ENGINEERING CHEMISTRY

LABORATORY MANUAL-I & II

For Students of First Year B.Tech
(Common to All Branches)

As Per the Kerala Technological University Syllabus

Compiled by
Dr. Tom Cherian,M.Sc., Ph.D.,
Assistant Professor, Department of Chemistry,
Christ College ,Iringlakuda
Mr. Shijith Thomas,M.Sc, M.Phil
Assistant Professor, Department of Chemistry,
VimalJyothi Engineering College, Chemperi
Mob:9847151817 ,Email:shijiththomas@vjec.ac.in
Mrs. Soumya John, M.Sc, B.Ed
Assistant Professor, Department of Chemistry,
VimalJyothi Engineering College, Chemperi

Designed by
NIMEESH THOMAS
Dept. of Applied Science & Humanities
Vimal Jyothi Engineering College, Chemperi
 LABORATORY MANUAL OF ENGINEERING
CHEMISTRY

FOR FIRST YEAR B.Tech. DEGREE COURSES

(Common for All Batches)

Name: _____________________________________________________________

Branch: ____________________________________________________________

Roll No: _________________________________________________________

University Reg. No: __________________________________________________

certificate

Certified that this is the record of the work done in the Engineering
Chemistry laboratory of Vimal Jyothi Engineering college, Chemperi
By Mr. /Ms. ……………………………………………during the
year………

Date: __ /___ /20__

Place: CHEMPERI

Staff in charge Internal Examiner

Mr. Nimeesh Thomas Mr. Shijith Thomas
Ms. Soumya John
 GENERAL INSTRUCTIONS

 Be punctual. Bring manual, record notebook, calculator etc.

 Maintain discipline and cleanliness in the laboratory.
 Handle the apparatus and reagent bottles with almost care.
 Report, breakage of glass wares to the laboratory Assistant
Immediately.
 Keep the reagent bottles in their respective places after use.
 Do not misplace the stoppers of the bottle.
 Do not throw waste paper, match - stick, broken glass wares
etc. Inside the sink; put them into the dust bin.
 Do not discharge concentrated acid into the sink, dilute it
before discharging.
 In case of accident, inform the faculty immediately.
 Before taking any liquid in the burette or the pipette, these
should be rinsed with the liquid.
 The conical flask should not be rinsed with any liquid It
should simply be washed with distilled water.
 Read the lower meniscus in case of colorless liquids and the
upper one in the case of colored liquids.
 The solution should be filled in the burette by means of a
funnel which must be removed before titration.
 The readings should be entered immediately in the practical
note-Book and not on some piece of paper.
 When the experimental is over, wash all the glass wares and
handover to the laboratory assistant before you leave the lab.
 Course Outcome
After the completion of Engineering chemistry Lab Syllabus, the
students will be able to attain the following qualities.
Students are able to estimate the
Exp.
CO1 impurities present in water.
1,12,13,4,5
Ability to select fuels for various
CO2 purposes. Exp. 7,13

Ability to prepare advanced polymer

CO3 materials. Exp. 6

Helps to Analyze potential of

unknown solution by Potentiometric
CO4 Exp. 14
titration.

Able to measure Conductivity of salt

CO5 solution by conductometry. Exp. 15

Ability to analyze spectra of unknown

Exp.
CO6 compounds by spectrophotometry.
10,11,16,2,3
 PERIODIC TABLE
The periodic table of the chemical elements (also known as the periodic
table or periodic table of the elements) is a tabular display of the118 known
chemical elements organized by selected properties of their atomic structures.
Elements are presented by increasing atomic number, the number of protons
in an atom’s atomic nucleus. While rectangular in general outline, gaps are
included in the horizontal rows (known as periods) as needed to keep elements
with similar properties together in vertical columns (known as groups), e.g.
alkali metals, alkali earths, halogens, noble gas.
 IMPORTANT TERMS IN VOLUMETRIC
ANALYSIS
TITRATION
The process of finding out the volume of one of the solutions required
to react completely with the definite volume of other solution.
TITRANT
The Solution of known strength.
TITRATE
The solution which contains a substance whose strength is to be
estimated.
INDICATOR
The substance which indicates the end point of titration is called
indicator. The indicator indicates the completion of reaction by change
in colour at the end point. e.g.: Phenolphthalein for acid base titration.
STRENGTH
The amount of substance dissolved in one litre of a solution expressed as
strength of a solution. Strength of solution can also be expressed in any
of the following ways.
 Normality:
It is the number of gram equivalents of the substance
dissolved per litre of the solution. It is denoted by N.

