DEPARTMENT OF PHYSICS AND CHEMISTRY

Engineering Chemistry Laboratory Manual

B.TECH. – I & II SEMESTER (Academic Year: 2022-23)

Name:

Roll. No. :

Branch:

Section:

Course code:

Signature of the Faculty In-charge

1
 INSTITUTE VISION AND MISSION
Vision
MGIT envisions, inspires and motivates its students to imbibe knowledge with which they can excel and
serve the nation with great elan. To nurture students into disciplined young citizens of irreproachable
character, coupled with hands – on training and to make them readily employable by fostering social,
cultural and environmental consciousness.

Mission
The Mission of MGIT is to strive towards the development and dissemination of knowledge in many
diversified academic and professional fields. It aims to reach the pinnacle of technical excellence while
pursuing quality improvement continuously. Also, its mission is to train manpower with a capacity to
take-up policy formulation and decision-making responsibilities in terms of resource management.

2
 DEPARTMENT OF PHYSICS AND CHEMISTRY

DEPARTMENT VISION& MISSION

Vision

 To train and develop the basic skill-sets which in turn facilitate the students in achieving academic
excellence.

 To introduce innovative teaching methodologies and evaluation strategies this would sharpen the
professional etiquette of the students.

Mission

 To inculcate the importance of Physics & Chemistry and develop a natural flair for Engineering and
Technology which would mould the student into a competent professional

3
 MAHATMA GANDHI INSTITUTE OF TECHNOLOGY (A)
Chaitanya Bharathi (P.O), Gandipet, Hyderabad-500 075
Department of Physics and Chemistry
Engineering Chemistry Laboratory
Instruction: Semester End Exam Marks : 60 Subject code :CH151BS
3hrs/week
Credits :1 Continual internal Evaluation marks :40 Duration of semester End exam : 3hours

COURSE OBJECTIVES : COURSE OUTCOMES :

Engineering student will learn the following After completing the course, the student will
gain practical knowledge on
1. Estimation of hardness of water to check it 1. Understand the estimation concepts of Metal
suitability for industrial and drinking purpose analysis using EDTA and Dichrometry
and estimation procedures through methods
volumetric analysis. 2. Gain the techniques for analysis of acids using
2. Estimation procedures using Conductometric and potentiometric methods
conductometry and potentiometry. 3. Acquire the skills for the preparation of
3. Preparation of polymers such as Bakelite and Commercially important polymers Bakelite and
Polystyrene in the laboratory. poly styrene
4. Understand the physical properties of 4. Gain the knowledge on Physical properties of
liquids such as saponification value and liquids using viscosity, acid value of oils
viscosity of oils. 5. Acquire the skills for corrosion of metal using
5. Understand the corrosion of metals in a inhibitors
corrosive medium.

CO-PO Mapping For Engineering Chemistry lab

CO PO1 PO2 PO3 PO4 PO5 PO6 PO7 PO8 PO9 PO10 PO11 PO12
1 3 2 1 1 1
2 3 2 1 1
3 2 1 1
4 2 1 1
5 2 1 1 1 1

4
 MAHATMA GANDHI INSTITUTE OF TECHNOLOGY (A)
Chaitanya Bharathi (P.O), Gandipet, Hyderabad-500 075
Department of Physics and Chemistry
Engineering Chemistry Laboratory

S.no Name of the Experiment CO POs

1. Estimation of the amount of Fe2+ in a given solution by 1 1,2,3

Dichrometry.
2. Estimation of Hardness of water by Complexometric method using 1 1,2,3,6
EDTA CIE-I
3. Estimation of the concentration of an acid by Conductometry 2 1,2,3
4. Determination of an acid concentration using Potentiometer 2 1,2,3
5. Estimation of the amount of Fe+2by Potentiometry. 2 1,2,3
6. Estimation of viscosity of lubricating oil using Ostwald’s 3 1,3
Viscometer
7. Estimation of acid value of given coconut oil. 3 1,3 CIE-II
8. Preparation of Bakelite. 4 1,2
9. Determination of rate of corrosion of mild steel in the presence and 5 1,2,3,5
absence of inhibitor.

Virtual lab experiments:

1. Construction of Fuel cell and it’s working.
2. Smart materials for biomedical applications.
3. Batteries for electrical vehicles.
4. Functioning of solar cell and its applications.

Instructions:
The instructions to be followed for the smooth conduct of the Engineering Chemistry Lab
 The students are requested to get their lab manuals.
 Students are advised to prepare for the week’s experiment before entering the lab.
 The experimental values should be attested by the faculty on the same day of performing the
experiment.
 The students must get their calculations evaluated before they enter the lab for the previous
experiments and submit the record without any errors.
 Marks will be deducted for delay in submission of record and observation.
 Repetition of experiments will be permitted only for students with valid reasons along with
evidence signed by parent &HoD.
 Marks will be deducted for repetition of experiments as per the evaluation procedure

5
Table 1a: Rubrics for Evaluation of day-to-dayPerformance
Particulars Marks allotted
Record writing(As per schedule) 10
Viva voce &Result 10
Observation book correction (On the same day)
Total 20
b) Criteria for evaluating marks
Parameter Allocated LOW MEDIUM HIGH
marks
The record was
The record was not Completed record was
submitted in the lab
Record submitted in the lab submitted in the lab
10 session but was
writing session or submitted later session in time
incomplete/mistakes
0-3 4-7 8-10
The student has The student has The student has
Result & 05 completed his exp with completed his exp with completed his exp with
Observation large deviation considerable deviation minute or no deviation
correction
0-1 2-3 4-5
The student did not
The student answered The student answered
answer or few less than
05 more than 50 % of viva more than 70% of viva
Viva voce 50 % of viva questions
questions asked questions asked
asked
0-1 2-3 4-5

Table2: Rubrics for Lab Project (10 Marks)

Particulars Marks allotted Marks obtained
Collection of Procedure 2
Conduct of experiment & Result 6
Viva voce 2
Total 10

Table3: Rubrics for Internal Exam (CIE 1&2) (10 Marks)

