explain the conductometric titration curve of Strong Acid – Weak base titration with
suitable examples.

Answers:

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Experiment No: 4

Title :- pH metry

Date: __________ Signature of teacher: ________

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Diagram:

Reaction:

Graph:

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Aim: To determine strength of strong acid HCl using pH metric


titration against strong base NaOH solution.
Theory: When a standard NaOH solution is added to HCl solution, H+ ions in solution are
replaced by Na+ ions.
Thus, as the concentration of H+ ions goes on decreasing with addition of Na+ ions and pH of
the solution goes on increasing steadily. This increase in pH occurs with every addition of
NaOH till all the H+ ions in solution are consumed.

HCl + NaOH → NaCl + H2O


When neutralization is complete there is sudden increase in pH from acidic to alkaline.
The graph of pH from acidic to alkaline. The graph of pH Vs ml of NaOH added is ‘S’ shaped.
After complete neutralization, the pH remains constant with every addition of NaOH.
1 ml 1 N NaOH = 36.5 mg of HCl
Apparatus: pH meter, glass electrode, burette, beakers , magnetic stirrer, measuring cylinder
Chemicals: 0.02N NaOH solution, buffer tablet, HCl solution, distilled water

Procedure: Part I: Calibration of pH meter


1. Prepare the standard pH solution by dissolving the buffer tablet or powder in 100 ml
distilled water.
2. Rinse the combined electrode with distilled water.
3. Make the electrical connections and immerse the electrode in the standard pH solution.
4. Keep the temperature knob on 200C and adjust the pH on display equal to std. pH by
standardizing the knob. Bring the temperature knob at room temperature.
Do not disturb the adjusted knobs throughout the experiment.
Part II: Determination of pH of given acid solution:
1. Fill the burette with 0.1 N NaOH solution.
2. Pipette out 25 ml of the HCl solution in a clean 100 ml beaker and dip the washed
combined electrode in it.
3. Read the pH at 0 ml burette solution added stage.
4. Add 1 ml burette solution in the beaker; stir using a magnetic stirrer, read the pH.
5. Similarly read the pH of titration mixture at 2, 3, 4, 5 …. ml burette solution added
stages.
6. See that at least 5 -7 readings are obtained after the pH changed suddenly.
7. Plot the graph of pH versus ml of the base solution added from burette.

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Observation table:
Sr. ml of NaOH added Conductance of Sr. ml of NaOH added Conductance of
No. from burette solution No. from burette Solution
1 27

2 28

3 29

4 30

5 31

6 32

7 33

8 34

9 35

10 36

11 37

12 38

13 39

14 40

15 41

16 42

17 43

18 44

19 45

20 46

21 47

22 48

23 49

24 50

25 51

26 52

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Calculations:
(I) Exact Normality of of HCl solution: HCl ☰ NaOH
N1 V1 ☰ N2 V2
As N2 = 0.02 N, V1 = 25 ml, V2 = Consider this value from graph _______ml
∴ N1 =

∴ Normality of HCl = _________ N

(II) Strength of HCl = Normality of HCl x Equivalent weight of HCl


= x 36.5

∴ Strength of HCl = _________ g/lit

Result:
(I) Normality of HCl ___________ N
(II) Strength of HCl ___________ g/lit

Questions:
1. What is meant by ‘Buffer solution’? Explain its types with examples.
2. Draw labeled diagrams of all Ion Selective Electrodes.
3. Explain briefly pH metric titration of mixture of & HCl Vs. NaOH.
(Give reaction, explanation, titration curve, calculation also).
4. Define reference electrode. Draw a labeled diagram of a calomel electrode and give its
representation.
5. Explain the construction of a glass electrode with a labeled diagram and its
representation.

Answers:

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Experiment No: 5

Title :- Preparation of
polymer

Date: __________ Signature of teacher: ________

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Diagram:

Reaction:
(a) Urea Formaldehyde Reaction:

(b) Phenol Formaldehyde Reaction:

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Aim: Preparation of Polymer i.e. Urea Formaldehyde Resin/Phenol


Formaldehyde Resin by Condensation Polymerization
(a) Urea Formaldehyde Resin –
Theory: Urea Formaldehyde is condensation polymer obtained by reaction between
Urea & Formaldehyde which gives rise to a network structure. The reaction can be
summarized as ‘Urea Formaldehyde is a thermosetting type of Resin’
Procedure:
1. Weigh the given a beaker & add 10ml of 40% Formaldehyde solution in it.
2. Add about 5gm of urea while stirring a saturated solution is obtained.
3. Add a few drops of conc.H2SO4 stirring continuously during the addition.
4. A voluminous white solid mass appears in the beaker. When the reaction is
completed, weigh the product & wash the residue with water.
Properties:
1. Formed by condensation polymerization.
2. Higher molecular weight.
3. Hard, strong, brittle % cannot be reclaimed from waste.
Uses:
1. It is used in packaging, accessories, unbreakable dishes, water tumblers, etc
2. It is used as sizing agent & textile finishing resins.
3. It is also used in the paper industry to improve wet strength of paper.