 Molarity:
It is the number of moles of solute per litre of the solution.
It is denoted by M.

 Molality:
It is the number of moles of the substance dissolved in
1000gm or 1kg of the solvent. It is denoted by m.
  Percentage by weight:
It is the weight in grams of a solute present in 100gms of the
solution.
 Equivalent Weight:
The equivalent weight of a substance is defined as the number of parts
by weight of it that combines with or displaces one part by weight of
hydrogen or eight parts by weight of oxygen.

 Basicity
It is the number of replaceable hydrogen atoms in an acid.
 Acidity
It is the number of replaceable OH groups in one molecule of a base.
 Standard Solution
A solution of known concentration is known as standard solution.
 Equivalent weights of Substances:
Substances Equivalent Weight
Sodium hydroxide 40
Sodium thiosulphate 248.19
Potassium dichromate 49.03
Potassium permanganate 31.6
Hydrochloric acid 36.46
Sulphuric acid 49.04
Nitric acid 63
Acetic acid 60
 CYL ENGINEERING CHEMISTRY LAB CATEGORY L T P CREDIT
120 BSC 0 0 2 1

Preamble: To impart scientific approach and to familiarize with the experiments in chemistry relevant
for research projects in higher semesters

Prerequisite: Experiments in chemistry introduced at the plus two levels in schools

Course outcomes: After the completion of the course the students will be able to

CO 1 Understand and practice different techniques of quantitative chemical analysis to

generate experimental skills and apply these skills to various analyses

CO 2 Develop skills relevant to synthesize organic polymers and acquire the practical skill to
use TLC for the identification of drugs
CO 3 Develop the ability to understand and explain the use of modern spectroscopic
techniques for analysing and interpreting the IR spectra and NMR spectra of some
organic compounds
CO 4 Acquire the ability to understand, explain and use instrumental techniques for chemical
analysis
CO 5 Learn to design and carry out scientific experiments as well as accurately record and
analyze the results of such experiments

CO 6 Function as a member of a team, communicate effectively and engage in further

learning. Also understand how chemistry addresses social, economical and
environmental problems and why it is an integral part of curriculum

Mapping of course outcomes with program outcomes

PO 1 PO 2 PO 3 PO 4 PO 5 PO 6 PO 7 PO 8 PO 9 PO PO PO
10 11 12
CO 1 3 2 3
CO 2 3 3 3
CO 3 3 3 3
CO 4 3 3 3
CO 5 3 1 3
CO 6 3 1 3
Mark distribution

Total Marks CIE ESE ESE

marks marks Duration(Internal)

100 100 - 1 hour

Experiments in Engineering Chemistry Vimal Jyothi Engineering College

SYLLABUS

LIST OF EXPERIMENTS (MINIMUM 8 MANDATORY)

1. Estimation of total hardness of water-EDTA method

2. Potentiometric titration
3. Determination of cell constant and conductance of solutions.
4. Calibration of pH meter and determination of pH of a solution
5. Estimation of chloride in water
6. Identification of drugs using TLC
7. Determination of wavelength of absorption maximum and colorimetric estimation of Fe3+ in
solution
8. Determination of molar absorptivity of a compound (KMnO4 or any water soluble food
colorant)
9. Synthesis of polymers (a) Urea-formaldehyde resin (b) Phenol-formaldehyde resin
10. Estimation of iron in iron ore
11. Estimation of copper in brass
12. Estimation of dissolved oxygen by Winkler’s method
13. (a) Analysis of IR spectra (minimum 3 spectra) (b) Analysis of 1H NMR spectra (
minimum 3 spectra)
14. Flame photometric estimation of Na+ to find out the salinity in sand
15. Determination of acid value of a vegetable oil
16. Determination of saponification of a vegetable oil
Reference Books