Particulars Marks allotted Marks obtained

Principle & Procedure 4
Conduct of experiment & Result 4
Viva voce 2
Total 10

6
 MAHATMA GANDHI INSTITUTE OF TECHNOLOGY (A)
Chaitanya Bharathi (P.O), Gandipet, Hyderabad-500 075
Department of Physics and Chemistry
Engineering Chemistry Laboratory
Laboratory Precautions:
The Chemistry laboratory must be a safe place to work and learn about Chemistry. Most of these involve
just using common sense.
1. Use protective clothing all the time (e.g. lab coat and safety glasses).
2. Be familiar with your lab assignment before you come to lab. Follow all written and verbal
instructions carefully. Observe the safety alerts in the laboratory directions. If you do not
understand a direction or part of a procedure, ask the teacher before proceeding.
3. Wash acid, base, or any chemical immediately with large amounts of waterif spilt on you. Notify
your teacher of the spill.
4. Clean up spills immediately. If you spill a very reactive substance such as an acid or base, notify
the people in the area and then obtain assistance from your teacher. Acid spills should be
neutralized with baking soda, base spills with vinegar before cleaning them up.
5. If chemical substances get in your eye, wash the eye out for 15 minutes. Hold your eye open with
your fingers while washing it out.
6. Place the reagents in a systemic manner.
7. If you burn yourself on a hot object, immediately hold the burned area under cold water for 15
minutes. Inform your teacher.
8. Always add acid to water and stir the solution while adding the acid. Never add water to an acid.
9. Report all accidents to your teacher.
10. Thoroughly clean your laboratory work space at the end of the laboratory session. Make sure that
all the items of equipment are clean and returned to its original place.
11. When weighing, never place chemicals directly on the balance pan. Never weigh a hot object.
12. Do not smell anything in the laboratory unless your teacher tells you it is safe. Do not smell a
substance by putting your nose directly over the container and inhaling. Instead, waft the vapors
toward your nose by gently fanning the vapors toward yourself.
13. Do not work in the laboratory without an instructor present. Work only with your lab partner(s).
Do not venture to other lab stations for any reason.

7
 14. Do not wear bulky or dangling clothing.
15. Do not eat or drink in the laboratory. Do not chew at the end of a pen which was lying on the lab
bench.
16. Do not use Mobile Phones.
17. Do not directly touch any chemical with your hands. Do not Taste materials in the laboratory.
18. Do not waste the reagents.
19. Do not touch any equipment, chemicals, or other materials while entering the lab/classroom
without being instructed to do so.
20. Do not perform any experiment not authorized by the instructor.
Precautions during the Experiment:
1. All the glassware should be properly cleaned and dried.

2. All solutions should be freshly prepared.

3. Same amount of the indicator must be used each time of the titration while repeating.

4. Addition of reagents from the burette should be drop wise.

5. Be careful about color change at the time of end point.

6. There should be no air bubbles inside the burette.

7. Note the reading of lower meniscus inside the burette in case of colorless solution and upper
meniscus in case of colored solution.
8. The end point must be observed meticulously during the titration.
BASIC CONCEPTS OF VOLUMETRIC ANALYSIS

Chemical analysis of the compounds is carried out in two ways

1. Qualitative analysis: Qualitative analysis shows what element a given substance contains.
Ex: Semi-microanalysis (salt analysis), Identification of organic functional groups
2. Quantitative analysis: Quantitative analysis determines the quantity of a particular component present
in substance. It is carried out in two ways:
1. Gravimetric analysis: Gravimetric analysis involves the estimation of the amount of a given
compound from the results of weighing.

Ex:Volatilization and Precipitation gravimetry

2. Volumetric analysis: Volumetric analysis is based on measuring the volume of the solution of a
substance.
It is classified into following types

8
 a) Acid –base titrations (Neutralization titrations)
b) Redox titrations
c) Complexometric titrations
d) Precipitation titrations
Terms involved in volumetric analysis
1. Titration: The process of finding out the volume of one of the solutions required to react completely
with a definite volume of the other solution of known concentration is called titration.
2. Titrant: The solution of known strength is called titrant.
3. Titrate: The solution whose concentration is to be estimated.
4. Indicator: The reagent which indicates the endpoint or equivalence point of the titration.
The strength of concentration of a solution is expressed in the following ways.
5. Normality: Number of gram equivalents of solute particles present per liter of the solution
is called Normality. It is denoted by N

6. Dilution Principle: Addition of water to a solution is called dilution. If a solution, initial concentration
(N1) and initial volume (V1), is diluted to volume (V2) and normality (N2). Then, N1V1 = N2V2
7. Molarity: Number of moles of solute particles present per liter of solution is called Molarity. It is
denoted by M
Weight of solute 1000
M = MolecularweightofsolutexVolume of solvent in ml.

8. Molality: It is the number of moles of the solute particles present per kg of the solvent. It is denoted by
(m).
Weight of solute 1000
m = Molecularweightofsolutexweight of solvent in grams

9
 EXPERIMENT NO: 1
ESTIMATION OF FERROUS BY DICHROMETRY
Aim: To estimate the amount of ferrous present in the given solution using a standard solution of
potassium dichromate (K2Cr2O7).
Apparatus: Pipettes, Burette, Conical Flask, Beakers, Weighing Bottle, Balance, Measuring jar, wash
bottle etc.
Chemicals: Pure K2Cr2O7 Salt, Acid mixture (6N H2SO4+6N H3PO4), FeSO4 solution, Barium
diphenylamine sulphonate indicator.
Principle: Ferrous iron is oxidized to ferric iron by potassium dichromate in acidic medium. The
completion of oxidation reaction is marked by the appearance of the bluish violet color of Barium
diphenylamine sulphonate, which is used as an internal indicator.
K2Cr2O7 + 4H2SO4 K2SO4 + Cr2 (SO4)3 + 4H2O + 3(O)
6FeSO4 + 3H2SO4 + 3(O) 3Fe2 (SO4)3 + 3H2O
Overall reaction:
K2Cr2O7 + 7H2SO4 + 6FeSO4 K2SO4 + Cr2 (SO4)3 +3Fe2 (SO4)3+ 7H2O
(K2Cr2O7 = 3(O) = 6Fe+2)
Equivalent weight of iron is its atomic weight i.e. 55.85. Since one equivalent weight of Potassium
dichromate oxidizes six equivalents of iron.
Procedure: It consists of 2 parts
Step-1: Preparation of standard Potassium dichromate solution: Weigh accurately the given pure
sample of potassium dichromate and transfer it into 100 ml standard flask with a funnel. Dissolve it in
small quantity of distilled water and make up the solution up to the mark. The contents in the flask are
shaken well for uniform concentration. Calculate the normality of potassium dichromate solution.
Weight of the weighing bottle + the salt taken (W1 ) = ------ gm
Weight of the empty weighing bottle (W2) = ------- gm
Weight of the Potassium dichromate (W1 – W2) = ------- gm
Equivalent weight of K2Cr2O7 = GMW/Z = 294/6=49
W1−W2 1000
Normality of Potassium dichromate solution (N1) = x
49 100