(b) Phenol Formaldehyde Resin –


Theory: Phenol formaldehyde resins are the most important and extensively used synthetic
plastics and perhaps the oldest synthetic plastics. In these resins one of the monomers is always
a phenol molecule. One of the most important members of this class is phenol formaldehyde
resin. This reaction is catalyzed by alkalies and acids. The nature of the product depends on
several factors, the major one being the nature of the catalyst and the proportion of the
reactants.
Procedure:
1. Take 5 ml gl. Acetic acid and 2.5 ml 40% formaldehyde solution in a 500 ml beaker.
2. Add 2 g phenol to it.
3. Then add a few ml of conc.HCl into the mixture carefully and heat it slightly.
4. Pink colored plastic is formed.
Properties:
1. Phenol formaldehyde molding resins have excellent heat resistance.
2. These have high dimensional stability & good dielectric properties.
3. They are however attacked by alkalies, because of free hydroxyl groups.
4. They are hard, rigid and scratch resistant

Uses:
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1. Phenolic resins mainly used in moulding applications. They are used in making
telephone parts, cabinets for radio, television and automobile parts.
2. Due to their adhesive properties and bonding strength, they are used for
producing brake linings, abrasive wheels and sand paper.
3. They are used for making electric insulator parts like switches, plugs, switch
boards, heater-handles etc.
Questions:
1. What are biodegradable polymers? Give important features of biodegradable
polymers. Give the structure of PHB & PHV.
2. What are Electroluminescent polymers? Give applications of electroluminescent
polymers. Explain construction and working of basic polymer LED based on
polyphenylene vinylene (PPV).
3. What are polymer composites? What are the constituents of polymer composite?
Give the types of polymer matrix and state important functions of matrix.

Answers:

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Experiment No: 6

Title :- Proximate Analysis

Date: __________ Signature of teacher: ________

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Diagram:
Crucible with lid -

Oven – Muffle furnace –

Desiccator -

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Aim: Estimation of moisture, volatile matter and ash content in the


given sample of coal by Proximate Analysis method.

Theory: In order to ascertain the quality of coal, proximate and ultimate analysis of
coal is done. Proximate analysis is determination of moisture content, volatile matter,
ash content and fixed carbon content. This gives information about the practical utility
of coal.
Moisture content is the loss in weight of coal when heated in crucible at
0
110 C for one hour. During burning of coal, moisture evaporates and is removed as
steam. Some amount of heat is required for this, which is taken during the burning of
fuel. Calorific value of fuel is reduced due to presence of moisture in fuel.
Volatile matter results from the thermal decomposition of the coal material.
Volatile matter is the percentage loss in weight of coal when it is heated in absence of
air for exactly 7 minutes at 950 ± 200C, in a crucible of standard dimensions. The coal
with high volatile matter is not suitable for production of steam as it burns with long
smoky flame. This type of coal is suitable for production of coal gas. The furnace
design depends upon the volatile matter. Caking quality of coal varies with its volatile
matter.
Ash content of coal is the weight of residue left after burning known
quantity of dry coal in open crucible at 7000 C in a muffle furnace. Ash reduces the
heating value of coal.

Procedure:-

Part A: - Determination of Moisture Content


1) Take 1 g powdered coal sample in a previously weighted silica crucible.
2) Heat the sample in a hot air oven at about 110oC for 1 hour.
3) Take out the crucible, cool in the desiccator and weigh it. Note down the weight.
Part B: - Determination of Volatile Matter (V.M.) Content
1) Take the above coal sample with the crucible and heat the crucible in a muffle
furnace at 925oC for 7 minutes.
2) Take out the crucible, Cool in desiccator and weigh it. Note down the weight.
Part C: - Determination of Ash Content
1) Take the above coal sample in crucible and burn the coal in crucible in an oven at
700oC for 30 minutes.
2) Take out the crucible, Cool in desiccator and weigh it. Note down the weight.

Part D: - Determination of Fixed Carbon (F.C.) Content


It is found by using the formula, F.C. = 100 – (moisture % + V.M. % + ash % )
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Observation Table:

Sr. Description Value


No.
1 Weight of Empty Crucible A gm

2 Weight of crucible & Coal before heating at 110 B gm


°C for 1 hr.