1. G. Svehla, B. Sivasankar, “Vogel's Qualitative Inorganic Analysis”, Pearson, 2012.

2. R. K. Mohapatra, “Engineering Chemistry with Laboratory Experiments”, PHI Learning, 2017.

3. Muhammed Arif, “Engineering Chemistry Lab Manual”, Owl publishers, 2019.

4. Ahad J., “Engineering Chemistry Lab manual”, Jai Publications, 2019.

5. Roy K Varghese, “Engineering Chemistry Laboratory Manual”, Crownplus Publishers, 2019.

6. Soney C George, Rino Laly Jose, “Lab Manual of Engineering Chemistry”, S. Chand & Company
Pvt Ltd, New Delhi, 2019.

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Experiments in Engineering Chemistry Vimal Jyothi Engineering College

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Experiments in Engineering Chemistry Vimal Jyothi Engineering College

INDEX

Sl.N Staff
o Date Name of experiment Marks Initial

1 To determine pH value of solution by pH meter.

2 Estimation of Total Hardness – EDTA method.

3 Potentiometric titration Acid-Base titration.

Conductivity measurements of salt solution

4
conductometry.

5 Preparation of Urea formaldehyde resin.

Estimation of dissolved oxygen by Winkler’s

6
method.
Flame photometric estimation of Na+ to find out
7
the salinity in sand
Determination of chloride ion in a given water
8
sample by Argentometric method (Mohr’s Method)

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Experiments in Engineering Chemistry Vimal Jyothi Engineering College
(a) Standardization of EDTA solution with standard hard water

Volume of standard Burette Readings in ml Volume of

SL.No
hard water in ml Initial Final EDTA solution in ml
1

4
Concordant Volume of EDTA solution, V 1 =………ml

(b) Estimation of Total Hardness of given water sample

Volume of given Burette Readings in ml Volume of

SL.No
water sample in ml Initial Final EDTA solution in ml
1

Concordant Volume of EDTA solution, V2 =……… ml

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Experiments in Engineering Chemistry Vimal Jyothi Engineering College

Experiment No: Date:

ESTIMATION OF TOTAL HARDNESS BY EDTA

METHOD
AIM
Estimation of hardness of water by EDTA method
APPARATUS
Burette, Pipette, beakers, Standard flask, Conical flask
CHEMICALS
0.1 M EDTA, Eriochrome, Black-T, water sample, buffer solution.
THEORY
Estimation of hardness by EDTA method is based on the following principles.
First, the indicator Eriochrome Black-T, which is a blue colored dye, forms an
unstable complex with calcium or Magnesium ions in hard water at pH of 9 to
10. The complex is wine red in color.
Mg 2 / Ca 2  Eriochrome Black-T  [Mg/Ca—Eriochrome black-T)
Unstable Complex (Wine Red)
As this solution is titrated against EDTA, the free Ca 2 and Mg 2 ions in water
from stable metal ion
EDTA  [Mg/Ca-EDTA] Stable Complex. ( Colourless )
Once the free metal ions are complexed, the EDTA replaces Ca and Mg ions
from the unstable indicator complex also, to form a stable complex, with the
result, the indicator is set free. Since the free indicator is blue in colour at the
above-mentioned pH, the end point is the appearance of blue color
[Mg/Ca-Eriochrome Black-T] +EDTA  [Mg/Ca-EDTA] + Eriochrome
Black-T(Blue)
The temporary hardness is removed by boiling and after the removal of
precipitate by filtration; the permanent hardness in the filtrate is determined by
titration with EDTA as above.
PROCEDURE
(a) Standardization of EDTA solution with standard hard water
Pipette out 20 ml of standard hard water in a washed conical flask. Add 5ml
basic buffer solution and 2-3 drops of Eriochrome Black-T indicator, the
colour of the solution turns wine red.

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Experiments in Engineering Chemistry Vimal Jyothi Engineering College

QUESTIONS
1. What is Hardness?
2. What are the differences between temporary and permanent Hardness?
3. How will you remove permanent Hardness?
4. Why does hard water consumes a lot of soap?
5. If the water contains Ca2+ and HCO3- will it be hard or soft Water. Give
reason

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Experiments in Engineering Chemistry Vimal Jyothi Engineering College

Titrate this solution against EDTA solution taken in the burette until the
colour changes from wine red to clear blue at the end. The final reading of
the burette is noted, and the titration is repeated to get concordant value.