Step-2: Estimation of Ferrous iron: Dilute the given unknown solution into a 100ml standard flask and
make the solution up to the mark with distilled water, and shake the flask for uniform concentration. Rinse
the pipette with the ferrous solution and pipette out 20 ml into a clean conical flask. Add 20ml of the acid
mixture (6N H2SO4 + 6N H3PO4) and add 3 - 4 drops of Barium diphenylamine sulphonate indicator.
Titrate the solution against standard potassium dichromate solution taken in the burette till, the color
10
changes to bluish violet color (end point) via green color. Repeat the titrations for at least two concurrent
titer values.
S.No. Volume of iron Burette readings Volume of
solution pipette Initial Final K2Cr2O7Solutionrequired
out(ml) (ml)
1
2
K2Cr2O7 FeSO4
Normality of K2Cr2O7 solution (N1) =------ N; Normality of Iron Solution (N2)=------ ?
Volume of K2Cr2O7 solution (V1) =------ ml; Volume of Iron solution (V2) =------ ml
Normality of Iron Solution (N2) = N1V1 = -------- N
V2
Amount of Ferrous ion present in the given solution:
N2 x Eq.wt.of Fe2+ = N2 x 55.85 = ----------- g/100ml
10 10
Result:1) Normality of Ferrous solution (N2) = -----------------N
2) Amount of Ferrous present in the given solution= --------- g/100ml
Viva – Questions
1. Define Molarity and Normality. Give the relationship between them.
2. Define standard solution. What is the standard solution used in this experiment
3. Define Oxidation ad Reduction? List out the oxidizing & reducing agents in Dichrometry
4. Name the indicator used in the titration and write its chemical structure
5. How do you estimate Fe+2 volumetrically?
6. What are the molecular and equivalent weights of Iron & K2Cr2O7 ?
7. Write the chemical principle of this experiment?
8. What is the purpose of adding sulfuric acid and phosphoric acid to the Fe +2solution before
titration?
9. Why the color of the contents of conical flask is green color before the end point?
10. How do you detect the end point in this experiment?

11
 EXPERIMENT NO: 2
ESTIMATION OF HARDNESS OF WATER BY COMPLEXOMETRIC METHOD USING EDTA
Aim: To determine the total hardness of water by Complexometric method using EDTA.
Apparatus: Standard Flask, Pipette, Burette, Conical Flask, Beakers, Weighing Bottle, Funnel etc.
Chemicals required: Epsom Salt (MgSO4 .7H2O), EDTA solution. (Ethylene diaminetetra acetic acid),
EBT indicator (Eriochrome black-T), Buffer solution (NH4Cl + NH4OH) (pH= 9-10) & Hard water
sample.
Principle:
The hardness of water is generally due to the presence of calcium and magnesium ions in water. The
chlorides, nitrates and sulphates of calcium & magnesium are responsible for permanent hardness, while
bicarbonates of calcium & magnesium are responsible for temporary hardness. EDTA forms a stable
complex of Ca-EDTA or Mg-EDTA with hardness causing ions of Ca and Mg present in hard water at
pH9-10. EBT is used as the indicator to detect the completion of the reaction. When a small amount of
EBT is added to hard water sample, it reacts with Mg 2+ or Ca2+ to produce wine red colored solution due
to the formation of a complex. This wine red colored solution is titrated with EDTA till the colour of the
solution changes blue, as EBT is released free in the solution and the stable Mg-EDTA or Ca-EDTA
complex is formed. End point is determined by the change in colour from wine red to blue.
pH 9 - 10
M + EBT --------- → M-EBT complex (wine red color)
2+

Hard water Blue Less stable

pH9 - 10
M-EBT complex + EDTA --------→ M –EDTA complex + EBT
More stable, (colorless) (blue)
+2 +2 +2
(Here M = Ca or Mg )
Procedure: It consists of 3 parts:
PART – I: Preparation of standard Epsom salt (MgSO4.7H2O) Solution:
Weigh out accurately the given Epsom salt (MgSO4.7H2O) and transfer it into clean 100ml standard
flask using a funnel. Dissolve the substance in minimum quantity of distilled water and make it up to the
mark with distilled water. Shake the solution thoroughly for uniform concentration.
Weight of the weighing bottle + Epsom salt (W1) = -------------- grams
Weight of the empty weighing bottle (W2) = ------------- grams
Weight of the Epsom salt (W1 – W2) = ----------------- grams
W1−W2 1000
Normality of Epsom salt solution. (N1) = x = ---------N
123 100

12
PART – II: Standardization of EDTA solution using standard MgSO 4.7H20 solution: Pipette out
20ml ofMgSO4.7H20 solution, into a clean conical flask and add 5ml of buffer solution of (mixture of
NH4OH + NH4Cl) followed by 4 to 5 drops of EBT-indicator. Titrate this solution against the EDTA
solution taken in the burette, until the wine-red color of the solution turns blue (end point). Repeat the
titration for at least two concurrent titer values.
S.No. Volume of Epsom Burette readings Volume of EDTA
salt solution(ml) Initial Final required(ml)
1
2
3