3 Weight of coal Z gm (B – A)

4 Weight of crucible + Coal (after heating at 110 C gm


°C)

5 Loss in weight (Due to removal of moisture) B - C gm

6 Wt of Crucible and Coal (Before heating at C gm


925°C for 7 min)

7 Wt of Crucible and Coal (After heating at 925 D gm


°C)

8 Loss in Wt (Due to Removal of Volatile matter) C - D gm

9 Wt of crucible & ash (after heating at 750 °C for E gm


30 min)

10 Weight Of Ash E - A gm

Calculations:
1) % Moisture = Loss in weight x 100 = (B - C) x 100 =
Weight of coal Z

2) % Volatile Matter = Loss in weight x 100 = (C - D) x 100


Weight of coal Z

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3) % Ash = Weight of ash x 100 = (E - A) x 100


Weight of coal Z

Result:

Sr. No. Description %


1 Moisture

2 Volatile Matter

3 Ash Content

4 Fixed Carbon =
100 – (% Moisture + % Volatile Matter + % Ash Content)

Questions:

1. Write Significance of Proximate Analysis.


2. A sample of coal was analyzed as follows: Exactly 2.5gm was weighed into a silica
crucible. After heating for one hour at 1100C, the residue weighed, 2.415gm. The crucible
next was covered with a vented lid and strongly heated for exactly 7 min. at 950 +200C.
The residue weighed 1.528 gm. The crucible was then heated without the cover, until a
constant weight was obtained. The last residue was found to be 0.245gm. Calculate the
percentage result of above analysis.
3. Calculate % C, H, N, S and O from the following observation for a sample of coal.
(i) 2.05gm of the coal is burnt in combustion tube. The increase in weight of anhydrous
CaCl2 is 0.55gm and increase in weight of KOH tube is 5.75gm.
(ii) 0.75gm of coal in Kjeldahl’s experiment released NH3, which is passed in 50ml 0.12
N HCl. the HCl requires 41 ml of 0.12 N NaOH to neutralize, in back titration.
(iii) Washing of bomb pot, when 1.8 gm of coal sample in bomb calorimeter experiment,
is treated with BaCl2 solution to give 0.31gm BaSO4.

Answers:

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Experiment No: 7

Title :- Colorimetry

Date: __________ Signature of teacher: ________

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Diagram:

Graph:
Determination of Unknown Concentration (Absorbance Vs. Concentration)

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Aim: Study of Beer-Lambert’s law and its application to spectrophotometric


analysis. Determine an unknown concentration of copper sulphate.
Theory: Colorimetry deals with measurement of color intensity. The color of the substance is due
to absorbance of light waves of certain wavelengths. If the solution does not absorb light, it is
transparent and colorless. The absorption of light by solution results in excitation of electrons in
its molecules.
The advantage of colorimetric analysis is that it requires much less sample and it is more
accurate than chemical analysis. Colorimetry is used to determine only low concentration,
usually less than 2%.
(I) Fundamental Laws of Colorimetry :
When light (monochromatic or polychromatic) is incident upon a homogeneous
medium, a part of the radiant power of the incident light (Po) is reflected (Pr), a part is
absorbed by the medium(Pa) and the remainder is transmitted(Pt).
Po = Pr + Pa + Pt
Po = Radiant power of incident, light Pr = Radiant power of reflected light
Pa = Radiant power of absorbed light, Pt = Radiant power of transmitted light
If a comparison cell or the same cell is used during analysis, the value of Pr, which is very
small (= 4%) can be eliminated for air-glass interfaces. Under this condition, the above relation
becomes, Po = Pa + Pt
(II) Lambert’s Law : This law can be stated as follows :
When a beam of monochromatic light is allowed to pass through a transparent medium,
the rate of decrease of radiant power with the thickness of the medium is directly proportional
to the thickness of medium or the path length.
(III) Beer - Lambert’s Law : The Lambert’s law states that
Absorbance = Constant X thickness of the medium
The Beer’s law states that
Absorbance = constant X (thickness of the medium) X (concentration of the
medium) i.e. A = constant X b X C
Thus, Beer-Lambert’s law can be defined as :
When a beam of monochromatic light is allowed to pass through a transparent medium,
the absorption of the medium is directly proportional to the thickness and concentration of the
medium (A α b C).
When the concentration is expressed in g/lit and thickness in cm, the constant in the
above equation is called as molar absorptivity and represented by the symbol ‘ ε ‘
Thus, A = εbC, when b = 1cm and C = 1 mol/litre
The molar absorptivity is the absorbance of a solution measured in a cell of one cm
thickness and with concentration of one mole per litre. It is a constant independent of
concentration, length of path and radiant power of incident light.
Now, for the given thickness of the medium and system, the relation A = ε b C takes the

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form A = constant x C or A α C and therefore, Beer-Lambert’s law can also be stated as For the
given system and the thickness of the medium, the absorbance of the solution is directly
proportional to the concentration of an absorbing species.
Apparatus: Colorimeter, measuring cylinder, cuvette.
Chemicals: 0.01 M CuSO4 stock solutions, liquor ammonia, distilled water.
Procedure: To find out the Absorbance and %T for the known and the unknown
solution: (Using Digital colorimeter)
1. Insert the filter having λmax in the proper place. If the inbuilt filter system is there, then
adjust the λmax filter in the light path with the help of a filter knob.
2. Rinse the cuvette with a ref solution & fill it with the same solution up to the mark.
3. The instrument is made on. On the display it shows reading. With the help of zero
adjustment knob it is adjusted to read zero optical density. Then this zero adjustment
knob is kept undisturbed throughout the experiment. Now the reference solution is
removed. The cuvette is washed with distilled water and rinsed with the 0.006 M
solution. Then it is filled up to the mark with 0.006M solution. Make the same
procedure for remaining solutions as well as unknown. Report the observations in the
observation table.
Observation Table:

Flask Concentration in moles/lit. Absorbance


No.