(b) Estimation of Total Hardness of given water sample

Pipette out 20 ml of given hard water in a washed conical flask. Add

5ml basic buffer solution and 2-3 drops of Eriochrome Black-T indicator, the
colour of the solution turns wine red. Titrate this solution against EDTA
solution taken in the burette until the colour changes from wine red to clear
blue at the end. The final reading of the burette is noted, and the titration is
repeated to get concordant value

RESULT
The Total hardness of water = ppm

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Experiments in Engineering Chemistry Vimal Jyothi Engineering College

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Experiments in Engineering Chemistry Vimal Jyothi Engineering College

MARKS

SCORING
0.5 1 1.5 2
AVERAGE SATISFACTORY GOOD VERYGOOD TOTAL
CRITERIA
ACCURACY OF
RESULT
NEATNESS
PUNCTUALITY
OVER ALL
PERFORMANCE
VIVA VOCE
TOTAL MARK

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Experiments in Engineering Chemistry Vimal Jyothi Engineering College

Observations and Calculations

Titration with the Blank solution

Burette Readings in ml Volume of AgNO3
S.No Volume of distilled water in ml
initial Final Solution in ml

Concordant Volume of AgNO3 solution, V1 =………ml

Titration with the Sample Water

Burette Readings in ml Volume of
Volume of given water sample
Sl..No AgNO3
in ml Initial Final Solution in ml
1

3
Concordant Volume of AgNO3 solution, V2 =………
Normality of standard AgNO3 solution, NA = 0.014N
Volume of standard AgNO3 solution, VA = (V2-V1)

= ……………ml
Volume of given water sample, VW = …………… ml

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Experiments in Engineering Chemistry Vimal Jyothi Engineering College
Experiment No: Date:

DETERMINATION OF CHLORIDE ION IN A

GIVEN WATER SAMPLE BY ARGENTOMETRIC
METHOD (MOHR’S METHOD)
AIM
To determine the chloride ion of a given water sample by
Argentometric method (Mohr’s method)
APPARATUS
Conical flask, Burette, Measuring flask, Beakers
REAGENTS
Standard silver nitrate solution (0.014N), Indicator potassium chromate
solution.
THEORY
Chlorides are present in water usually as NaCl, MgCl2 and CaCl2.
Although chlorides are not harmful as such, their concentrations over 250
ppm impart a peculiar taste to the water thus rendering the water unacceptable
for drinking purposes. By argentometric method, chloride ions in a water
sample (neutral or slightly alkaline) can be determined by titrating it against
standard silver nitrate (AgNO3) solution using potassium chromate (K2CrO4)
as an indicator. The pH should be in between 7-8. At higher pH, silver ions
are precipitated as silver hydroxide. At lower pH, potassium chromate
indicator is converted to potassium dichromate (K2Cr2O7).
Argentometric method is based on the precipitation titration in which
silver nitrate solution is released from the burette to the water sample which
contains chloride ions and indicator. The silver ions (from silver nitrate
solution) react with chloride ions (from water sample) and chromate ions
(from indicator) to form white precipitate of silver chloride and red
precipitate of silver chromate.
Ag+ +Cl- ⟶ AgCl (White precipitate)
2Ag++CrO2-4⟶Ag2CrO4 (Red precipitate)
Red colour formed because of formation of silver chromate disappears
initially as the solution contains high concentration of chloride ions.
Ag2CrO4+ 2Cl- ⟶ 2AgCl +CrO2-4
When the concentration of chloride ions has decreased, the red colour

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Experiments in Engineering Chemistry Vimal Jyothi Engineering College
Normality of given water sample, NW can be calculated from the normality
formula i.e., NA x VA = NW x VW
×
Normality of given water sample, NW=
. ×
=
Amount of chloride ions = NW x Eq.wt.Of chlorine = NW x 35.45 g/Lit
= ……………..g/Lit
Amount of chloride ions in ppm = ………….× 1000 mg/Lit
= ………………..ppm

QUESTION’S
1. What do you mean by argentometric titrations?