Epsom salt solutionEDTA solution

Normality of Epsom salt solution(N1) =------ N Normality of EDTA solution (N2) = -----
Volume of Epsom saltsolution (V1)= -------ml Volume of EDTA solution (V2) = ------
Normality of EDTA solution (N2) = N1V1= ------------- N
V2
PART – III: Estimation of Total hardness of water:
Dilute the given unknown hard water into a 100ml standard flask and make the solution up to the mark
with distilled water, pipette out 20 ml freshly prepared solution and add 5ml buffer solution
(NH4OH+NH4Cl) followed by 4 - 5 drops of EBT indicator. Titrate this solution against the standardized
EDTA solution, until the wine-redcolor changes blue (end point). Repeat the titration for at least two
concurrent titer values.
S.no Volume of Hard Water Burette readings Volume of EDTA
Pipette out(ml) Initial Final required (ml)
1
2
3
EDTASolutionHard water
Normality of EDTA solution (N2) =------N; Normality of hard water (N3) =------- N
Volume of EDTA solution (V2) =------ml; Volume of hard water (V3) =------- ml
Normality of hard water (N3) = N2V2 =----------- N
V3

13
Total hardness of water in terms of CaCO3 equivalents = N3 x 50 x1000 mg/lit
=---------------- mg/lit or ppm
RESULT:
1) Normality of EDTA solution (N2) =--------------N
2) Normality of Hard Water in terms of CaCO3 equivalents (N3) = ------------- N
3) Total hardness of water in terms of CaCO3 equivalents =---------------- ppm

Viva – Questions
1. Mention the various units of hardness of water

2. What are the chemical substances responsible for temporary and permanent hardness of water

3. Why carbonate hardness is temporary?

4. Non-carbonate hardness cannot be removed easily. Give the reason.

5. Write the chemical reactions taking place between hardness causing ions & EDTA

6. Define buffer solution. Why basic buffer is added to hard water during titration.

7. Why this method of estimation is known as Complexometric method

8. What is the indicator used in this method? Draw its chemical structure

9. What are the colour changes observed with metal indicator complex and metal EDTA complex

10. Draw the structure of Na2EDTA and Ca-EDTA

11. What are the equivalent weights of Epsom salt (MgSO 4.7H2O) and Calcium Carbonate?

12. Calculate the weight of MgSO4.7H2O required to prepare 100ml of 0.01N solution?

14
 EXPERIMENT NO: 3
ESTIMATION OF HCl BY CONDUCTOMETRY
(STRONG ACID VS STRONG BASE)
Aim: To estimate the amount of HCl present in the given solution using NaOH solution by
Conductometric titration.
Apparatus: Conductometer, conductivity cell, beakers, glass rod, conical flask, burette, standard flask,
weighing bottle, funnel, pipette, Wash bottle etc...
Chemicals: Oxalic acid (H2C2O4.2H2O), NaOH solution, HCl solution, phenolphthalein indicator, and
distilled water.
Theory: The electrical conductance of any electrolytic solution depends on the number of ions and their
mobilities. In the titration of HClv/sNaOH, before the addition of NaOH, HCl shows high conductance,
due to the presence of highly mobile H+ ions. As NaOH solution is added, the H+ ions combine with OH -
and form feebly ionizable H2O molecules.
[ H+ + Cl-] + [Na+ + OH-] → [Na++ Cl-] + H2O
Hence the conductance of the solution decreases gradually by the addition of NaOH solution. When all the
H+ ions have been neutralized, the conductance starts increasing with the further addition of NaOH, due to
the increase in no. of OH- ions. When a graph is drawn between the volume of NaOH added and
conductance, the point of intersection gives the end point.
Operational instructions:
Procedure: It consists of 3 parts
Part–I: Preparation of standard solution of oxalic acid:
Weigh accurately a sample of oxalic acid and transfer it into a clean 100ml standard (volumetric) flask
using a funnel. Dissolve the substance in minimum quantity of distilled water. Make the solution up to the
mark with distilled water and shake well for uniform concentration.
Weight of weighing bottle + oxalic acid (W1) =--------- grams
Weight of empty weighing bottle (W2) =---------- grams
Weight of oxalic acid taken (W1- W2) = --------- grams
W1−W2 1000
Normality of oxalic acid (N1) = x = ---------N
63 100

15
Part- II: Standardization of given NaOH solution: Pipette out 20ml of standard oxalic acid solution
into a clean conical flask and add 2 - 3drops of phenolphthalein indicator. Titrate the contents of the
conical flask against the NaOH solution taken in the burette until a pale pink colour (end point) is
obtained. Repeat the titration for at least two concurrent titre values.
S.No Vol. of Oxalic acid Burette readings Vol. of NaOH
Pipette out(ml) Initial Final Required
(Initial-Final) (ml)
1
2
3

Oxalic acid Solution NaOH Solution

N1 = -------- N N2= -------- N
V1 = 20 ml V2 = ------- ml
Normality of NaOH solution (N2)=N1V1 = --------- N
V2
Part-III: Estimation of the amount of HCl using Conductometric titration:
Dilute the given unknown solution into a 100ml standard flask and make the solution up to the mark with
distilled water. Pipette out 40ml of the above HCl solution into a well cleaned 100 ml beaker, dip the
conductivity cell in it. Then press the push button and stir the solution with glass rod, measure the initial
conductance. Add 1ml of NaOH solution from the burette and note down the corresponding conductance
after stirring the solution. Take a minimum of 20 readings.
S.No. Volume of Conductance x
NaOH (ml) range (mS)
1 0
2 1
3 2
4 3
5 4
6 5
7 6
8 7
9 8
10 9
11 10
12 11
16
 13 12
14 13
15 14
16 15
17 16
18 17
19 18
20 19
21 20

Graph: Plot a graph taking volume of NaOH added on X-axis and corresponding conductance on Y-axis.
It gives two straight lines. Intersection of the two straight lines indicates the neutralization point.

NaOH Solution HCl Solution

N2= --------- N N3 =-------- N
V2 = ----------ml (from graph) V3 = 40ml
Normality of HCl solution (N3) = N2V2 = --------------N
V3
Amount of HCl in the given solution = N3X 36.5/10
= -----------g/100ml
Result:
1. Normality of NaOH solution (N2) =-------N
2. End point of the HCl (from graph) =-------- ml
3. Normality of HCl solution (N3)=----------N
4. The amount of HCl present in the given solution = ---------g/100ml

17
 Viva – Questions
1. What is conductance? What are its units?
2. What are responsible for conductance of an electrolyte?
3. What happen to specific and equivalent conductance on dilution?
4. What are the advantages of instrumental chemical analysis over conventional volumetric analysis?
5. What is cell constant and give its units?
6. In the titration of HClVsNaOH even at the neutralization point some conductivity is observed .Why?
7. Conductivity cell is an electrolytic cell? Give the reason.
8. Draw a model graph for this experiment?
9. What is the effect of temperature on the conductance of the electrolyte?
10. How equivalent conductance from molar conductance is differentiated?