1 0.006

2 0.005

3 0.004

4 0.003

5 0.002

6 0.001

7 Unknown

Result:
The concentration of the unknown solution (from graph ii) = ___________ moles/lit.
Questions:
1. State the following with equations - Lambert-Beer’s law, Lambert’s Law, Beer’s Law.
2. Give the principle of UV-Visible spectroscopy. Explain different types of electronic
transitions that occur in an organic molecule after absorbing UV radiations.
3. Define – (a) Auxochrome, (b) Chromophore, (c) Bathochromic shift,
(d) Hypsochromic shift, (e) Hyperchromic shift, (f) Hypochromic shift

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Answers:

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Experiment No: 8

Title :- Electroplating

Date: __________ Signature of teacher: ________

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Diagram:

Reaction:

At Anode (Oxidation) - Zn(s) → Zn2+ + 2e−

At Cathode (Reduction) - Zn2+ + 2e− → Zn(s)

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First Year Engineering (2019 Pattern) Semester I / II Engineering Chemistry

Aim: To study Electroplating.


Theory: Electroplating is a process in which coating metal is deposited by passing a
direct current through an electrolytic solution containing the soluble salt of coating metal on
the metallic substrate. In this process generally an article to be plated is made cathode and
anode is made up of material which is to be deposited.
For uniform plating, the article to be plated must be free from impurities. Therefore,
to get a clean article it’s surface is pretreated with acid (pickling).
Apparatus: Beaker, copper wires, DC source
Chemicals: H2SO4 , HNO3 , Zinc rod, Copper plate, Iron plates
Procedure: Zinc coating on copper plate
1. First zinc sulphate is dissolved in distilled water (10% solution).
2. Clean the surface of Zn rod and copper plate. First dip in 2M HNO3 and wash with water.
Then clean with polish paper again wash with distilled water and dry it.
3. Connect the +ve terminal of the battery to zinc plate and copper with anode.
4. Attach the copper plate to be coated to hook by copper wire and connect the wire to – ve
terminal of the battery (cathode).
5. Immerse the zinc plate partially in solution and also place the copper plate to be coated
completely in solution.
6. Apply the potential across terminals by using power supply.
7. After 10 min. switch off power supply & carefully take out the copper plate, wash with
water and dry it.
Questions:
1. What is electroplating of metal? Explain electroplating process with neat labeled
diagram, reactions and applications.
2. Explain briefly – (i) Metal Cladding & (ii) Cementation.
3. What is anodic and cathodic coating? Which is more protective and why?
4. Distinguish between Galvanizing & tinning.
5. Explain Anodic Protection with a suitable diagram.
Answers:

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Marathwada Mitramandal’s College of Engineering, Karvenagar, Pune - 52
First Year Engineering (2019 Pattern) Semester I / II Engineering Chemistry

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Marathwada Mitramandal’s College of Engineering, Karvenagar, Pune - 52
First Year Engineering (2019 Pattern) Semester I / II Engineering Chemistry

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Marathwada Mitramandal’s College of Engineering, Karvenagar, Pune - 52
First Year Engineering (2019 Pattern) Semester I / II Engineering Chemistry

Experiment No: 9

Title :- Electroless Plating


(Content Beyond Syllabus)

Date: __________ Signature of teacher: ________

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Diagram:

Sr. No. Components Role

1 Metallic ions Source of metal to be deposited

2 Reducing agent Source of Electrons co-deposited metal

3 Complexing agent Complexes the metallic ions to


● increase the metallic ions solubility
● increase the stability by avoiding precipitation
But decreases the deposition current

4 Stabilizer Regulate deposition speed by blocking a part of the catalytic sites

5 pH adjuster Regulates pH

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Marathwada Mitramandal’s College of Engineering, Karvenagar, Pune - 52
First Year Engineering (2019 Pattern) Semester I / II Engineering Chemistry

Aim: To study Electroless Plating


Theory:
Electroless plating is a chemical process used for depositing an anode metal (from its
solution) on a catalytically active surface of less noble metal by suitable reducing agent without
application of current (electrical energy).