2. What is redox titration?

3. Write a note on different type of indicators?

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

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Experiments in Engineering Chemistry Vimal Jyothi Engineering College
Starts disappearing slowly and slowly on shaking and a stage is reached when
all the chloride ions have formed silver chloride. One extra drop of silver
nitrate at this point reacts with potassium chromate and reddish coloured
silver chromate is formed.
2AgNO3+ K2CrO4⟶ Ag2CrO4+2KNO3
PROCEDURE
TITRATION WITH THE BLANK SOLUTION
Transfer 10 ml of the distilled water in a conical flask and add 3-4 drops of
indicator potassium chromate solution. Slowly add standard silver nitrate
solution from the burette and shake the solution well. At the end point, light
yellow colour starts changing to red colour. The titration is repeated until a
concordant volume V1 is obtained. The blank correction for the indicator
should be subtracted from the volume of the titrant obtained after titrating the
sample solution as given below
TITRATION WITH THE SAMPLE WATER
Transfer 10 ml of the given water sample in a conical flask and add 3-4 drops
of indicator potassium chromate solution. Slowly add standard silver nitrate
solution from the burette and shake the solution well. At the end point, light
yellow colour starts changing to red colour and red colour persists. The
titration is repeated until a concordant volume V2 is obtained.
RESULT
The amount of chloride ion in the given water sample is…………..

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Experiments in Engineering Chemistry Vimal Jyothi Engineering College

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Experiments in Engineering Chemistry Vimal Jyothi Engineering College

MARKS

SCORING
0.5 1 1.5 2
AVERAGE SATISFACTORY GOOD VERYGOOD TOTAL
CRITERIA
ACCURACY OF
RESULT
NEATNESS
PUNCTUALITY
OVER ALL
PERFORMANCE
VIVA VOCE
TOTAL MARK

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Experiments in Engineering Chemistry Vimal Jyothi Engineering College

OBSERVATIONS AND CALCULATIONS

Standardisation of thiosulphate solution
Standard dichromate solution X thiosulphate solution
Indicator: starch

Volume of std. dichromate solution, V1 = 20 mL

Volume of thiosulphate solution, V2 = …………….mL
Normality of K2Cr2O7 solution N1 = ………………..
At the end point
No. of equivalents of dichromate = No. of equivalents of thiosulphate solution
ie., V1N1 = V2N2
Vol. water sample, V1 = 125 mL
Vol. of thiosulphate solution, V2 = ………………….. mL
Volume of Burette Readings in ml Volume of
std.dichromate solution Thiosulphate
SL.No ( V2 mL)
( V1 mL) Initial Final
1 20

2 20

No. of equivalents of Dissolved oxygen = No. of equivalents of thiosulphate

solution
ie., V1N1 = V2N2
Normality of Water sample, N1 = = ……………………
Weight of oxygen per litre = Normality x Eq. wt. of O2
= N1 x 8 g/L
= N1 x 8 x 1000 mg/L or ppm = …………………………..
Amount of dissolved oxygen in the given water sample = ………………………… ppm

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Experiments in Engineering Chemistry Vimal Jyothi Engineering College
Experiment No: Date:

DETERMINATION OF DISSOLVED OXYGEN IN

WATER SAMPLE BY WINKLER’S METHOD

AIM
To determine the dissolved oxygen in the given sample of water, being
provided with thiosulphate solution approximate normality 0.01 and A.R
K2Cr2O7 crystals.
PRINCIPLE
Dissolved oxygen present in water can oxidize I- from KI to Iodine(I2). The
liberated iodine can be titrated against Na2S2O3 solution using starch as
indicator. Here MnSO4 in alkaline medium is used to bring about the reaction
between KI and dissolved O2 indirectly.
MnSO4 + KOH Mn(OH)2 (s) + K2SO4
2Mn(OH)2 + O2 2MnO(OH)2

The above reaction is called O2 fixing step and it takes about 15 minutes.
After fixing O2 the medium is made acidic so that MnO(OH)2 can oxidize I-
from KI to Iodine(I2)
2 I- I2 + 2e-