EXPERIMENT NO: 4
DETERMINATION OF AN ACID CONCENTRATION USING POTENTIOMETER
Aim: To Estimate the amount of HCl present in the given solution using NaOH by potentiometric
titration.
Apparatus: Potentiometer, saturated calomel electrode, platinum electrode, salt bridge, beakers, glass rod,
conical flask, burette, standard flask, weighing bottle, funnel, pipette...
Chemicals: Oxalic acid (H2C2O4.2H2O), NaOH solution, HCl solution, phenolphthalein indicator,
saturated KCl solution, quinhydrone powder, and distilled water.
Theory:
It involves potentiometric measurement of EMF of a cell constructed using the test solution-HCl which is
used for determining the end point in acid-base titration. The cell consists of a saturated calomel electrode
(SCE) as reference electrode and quinhydrone electrode (Q 1+ QH2) as the indicator electrode, the EMF of
which depends on the H+ ion concentration of test solution. The quinhydrone is a powdered organic
substance having equimolar mixture of quinone (Q) and hydroquinone (QH2). When a pinch of
quinhydrone is added to the acid solution in contact with platinum wire/electrode, quinone, hydroquinone
and H+ ions form a reversible redox system.

18
Initially, before titration, the EMF measured will be high due to high H+ concentration (low PH ) and on
addition of NaOH solution, it decreases due to decrease in concentration of H+ as a consequence of
neutralization to form H2O.
HCl + NaOH → NaCl + H2O
After neutralization, it decreases even below zero as indicated by –ve value. The cell used can be
represented asPt, Hg(l) / Hg2Cl2(S),KCl(sat.soln) // H+(C=?),Q / QH2, Pt.
Oxidation takes place at calomel electrode and reduction takes place at quinhydrone electrode. Thus EMF
of the cell is calculated as
Ecell = Eright- Eleft=EQ- Ecalomel
= [0.6994-0.0591PH] – 0.2422
Ecell= 0.4572 – 0.0591PH
Procedure: It consists of 3 parts
Part –I: Preparation of standard solution of oxalic acid
Weigh accurately a sample of oxalic acid and transfer it into a clean 100ml standard (volumetric)
flask using funnel. Dissolve the substance in minimum quantity of distilled water. Make the solution up to
the mark with distilled water and shake well for uniform concentration.
Weight of weighing bottle + oxalic acid (w1) = ------- grams
Weight of empty weighing bottle (w2) = -------- grams
Weight of oxalic acid taken (w1- w2) = -------- grams
W1−W2 1000
Normality of oxalic acid (N1) = x = ----------N
63 100

Part- II: Standardization of given NaOH solution:

Pipette out 20ml of the standard oxalic acid solution into a clean conical flask and add 1-2 drops of
phenolphthalein indicator. Titrate the contents of the conical flask against the NaOH solution taken in the
burette until a pale pink color (end point) is obtained. Repeat the titration for least two concurrent titer
values.
S.No Vol. of Oxalic acid Burette readings Vol. of NaOH required
(ml) IBR FBR (FBR – IBR) (ml)
1
2
3

19
Oxalic acid Solution NaOH Solution
N1 =--------- N N2 =-------- N
V1 = 20 ml V2 =--------ml
N1V1
Normality of NaOH solution (N2) = = ---------N
𝑁2

Part-III: Estimation of the amount of HCl in the given solution using potentiometer:
Dilute the given unknown solution into a 100ml standard flask and make the solution up to the mark with
distilled water. Pipette out 20 ml of above HCl solution into a clean 100ml beaker and add a pinch of
quinhydrone powder. Dip the platinum electrode into it and connect it to the potentiometer. Dip the
calomel electrode into saturated KCl solution provided in another beaker. Connect these two solutions
with salt bridge and measure the initial EMF. Now add 1ml ofNaOH solution from burette and stir it with
glass rod. Note down the corresponding EMF. Take about 20 readings. Note the volume of NaOH where
there is a steep change in EMF (+ve EMF to –ve EMF), this indicates the neutralization point.
S.No. Volume of EMF ∆E=E1-E2 ∆V=V2-V1 ∆E/∆V
NaOH (ml) (mV)
1 0
2 1
3 2
4 3
5 4
6 5
7 6
8 7
9 8
10 9
11 10
12 11
13 12
14 13
15 14
16 15
17 16
18 17

20
 19 18
20 19
21 20

Graphs: Plot a graph between volume of NaOH on X-axis and corresponding EMF on Y-axis the volume
of NaOH at which (+ve) EMF changes to (–ve) EMF gives the end point (approximate) which has been
consumed to neutralize 20ml of HCl taken in the beaker. Plot another graph taking volume of NaOH on
X-axis and ∆E/∆V on Y-axis, the highest inflection point gives the exact end point of HCl solution.

HCl Solution NaOH Solution

N2= -------- N N3 = --------- N
V2 = --------ml (from graph -2) V3 = 20 ml
Normality of HCl solution (N3) = N2V2 = ---------- N
V3
Amount of HClin given solution= N3 X 36.5/10 = ------------g/100ml
Results:
1. Normality of NaOH solution (N2) =---------N
2. End point of HCl (from graph -2) = ----------ml
3. Normality of HCl solution (N3) = ----------N
4. The amount of HCl present in the given solution = ---------g/100ml
VIVA questions
1. What is an Electrochemical Cell? Give an Example.
2. Define electrode potential and standard electrode potential?
3. What is SCE? Give its EMF values.
4. WhyQuinhydronepowder is added to HCl solution? Give the reason.
5. What is Cell notation? Write the cell notation of the cell used in the experiment.
21
6. Why cell potential decreases with addition of alkali to the acid solution.
7. How do you get EMF of a cell consisting of two electrodes?
8. Give the relation between pH and EMF of Quinhydrone electrode?
9.What is the role of a referenceelectrode and indicator electrode in this experiment?
10. How to prepare salt bridge? List out its functions?
EXPERIMENT NO: 5
ESTIMATION OF FERROUS (Fe+2) BY POTENTIOMETRY
Aim: To estimate the amount of Fe2+ present in given solution, using KMnO4 solution by Potentiometric
titration.
Apparatus: Potentiometer, saturated calomel electrode, platinum electrode, salt bridge, beakers, glass rod,
conical flask, burette, standard flask, weighing bottle, funnel, pipette.etc...
Chemicals: Mohr’s salt (Ferrous ammonium sulphate), Conc. H2SO4, 6N H2SO4, KMnO4, saturatedKCl
solution and distilled water.
Theory: Potentiometric measurement of EMF is used for locating the end point in the redox titrations.
The cell consists of a saturated calomel electrode (SCE) as reference electrode and the platinum electrode.
The EMF of the electrode dipped in Fe2+ (Test) solution as an indicator electrode depends upon the
ratio,(Fe+2/ Fe+3)
The cell can be represented as: (-) Pt, Hg/Hg2Cl2(s)/ KCl (sat) // Fe3+/ Fe2+, Pt (+).
The EMF of the cell is given by