Apparatus: Beaker, Glass rod, Glass dropper

Chemicals: H2SO4, CuSO4, HNO3, Iron plate

Procedure: Copper plating on Iron plate


1. In the first step, dissolve copper sulphate in distilled water and add a few drops of H2SO4.

2. An electrolytic solution is taken in the beaker.


3. Clean the surface of the iron plate to be coated by dipping it first in 2M nitric acid and
then wash it with distilled water. Polish the iron plate and then dry it.
4. After cleaning, dip the iron plate in electrolyte for 5 min. Iron plate must be completely
dipped in electrolyte.
5. Finally, take out an iron plate from an electrolytic solution.
6. Wash the article with water and dry it to observe good coating of copper on the iron plate.

Advantages:
1. No Electrical power is required
2. Insulators & semiconductors can also be plated
3. Better throwing power as compared to electroplating so objects of complex shapes can
be plated
4. More compact & highly adherent deposits

Applications:
1. Electro less Ni plating (Applications include oil field valves, rotors, drive shafts, paper
handling equipment, fuel rails, optical surfaces for diamond turning, door knobs, kitchen
utensils, bathroom fixtures, electrical/mechanical tools and office equipment)
2. Used in jewelry, shock absorbers
5. Gears, cylinders in automobiles
6. Used in making PCB’s

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First Year Engineering (2019 Pattern) Semester I / II Engineering Chemistry

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First Year Engineering (2019 Pattern) Semester I / II Engineering Chemistry

Experiment No: 10

Title :- Estimation of Phosphate


Content in Soft Drinks
(V - Lab)

Date: __________ Signature of teacher: ________

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First Year Engineering (2019 Pattern) Semester I / II Engineering Chemistry

Diagram:

Simplified diagram of a colorimeter

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First Year Engineering (2019 Pattern) Semester I / II Engineering Chemistry

Aim: To determine the amount of phosphate in soft drinks.


Theory: Soft drinks are complex mixtures containing a variety of substances such as coloring
compounds, flavoring agents, acidifiers, sweeteners, preservatives, and caffeine. The most
common acidifier used in soft drinks is phosphoric which gives a tangy taste in the mouth.
Phosphoric acid can also acts as a preservative, keeping the contents of the bottle fresh.
Health Effects of Phosphate in Soft Drinks:
Cola linked to brittle bones risk: “Drinking cola could lead to weaker bones”, experts
have said. A US study found that drinking just four cans of regular or diet cola a week led to
lower bone density in women - a condition which increases the risk of osteoporosis. Soft drinks
have long been suspected of leading to lower calcium levels and higher phosphate levels in the
blood. When phosphate levels are high and calcium levels are low, calcium is pulled out of the
bones. The phosphate content of soft drinks is very high, and they contain virtually no calcium.
Phosphoric acid contained in some soft drinks displaces calcium from the bones, lowering bone
density of the skeleton and leading to weakened bones.
Dental Decay: The pH of a soft drink ranges from 2.47-3.35. The PH in our mouth is
normally about 6.2 to 7.0 slightly more acidic than water. At a pH of 5.2 to 5.5 or below the
acid begins to dissolve the hard enamel of our teeth. Because good health depends upon our
bodies being able to maintain a one-to-one balance between calcium and phosphorus in our
systems, calcium is released from our teeth eventually the phosphoric acid is excreted, taking
with it the released calcium. Thus, a habit of soft drink consumption actually robs our bodies of
calcium, leading to soft teeth.
Stomach Problems: When you open the bottle of a soft drink, bubbles and fizz are
immediately emitted out. This is due to phosphoric acid and carbon dioxide (CO2) content,
which make these drinks highly acidic. The pH of soft drink ranges from 2.5-3.4 which
generates a highly acidic environment in the stomach. The phosphoric acid present in soft drink
reacts with the hydrochloric acid of the stomach and affects its functions. When the stomach
becomes ineffective, food remains undigested causing indigestion, gassiness or bloating
(swelling of stomach).
Effect on Kidneys: The amount of phosphoric acid is excess the kidneys are less able to
excrete. Thus, there is an extra work for kidney. Soft drinks remove Calcium from the body,
and deposited in kidney, resulting in kidney stones.
Other major side effects are: Researches show that phosphate, which gives many soft drinks
their tangy taste, can accelerate ageing. A low calcium-to-phosphorus ratio in the diet increases
the incidence of hypertension and the risk of colon-rectal cancer.

Principle: Colourimetric analysis for determining the amount of an inorganic compound in


solution involves a reaction between an organic reagent and an analyte to form a coloured
complex. The reaction can be used to determine analyte concentrations assuming the colour
intensity and absorbance is proportional to the analyte concentration.
Phosphate ion (PO43-) reacts with molybedic acid (H2MoO4) to form phosphomolybdate, a