Initially, the conc. of Fe3+ in the solution is very low and the EMF measured will be low and on addition
of KMnO4 solution to Fe2+ solution, the concentration of Fe3+ increases ( due to oxidation of Fe2+) and the
EMF increases. Finally, at the end point, the EMF increases sharply and an inflection in the titration curve
can be observed due to sharp decrease in Fe2+ concentration.
5Fe2+ + MnO-4 + 8H+ -----→ 5Fe3+ + Mn2+ + 4H2O
Procedure: It consists of 3 parts
Part –I: Preparation of standard solution of Mohr’s salt(FeSO 4(NH4)2SO4.24H2O):
Weigh accurately a sample of Mohr’s salt and transfer it into a clean 100ml standard (volumetric)
flask using a funnel. Add about 50ml of distilled water followed by 8 drops of conc.H2SO4 and shake the
flask to dissolve the substance. Make the solution up to the mark with distilled water and shake well for
uniform concentration.
Weight of weighing bottle + Mohr’s salt (W1) =--------- gm
22
Weight of empty weighing bottle (W2) = -------- gm
Weight of Mohr’s salt taken (W1-W2) = --------- gm
W1−W2 1000
Normality of Mohr’s salt (N1) = x = ----------N
392 100

Part- II: Standardization of KMnO4 solution:

Pipette out 20ml of standard Mohr’s salt solution into a clean conical flask and add about 20ml of
6N H2SO4 solution. Titrate the contents of the conical flask against the KMnO 4 solution taken in the
burette until a permanent pale pink color (end point) is obtained. Repeat the titration for at least two
concurrent titer values.
S.No Vol. of Mohr’s salt Burette readings Vol. of KMnO4
(ml) Initial Final (ml)
1
2

Mohr’s salt solution KMnO4 Solution

N1= ---------- N N2 =--------N
V1 = 20 ml V2 = titer value-- ml
Normality of KMnO4 solution (N2)= N1V1 = ----------N
V2
Part-III: Estimate the amount of Fe2+ in the given solution:
Dilute the given unknown solution into a 100ml standard flask and make the solution up to the mark with
distilled waterand shake the solution thoroughly. Pipette out 20ml of Fe2+ solution into a clean beaker and
add a 20ml 6N H2SO4 to it. Dip the platinum electrode into the same solution and connect it to the
potentiometer. Dip the calomel electrode into saturated KCl solution provided in another beaker. Connect
these two electrodes with a salt bridge and measure the initial EMF. Now titrate the solution by adding
1ml of KMnO4 each time and note down the corresponding EMF. Take about 21 readings in the following
tabular column. (Note the volume of KMnO4 where there is a steep change in EMF. This volume is the
approximate volume of KMnO4 required for oxidation of Fe2+.
S.No. Volume of EMF ∆E=E2-E1 ∆V=V2-V1 ∆E/∆V
KMnO4 in (ml) (mV)
1 0
2 1
3 2

23
 4 3
5 4
6 5
7 6
8 7
9 8
10 9
11 10
12 11
13 12
14 13
15 14
16 15
17 16
18 17
19 18
20 19

Graphs: Plot a graph between volume of KMnO4 on X-axis and corresponding EMF on Y-axis. Plot
another graph (differential graph) taking the volume of KMnO 4 on X- axis and ∆E/∆V on Y-axis. From
graph – 1, the volume of KMnO4 at which steep change in EMF is noted. This gives the approximate
volume of KMnO4 needed for oxidation of given ferrous solution. From graph – II (inflexion point), the
exact titre value can be known.

24
KMnO4 Solution Fe2+ Solution
N2= from step 2 N3 =--------N
V2= ------- ml(from graph – 2) V3 = 20 ml
Normality of KMnO4 solution = N3 = N2V2 = -----------N
V3
Amount of Ferrous in given 100 ml solution = N3 x 56 = -----------g/100ml.
10
RESULT:
1) Normality of KMnO4 solution(N2) = ---------- N
2) End point of FeSO4 solution (from graph -2) =---------- ml
3) Normality FeSO4 solution(N3) = --------- N
4) Amount of Ferrous iron in given solution = --------- g/100ml
Viva questions
1. What is Single electrode potential? How it is calculated?
2. What is Electromotive force? Give its units.
3. What is the role of KCl in Salt Bridge?
4. How do you find out inflection point from the graph?
5. Write the chemical reactions involved in this experiment?
6. Give the principle of potentiometric titration
7. What type of cell is setup in Potentiometric titration? Write its components.
8. What is cell notation? Write the cell notation.
9. What are the advantages of potentiometric titrations over Conductometric titrations?
10. Why is the concentrated sulphuric acid added during the preparation of Mohr’s salt solution?
11. Name the electrodes used in potentiometric titration? Give their significance.

25
 EXPERIMENT- 6
PREPARATION OF BAKELITE
Aim: To prepare phenol formaldehyde resin (Bakelite).
Chemicals: Glacial acetic acid, 40% formaldehyde solution, Phenol, Conc. H 2SO4.
Apparatus: Glass rod, beakers, funnel, measuring cylinder, dropper and filter paper.
Principle: Phenol formaldehyde resins (PFs) are condensation polymers and are obtained by condensing
phenol with formaldehyde in the presence of an acidic or alkaline catalyst. These are thermosetting
polymers. Phenol formaldehyde resins (PFs) are prepared by the reaction of phenol with formaldehyde in
the presence of acidic or basic catalyst. A mixture of phenol and formaldehyde are allowed to react in the
presence of a catalyst. The process involves formation of methylene bridges in ortho, para or both ortho
and para positions. These results first the formation of linear polymer (called NOVALAC) and then into
cross-linked polymer called phenol-formaldehyde resin or Bakelite.

26
Procedure:
1. Place 5 ml of glacial acetic acid and 2.5 ml of 40 % aq formaldehyde solution in a 100
ml beaker. Add 2 g phenol safely.
2. Wrap the beaker with a wet cloth or place it in a 250 ml beaker having small amount
of water in it.
3. Add conc. HCl drop wise with vigorous stirring by a glass rod till a pink colored
gummy mass appears.
4. Wash the pink residue several times with water to make it free from acid.
5. Filter the product and weigh it after drying in folds of a filter or in an oven. Report the
yield of polymer formed.
Result: The weight of the phenol formaldehyde resin is ___ g.
Precautions:
1. The reaction is sometimes vigorous and it is better to be a few feet away from the beaker while adding
the H2SO4 and until the reaction is complete.
2. The experiment should be preferably carried out in fume cupboard.
Viva voce:
1. Define Polymer? Give an example.
2. What is Monomer? Give the monomers of this experiment
3. Define functionality. What is the functionality of Phenol and acetylene?
4. Give main uses of the phenol formaldehyde resin.
5. What is the principle of preparation of Bakelite?
6. Briefly describe the properties and applications of Bakelite.
7. Write chemical equations for preparation of phenolic resins.
8. Phenol formaldehyde resin is also called _________________.
9. What is the Catalyst used for this experiment?
10. Why is Bakelite a thermosetting polymer?

27
 EXPERIMENT: 7
DETERMINATION OF ACID VALUE OF COCONUT OIL
Aim: To determine the acid value of coconut oil using potassium hydroxide solution.
Apparatus: Burette, beaker, conical flask, measuring cylinder and 100ml standard flask.
Chemicals: Coconut oil, NaOH solution, fat solvent (mixture of 100ml ethanol and 100ml diethyl ether)
and phenolphthalein indicator.
Theory: Acid value is expressed as the percentage of free fatty acid present in oil or fat. It is defined as
the number of milligrams of caustic potash or caustic soda required to neutralize the acid in 1 gm of the
sample. Fatty acids are normally found in the triglyceride form, but hydrolysis of these fatty acids
accounts to the decreased quality of the oil. The normal acid value for most samples lies within 0.5mg.
high acid value indicates a stale oil or fat stored under improper conditions.

Procedure: It consists of 3 steps.

Part –I: Preparation of standard solution of oxalic acid:
Weigh accurately a sample of oxalic acid and transfer it into a clean 100ml standard (volumetric)
flask using a funnel. Dissolve the substance in minimum quantity of distilled water. Make the solution up
to the mark with distilled water and shake well for uniform concentration.
Weight of weighing bottle + oxalic acid (w1) = ------- gms
Weight of empty weighing bottle (w2) = -------- gms
Weight of oxalic acid taken (w1- w2) = -------- gms
W1−W2 1000
Normality of oxalic acid (N1) = x = ----------N
63 100

Part- II: Standardization of given KOH solution:

Pipette out the standard oxalic acid solution into a clean conical flask and add 1-2 drops of
phenolphthalein indicator. Titrate the contents of the conical flask against the KOH solution taken in the
burette until a pale pink color (end point) is obtained. Repeat the titration for at least two concurrent titer
values.

28
 S.No Vol. of Oxalic acid Burette readings Vol. of NaOH required
(ml) IBR FBR (FBR – IBR) (ml)
1 20
2 20
Oxalic acid Solution NaOH Solution
N1 =--------- N N2 =-------- N
V1 = 20 ml V2 =--------ml
N1V1
Normality of NaOH solution (N2) = = ---------N
𝑁2

Step – III: Determination of acid value:

Take the given oil weigh and transfer into 250 ml conical flask. To this add 50ml of neutralized alcohol
solution and 2 drops of phenolphthalein indicator are and titrate against KOH solution till the color
changes to pale pink.
Burette Readings Vol. of NaOH required
S.No Vol. of coconut oil
IBR FBR (FBR – IBR) (ml)
1 5 ml
2 5 ml
3 5 ml

Calculations
Volume of NaOH x Normality of NaOH x Eq.Wt of KOH
Acid value = Weight of Oil sample

Equivalent weight of KOH = 55.85

Acid Value = __________.
Result: The acid value of the coconut oil is ___________mg of KOH/gm of sample.
Viva-Voice
1. What is Acid value? How the acid value of given oil is calculated?
2. What is saponification? Give an example
3. Write the chemical reactions involved in this experiment?
4. What are triglycerides?
5. What happens when alcohol is mixed with oil?
6. What is Acidity? Give the Acidity of KOH.
7. Write the chemical formula of Lauric acid, Myristic acid. Give its percentage in coconut oil
8. What are the products formed during hydrolysis of fats?
29
 EXPERIMENT NO: 8
DETERMINATION OF VISCOSITY
Aim: To determine the viscosity of a given liquid using Ostwald viscometer.
Apparatus: Ostwald viscometer, beaker, pipette, rubber tube, stand.
Chemicals required: n-Butanol and distilled water.
Principle: It is the property of fluids. It is defined as the resistance to the flow of a liquid. It measures the
resistance to the flow shown by a layer of fluid when another adjacent parallel layer tends to flow past the
first layer. When a liquid flows through a narrow tube, the velocity of flow depends on the force that
produces the flow. The same amount of various liquids flowing through the same capillary tube doesn’t
take the same time to flow. This is due to the difference in their viscosities. If two liquids with viscosities
η1, η2 having densities d1, d2 and their time of flow t1, t2 respectively then,
𝜂1 𝑑1𝑡1
=
𝜂2 𝑑2𝑡2
Procedure: Clean the viscometer with chromic acid and then with distilled water. Dry the apparatus and
clamp it in vertical position to the stand. Now pipette out distilled water and introduce into the viscometer
to bulb A side. Suck the liquid by means of rubber tubing a little beyond level A of the bulb B. allow the
liquid to flow through the capillary tube under its own weight. When the liquid reaches level A start the
stop clock and when the liquid reaches level B, stop the clock. Note down the time taken for the flow of
water. Repeat the above procedure for 3 times and find the mean time flow for distilled water. Let it be t 1.
Repeat the above procedure for organic liquid after cleaning and drying the viscometer. Note
down the mean time flow for organic liquid. Let it be t 2.