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complex ion [PMo12O40]3-. The phosphomolybdate on reduction forms another complex, called
molybdenum blue which can be monitored colourimetrically.
Principle of Colorimetry: A colorimeter can be used to measure any test substance that is
itself colored or can be reacted to produce a color. It is a device consisting of,
1) A light source, 2) Some optics for focusing the light, 3) A colored filter, which passes
light of the color which is absorbed by the treated sample, 4) A sample compartment to hold a
transparent tube or cell containing the sample and 5) A light-sensitive detector.
Beer-Lambert Law: The Beer-Lambert Law relates the absorption of light at a particular
wavelength to the concentration of the substance that is absorbing the light as
A = εbC
Where, A is the absorption at a particular wavelength
ε is the molar absorption coefficient for the compound at the wavelength at which the
absorption is measured and is characteristic for the compound. This constant is a measure of
how strongly a compound absorbs at a particular wavelength.
c is the concentration of the compound and is independent of wavelength.
b is the path length of the test tube used to hold the sample.
To estimate the amount of phosphate in soft drink sample, one first constructs a graph from
stock solutions of phosphate. The absorbance associated with a set of phosphate solutions of
known concentrations is called a phosphate standard curve. The amount of phosphate in
sample solution can be determined from the standard curve by drawing a horizontal line on the
graph parallel to the X-axis which corresponds to the absorbance of soft drink sample. This line
will intersect the standard curve; at this intersection, a vertical line is drawn to the X-axis. This
point corresponds to the volume of phosphate in sample solution.
Procedure: Preparation of Solutions: Molybdate Solution:
Add 13.6 mL of con.H2SO4 to 35 mL of water and allow the solution to cool. In a separate
vessel add 2.5 g of ammonium molybdate to 50 mL of water. Add sulphuric acid solution to it
& make up the volume.
Reducing Solution:
Dissolve 11.25 g sodium hydrogen phosphate in 30 mL water. Add 2.25 g sodium sulphate and
0.19 g 1-amino 2-naphthol 4-sulphonic acid and dilute the mixture to 75 mL with water. Stir the
mixture thoroughly & filter.
Standard Solutions of Phosphate:
Dissolve 20 mg of potassium dihydrogen phosphate in 100 mL of water. The concentration of
phosphate standard solution is 0.2 mg/mL.
Prepare 9 standard solutions containing 0.5 mL molybdate solution, 0.2 mL reducing
solution & x mL of phosphate stock solution + y mL of distilled water. Where, x+y =9.3 mL
and x= 2-0.2n, n = 1,2,…………9.
Also prepare a blank solution by mixing 0.5 ml of molybdate solution, 0.2 ml of reducing
solution and 9.3 mL of water.
Set the wave length to 635nm and adjust the colorimeter reading to 0 with the blank.
Place each standard solution of phosphate in turn in the curette and record the absorbance.

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Dilute the soft drink sample 5 times. Mix 1mL of this diluted solution with 0.5 mL
molybdate, 0.2 mL reducing solution and 8.3 mL water, so as to get the test solution.
Measure the absorbance of the sample solutions.
Plot a graph between absorbance and volume of phosphate in various standard solutions and
obtain the calibrated curve.
From the curve determine the amount of phosphate in the test solution.
The amount of phosphate in the sample of soft drink is -
5 x 0.2 x V = 1 x V mg /mL.
where, 5 is the dilution factor.
0.2 mg/mL amount of phosphate in standard solution.
V is the volume of phosphate solution obtained from graph.
Questions:
1. Which statements about the absorbance of a compound in a colorimeter is correct?
a) The absorbance will double if the concentration of the colored compound is doubled.
b) The absorbance will double if the concentration of the colored compound is halved.
c) The absorbance does not depend on the concentration of the colored compound.
d) The absorbance is highest for light of the same colour as that of the solution.
2. Why is it generally preferable to use absorbance as a measure of absorption rather than
% Transmittance?
a) Because %T cannot be measured as accurately as absorbance
b) Because %T is dependant on the power of the incident radiation
c) Because absorbance is proportional to the conc of the analyte, whereas %T is not.
3. The blank for a colorimeter should be composed of
a) Water b) Empty cuvette c) Test solution
d) Everything except the compound of interest which absorbs light
4. Using a standard curve, if you know the absorbance of an unknown sample, what else
can be determined about the unknown?
a) The wave length of the maximum absorbance c) The identity of the sample
b) The molecular weight of the sample d) The concentration of the sample

Books: Instrumental methods of analysis by Willard.

Webliography:
1. http://www.just-drinks.com/news/cola-linked-to-brittle-bones-in-women_id87994.aspx
2. http://www.dentalgentlecare.com/diet_soda.htm
http://www.ehow.com/list_6162284_effects-soft-drinks-stomach.html#ixzz1b7ZayBa0

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First Year Engineering (2019 Pattern) Semester I / II Engineering Chemistry

Experiment No: 11

Title :- Soil analysis – Kjeldahl’s


Method (V - Lab)

Date: __________ Signature of teacher: ________

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Diagram:

Nitrogen cycle

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Aim: To determine the available nitrogen in the soil sample by Kjeldahl’s method.
Theory: A soil analysis is a process by which elements such as P, K, Ca, Mg, Na, S, Mn, Cu
and Zn are chemically extracted from the soil and measured for their “plant available” content
within the soil sample.
Significance of Soil Analysis:
It increases the knowledge of what nutrients are especially available in our soil.
It reduces the environmental impacts due to soil amendments.
It increases the efficiency of resource inputs such as fertilisers and water.
It helps to predict the nutritional values needed for crop production.
It helps to evaluate the fertility status of soils of a country or a state or a district.
Procedure for Taking Good Soil Samples:
Determine the soil unit (or plot).
Make a traverse over the soil unit (or plot).
Clean the site (with spade) from where soil sample is to be collected.
Insert the spade into soil.
Standing on the opposite side, again insert the spade into soil.
A lump of soil is removed.
A pit of ‘V’ shape is formed. Its depth should be 0-6" or 0-9" or 0-12"
Take out the soil-slice (like a bread slice) of ½ inch thick from both the exposed surface of the
pit from top to bottom. This slice is also termed furrow-slice. To collect the soil-slice spade
may be used. Collect the soil samples in a polyethylene bucket.
Collect furrow-slices from 8-10 or sometimes 20-30 sites. Select the sites at random in a zigzag
(or criss-cross) manner. Distribute the sites throughout the entire soil unit (plot). Do not take the
prohibited samples and local problem soils.
Furnish the following information in two sheets of thick paper with the sample. One sheet is
folded and kept inside the bag. Another sheet is folded and attached to the bag.
Available Nitrogen Content in Soil:
Nitrogen is one of the major elements required for life. It will stimulate above ground growth,
and produces the rich green color that is the characteristic of healthy plants, because of this
Nitrogen is essential for plant life. 78% of the atmosphere is covered by molecular Nitrogen
(N2); this form of Nitrogen cannot be used by animals. This molecular Nitrogen must first
combine with Oxygen or Hydrogen to produce compounds such as Ammonia or Nitrate, or
some other organic form of Nitrogen. This is called Nitrogen Fixation. Some Nitrogen Fixation
occurs by lightning and some other by blue green algae. However, the bulk of Nitrogen
Fixation is preferred by bacteria living in the soil. Some of the Nitrogen Fixation bacteria were
living free in the soil, while the others were living within the root nodules of some plants such
as soya bean, peanut, beans, clover, alfalfa, etc. Because of Ammonia or Ammonium is
produced by the decomposition process, the decomposition of materials in the forest is also a
source of Nitrogen. The movement of Nitrogen from the atmosphere into inorganic forms,
followed by the incorporation of Nitrogen into plant matter is represented as the Nitrogen
Cycle, which is shown in the figure.
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The rate of plant growth is proportional to the rate of nitrogen supply. If the soil is deficient in
Nitrogen, the plants become stunted and pale. However, an excess of Nitrogen can damage the
plants just as over-fertilizing the lawn can burn and damage the grass.
Apparatus: - Kjeldahl’s Digestion Assembly, Ammonia Distillation Assembly.
Principle:- The Kjeldahl’s method permits the available nitrogen to be precisely determined in
the plant and in the soil. The method of determination involves three successive phases which
are,
1. Digestion of the organic material to convert nitrogen into HNO3
2. Distillation of the released Ammonia into an absorbing surface or medium
3. Volumetric analysis of the Ammonia formed during the digestion process
Digestion:- Digestion of the organic material is carried out by digesting the sample with Con.
H2SO4 in the presence of CuSO4.H2O as a catalyst and K2SO4 which raise the digestion
temperature. The organic material decomposes into several components i.e.;
C → CO2, O → H2O and N → NH3
In the organic matter, some nitrates are present, most of which are lost during the digestion. The
loss may be disregarded for most soils. Since the amount of NO3- N is far lesser than the
Organic Nitrogen.
2 C6H3 (OH) NH2COO + 26 H2SO4→ (NH4)2SO4+ 25 SO2+ 14 CO2 + 28 H2O
Distillation:- The Ammonia content of the digest is determined by distillation with excess
NaOH and absorption of the evolved NH3 is in standard HCl
(NH4)2SO4 + 2 NaOH → Na2SO4 + 2 NH3 + 2 H2O
NH3 +HCl → NH4Cl
Volumetric Analysis: The excess of standard HCl is titrated against standard NaOH using
Methyl Red as an indicator. The decrease in the multi equivalence of acid as determined by
acid-base titration, which gives a measure of the N content of the sample. The end point is
determined by a change of color from pink to yellow.
2 HCl + 2 NaOH → 2 NaCl + H2O
Significance: The chemical analysis of the soil for nitrogen is less precise when the
requirement for this element needs to be forecast over a longer period of time, as they vary not
only with species, but with the phase of growth and season as well. Therefore the chemical test
for NO3- and NH4+signifies the momentary status when the sample is taken and measures must
be taken instantaneously. The analysis of the extractable Nitrogen content of the soil using a
given extractable method.
In reaction to crop response study provides a basis of N fertility levels, which will
rationalize the use efficiency of Nitrogen fertilizer content of the soil are also needed for the
evaluation of C-N ratios of soils which give an indication of the process of transformation of
organic N to available Nitrogen like ammoniated nitrate Nitrogen.
Procedure:
Determination of Available Nitrogen Content in Soil:-
● Weigh 50 g of processed soil sample in 500 mL Kjeldahl’s flask.
● Add 1 g CuSO4, 10 g K2SO4 and 30 mL Con. H2SO4.
● Shake the contents of the flask until through mixing and allow it to stand for at least 30
minutes with frequent shaking or until the complete solution results.
● Digest the content until greenish color appears. K2SO4 raises the boiling point of the acid.
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So that the loss of acid volatile solution is prevented. CuSO4 5H2O is a digestion
accelerator which catalyzes the speed of the digestion process.
● The reagents sometimes contain impurities so run a blank with the same quantities of
reagents and subtract the blank value from the value of the soil digest
● Digestion is effected on the Kjeldahl’s digestion rack with low flame for the first 10 – 30
min until the frothing stops and then gradually more strongly until the sample is completely
charred. The heat is gradually raised until the acid reaches approximately one third the way
up the digestion-flask. The flame is not allowed to touch the flask above the part occurred
by the liquid. Excessive boiling may cause volatilization of the acid before the organic
matter is oxidized.
● Cool the content and dilute to about 100 mL with distilled water. Swirl the flask for about 2
minutes and transfer the fluid part to a 1000 mL distillation flask.
● Wash the residue left in the Kjeldahl’s flask with 4 or 5 lots of 50 – 60 mL distilled water,
decanting the washings into the distillation flask.
● Add a few, glass bead to prevent bumping.
● Fit the flask with two neck joints to one neck dropping funnel is connected for adding 40 %
NaOH while to the other neck Kjeldahl’s trap, which is used to trap the NaOH coming with
the distillate. The trap is connected to the condenser with a delivery tube which dips into 50
mL of 0.1 N HCl contained in a conical flask, with one or two drops of methyl red
indicator.
● Add about 125 mL (or 100 ml if bumping is a problem) of 40 % NaOH solution till the
content are alkaline in reaction (about 5 times the volume of Con. H2SO4 used during the
digestion). Heat the RB flask.
● Allow the ammonia formed to be absorbed in standard HCl. Wash down the end of the
tube. 150 mL distilled water is added to the conical flask. When no more ammonia is
received (test with a red litmus paper turning blue) stop the distillation.
● Titrate excess of the acid with 0.1N NaOH solution till the pink color changes to yellow.
From the titre value calculate the multi equivalence of the acid participating in the process
of ammonia absorbing during digestion.