30
Observation table
Time taken for the flow of
S.No. Time taken for the flow of water(t 1) sec. organic liquid(t2) sec.
1
2
3
Average time taken = Average time taken =

𝜂1 𝑑1𝑡1
=
𝜂2 𝑑2𝑡2
η1 = Viscosity of distilled water = 8.90 millipoise.
η2 = Viscosity of organic liquid = -------------- millipoise.
d1 = Density of water = 1 gm/cm3.
d2 = Density of organic liquid = 0.81 gm/cm3.
t1 = time taken for the flow of water = --------------- sec.
t2 = time taken for the flow of organic liquid = ----------- sec.
𝜼𝟏 ×𝒅𝟐 𝒕𝟐
Therefore, viscosity of organic liquid, η2 = 𝒅 𝟏 𝒕𝟏

RESULT: Viscosity of the given organic liquid is -------------------- millipoise.

Viva – Questions
1. Define Viscosity.
2. Define absolute Viscosity.
3. Define kinematic Viscosity.
4. How to calculate the viscosity of given liquid?
5. Give the relation between absolute and kinematic viscosity.
6. What is the importance of viscosity? Where is this phenomenon used?
7. Give the relation between viscosity and density of lubricants.
8. Give the relation between viscosity and temperature of lubricants.

31
 Exp: 9
DETERMINATION OF RATE OF CORROSION OF MILD STEEL IN THE
PRESENCE AND ABSENCE OF INHIBITOR.
AIM: To determine the rate of the corrosion of mild steel in the presence and absence of Inhibitor.
Chemicals: HCl solution, Hexamethylene Diamine, Iron samples
Apparatus: Beaker, weighing machine, emery paper, dryer
Theory:
The process of decay of metal by environmental attack is called corrosion (or) the process of deterioration
and consequent loss of metallic material through unwanted chemical or electrochemical attack by its
environment.
In India, most of the machinery of Industry and railways are equipped with steel of different composition,
among all mild steel is of prominent use.
The corrosion is due to the formation of anodic and cathodic area between which current flows through
the conducting solution. The anodic reaction involves dissolution of metal as corresponding metallic ions
with the liberation of free electrons. At anode: M →M n+
+ne- (oxidation) On the contrary, the cathodic
reaction consumes electrons with either by (i) Evolution of Hydrogen or (ii) Absorption of oxygen,
depending upon the nature of corrosive environment
Evolution of Hydrogen Electrochemical corrosion occurs with evolution of H2 in acidic Environment
At anode: Fe →Fe2+ + 2e-(oxidation)
At cathode: 2H+ + 2e -→H2(reduction)
Overall reaction: Fe +2H+ →Fe2+ 2H2O+O2

4Fe2++ 8OH- --------- 4Fe(OH)2 - ---------- ----4 4Fe(OH)3------- 2Fe2 O3. 3H2O (rust)
Inhibitors are chemical substances which when added to corrosive environment reduce corrosion rates to a
considerable extent. The use of inhibitors has become the most widely used technique of combating
corrosion of metals by using amines, aldehydes, and sulphur compounds. Inhibitors are mainly classified
according to the chemical composition and structure. Most of the compounds or species used as inhibitors
are organic and inorganic. Therefore, in the present investigation the corrosion of mild steel wil be studied
in the absence and presence of inhibitors at room temperature.
Procedure:
1. Take 4 samples of iron and prepare them by polishing the surface with emery paper to remove
oxide layer
2. Mark the area 1 sq.inch to be exposed to the environment and measure the initial weight of the
sample
32
 3. Take 1M hydrochloric acid and dilute to different concentrations
4. Take 4 beakers and fill each beaker with different concentration as 0.25M, 0.5M HCl solution.
5. Dip the 2 iron samples in each beaker with different concentration of HCl (without inhibitor) and
keep them for 30 minutes.
6. Dip the 2 iron samples in each beaker with different concentration of HCl solution containing
inhibitor for 30 minutes.
7. After the required time of immersion take out the samples and wash them and dry them.
8. After drying take the final weights and find out weight loss by following principle
mm/year = 87.6 ∆W/DAT
∆W= loss of weight
D= Density gr/cc
A=Area exposed sq.cm
T=Time exposed in min
Table: Calculation of rate of corrosion
Table:
S.no HCl conc. Area of Initial wt. Final wt Loss of wt. mm/year
specimen W1 W2. ∆W
Sq.inch
1 0.25
2 0.5
3 0.25(i)
4 0.5(i)

*i=inhibitor
Result:
1. Rate of corrosion of first specimen without inhibitor =---------------mm/yr
2. Rate of corrosion of first specimen with inhibitor =---------------mm/yr
Viva questions
1. Define corrosion.
2. Define electrochemical corrosion give with suitable examples
3. What are the differences between chemical and electrochemical corrosion?
4. Why does corrosion of water filled steel tanks occur below the water line?
5. How the corrosion is controlled by cathodic protection?
33
 6. Define corrosion inhibitors. Give an example for each.
7. Why impure metal corrodes faster than pure metal on identical conditions?
8. Corrosion occurs in steel pipe connected to copper plumbing. Explain.
9. Small anodic area results in intense corrosion. Explain.
10. Rusting of iron is quicker in saline water than in ordinary water. Explain.

REFERENCEBOOKS:
1. Lab manual for Engineering chemistry by B.Ramadevi and P.Aparna -S Chand
Publications, NewDelhi (2022)
2. Vogel’s textbook of practical organic chemistry -5th edition
3. Inorganic Quantitative analysis by A.I.Vogel –ELBS Publications.
4. College Practical Chemistry byV.K. Ahluwalia – Narosa Publications Ltd., NewDelhi (2007).

34