a) Calculation:
i. Blank:
Volume of HCl taken for blank = a mL
Volume of NaOH used = b mL
Volume of HCl consumed by liberated NH3 present in blank = a – b = z mL

ii. Sample:
Volume of HCl taken for sample = v mL
Volume of NaOH used = u mL
Volume of HCl consumed by liberated NH3 present in sample = v – u = w mL
Volume of HCl consumed for NH3 liberated by sample only = w – z = y mL
1000 mL 1N HCl = 1000 mL 1 N NH3 = 17 g NH3 = 14 g N
1 mL 1N HCl = 1 mL 1 N NH3 = 0.014 g N
1 mL 0.1 N HCl = 1 mL 0.1 N NH3 = 0.0014 g N

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Weight of Nitrogen in 5 g of Sample = y x 0.0014 g N = q g N

Questions: -
1. Balance the equation CH₃(OH)NH₂COO + H₂SO₄ → (NH₄)₂SO₄ + SO₂ + 14 CO₂ + H₂O
a) 2, 29, 24, 17, 28 b) 2, 29, 24, 17, 28 c) 2, 24, 25, 12, 30 d) 2, 26, 25, 14, 28
2. Which one of the following inorganic forms of nitrogen predominates in the soil?
a) NO3- b) NO2 c) NO d) None of these
3. The process by which organic nitrogen is converted to nitrate through bacterial activity
is known as…………
a) Immobilisation b) Nitrification c) Denitrification d) Aminization
4. In which condition denitrification occurs?
a) Oxygen limiting condition b) Oxygen excess condition
c) Oxygen and nitrogen limiting condition d) Nitrogen limiting condition
5. The microbial transformation of organic nitrogen to inorganic forms is referred to as?
a) Ammonification b) Immobilisation c) Aminization d) Mineralization

Reference: Book: M. L Jackson, "Soil Chemical Analysis", Prentice-Hall, Inc. (1956).

Webliography:
http://www.buzzle.com/articles/soil-ph-levels.html
http://passel.unl.edu/pages/informationmodule.php?idinformationmodule=1130447043&topicorder=
3&maxto=15&minto=1
http://mykitchenbythelake.blogspot.in/2011/05/hydrangeasblue-or-pink.html
http://homeguides.sfgate.com/reduce-alkalinity-soil-20955.html

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