The liberated iodine is then titrated with standard thiosulphate solution

I2 + 2e- 2 I- E0 = +0.54V (1)
S4O6 2- + 2e- 2S2O3 2- E0 = +0.09V (2)

(1) - (2) gives

I2 + 2S2O3 2- S4 O6 2-

PROCEDURE
Standardization of thiosulphate solution: 20 mL of standard dichromate
solution (about 0.01N) is pipetted into a conical flask, add about 5 mL 5% KI
solution and 3 mL con. HCl and titrated against thiosulphate solution taken
in the burette. When the solution becomes pale yellow add 4 drops of freshly

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Experiments in Engineering Chemistry Vimal Jyothi Engineering College

QUESTION
1. What is the role of buffer solution?
2. Why estimation of dissolved oxygen is of great significance?
3. What is the role of KI used in estimation?
4. Complete the reaction Mn (SO4)2 + 2KI
5. What is the amount of dissolved oxygen present in pure water?
6. What is BOD? Explain it?

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Experiments in Engineering Chemistry Vimal Jyothi Engineering College
prepared starch solution, then the solution becomes blue in colour. The
titration is continued by adding thiosulphate solution drop by drop till the
blue colour disappears.
Estimation of dissolved oxygen in water: Take a 125 mL glass bottle
having air tight stopper. Fill the bottle completely with water without
bubbling. 1mL MnSO4 solution and 1 mL alkaline KI solution are introduced
at the bottom using a graduated pipette. Close the lid without leaving any air
bubble and shaken vigorously and allowed to stand for about 15 minutes. The
precipitate formed gets settled at the bottom. Add 2mL 1:1 sulphuric acid
from the top using a graduated pipette. Close the lid and shaken well till all
precipitate get dissolved. The solution is then transferred to a 250 mL conical
flask and titrated against standard thiosulphate solution taken in the burette
using starch as indicator. Note the temperature of water sample before
collecting into the glass bottle, since the amount dissolved oxygen in water
is a function of temperature.
Result: The amount of dissolved oxygen in the given water sample at
…….C0 =…………………………..ppm

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Experiments in Engineering Chemistry Vimal Jyothi Engineering College

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Experiments in Engineering Chemistry Vimal Jyothi Engineering College
MARKS
SCORING 0.5 1 1.5 2
CRITERIA AVERAGE SATISFACTORY GOOD VERYGOOD TOTAL
ACCURACY OF
RESULT
NEATNESS
PUNCTUALITY
OVERALL
PERFOMANCE
VIVA VOCE
TOTAL MARK

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Experiments in Engineering Chemistry Vimal Jyothi Engineering College

Observations and Calculations

Titration with the Blank solutionObservations and Calculations

Volume of given Burette Readings in ml

Volume of
Sl.No bleaching powder
Initial Final Na2S2O3 solution in ml
solution in ml

Concordant Volume of Na2S2O3 solution, V1 =………ml

Normality of standard Na2S2O3 solution, N1 = 0.025N

Volume of standard Na2S2O3 solution, V1 = ……………ml
Volume of given bleaching powder solution, V2 = ………….....ml
Normality of given water sample, N2 can be calculated from the normality
formula,
i.e., N1 x V1 = N2 x V2
×
Normality of given bleaching powder solution, N2 =

=……………………N
Amount of available chlorine=N2×35.45
= ………………..g/Lit
Amount of available chlorine present in 100 ml other solution
..…..×
= 𝑔
= ………………..g

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Experiments in Engineering Chemistry Vimal Jyothi Engineering College

Experiment No: Date:

DETERMINATION OF THE PERCENTAGE OF

AVAILABLECHLORINE PRESENT IN BLEACHING
POWDER SAMPLE

AIM
Determine the percentage of available chlorine present in the given sample
of bleaching powder.
THEORY
Bleaching powder is used as a bleaching agent and also as a disinfectant.
The main constituent of bleaching powder is calcium hypochlorite
[Ca(OCl)2] which supplies
chlorine [Cl2] with dilute acids.
Ca(OCl)2+4HCl ⟶CaCl2 +2H2O + 2Cl2
So the available chlorine is defined as the percentage of chlorine made
available by bleaching powder when treated with dilute acids. The available
chlorine present in bleaching powder sample is determined iodometrically by
treating its solution with an excess of potassium iodide solution in the acidic
medium.
ClO- + 2H+ +2I-⟶ I2 +H2O +Cl-
The liberated iodine (I2) is treated with sodium thiosulphate (Na2S2O3)
solution using freshly prepared starch solution as indicator to be added near
the end point.
(Starch +I2⟶ Blue coloured complex)
I2+2Na2S2O3⟶Na2S4O6=2NaI
APPARATUS
Digital Balance, Burette, Conical flask, Measuring flask, Funnel, Glass rod,
Beakers
REAGENTS
Bleaching powder, Standard sodium thiosulphate solution 10% Potassium
iodide (KI) solution, dilute acetic acid, freshly prepared starch solution as
indicator

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Experiments in Engineering Chemistry Vimal Jyothi Engineering College
QUESTIONS
1.what is the common name of this compound CaCOCl2?
2.What happens when bleaching powder is left exposed to air?
3.write about the uses of bleaching powder?

36
Experiments in Engineering Chemistry Vimal Jyothi Engineering College
PROCEDURE

………….g of bleaching powder is accurately weighed in a weighing bottle.

It is transferred to a clean beaker and is ground to a thin paste with water. The
mixture is allowed to settle, and the milky supernatant liquid poured into a
100 ml standard flask. The residue in the beakers ground with a little more
water and the operation repeated until the whole of the sample has been
quantitatively transferred into the standard flask.
Then the solution is made up to the volume. The flask is shaken well
for uniform concentration. 25 ml of the solution (use measuring flask) in a
state of very fine suspension is taken into a conical flask and add 10 ml of
distilled water into it. Then add 10 ml of 10% potassium iodide (KI) solution
and 10 ml of dilute acetic acid. This solution [which contains liberated iodine
(I2)] titrates with standard sodium thiosulphate solution (taken in the burette)
until the dark brown colour changes to pale yellow. To this add, 2 ml of
freshly prepared starch solution as indicator, so the colour of the solution
turned into blue. Continue the titration till the disappearance of blue colour
of the solution and note down the volume of the titrant used. The titration is
repeated until a concordant volume is obtained.
RESULT
Amount of available chlorine present in the given sample of bleaching powder
is………….g

MARKS

SCORING 0.5 1 1.5 2

CRITERIA AVERAGE SATISFACTORY GOOD VERYGOOD TOTAL

ACCURACY OF
RESULT
NEATNESS
PUNCTUALITY
OVERALL
PERFORMANCE
VIVA VOCE
TOTAL
MARK

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Experiments in Engineering Chemistry Vimal Jyothi Engineering College
(a) Standardization of KMnO4 solution with standard Mohr’s salt solution

Volume of standard Burette Readings in ml Volume of

S.No
Mohr’s salt in ml, V 1 Initial Final KMnO4 solution in
ml
1
2
3
4
Concordant Volume of KMnO4solution, V2
=………ml

(b) Estimation of iron in the given iron ore/alloy

Volume of given
Burette Readings in ml Volume of
S.No solution
of iron ore/alloy in ml Initial Final KMnO4 solution in ml

1
2
3
4
Concordant Volume of KMnO4 solution, V2a
=………ml
By law of equivalence, N1V1=N2V2
N2= N1V1
V2

For estimation N3V3=N2V2a

N3=N2V2a
V3
∴Amount of ferrous iron present in the given solution =

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Experiments in Engineering Chemistry Vimal Jyothi Engineering College

Experiment No: Date:

ESTIMATION OF Fe IN Fe ORE

AIM
Estimation of ferrous iron in a given 100 ml of ore solution by titration against
a standard of potassium permanganate
APPARATUS
Pipette, Burette, Conical flask, Measuring jar, Standard flask
CHEMICALS
KMnO4 , Mohr’s salt ,Sulphuric acid(1:1)
THEORY
The Potassium permanganate is a powerful oxidizing agent has the formula
Kmno4 in which Manganese is in +7 oxidation state and Mohr’s salt with
the formulafeso4(NH4)2 SO4. 6H2O in which Iron (II) is acts as a
reducing agent. These two reacts in presence of sulphuric acid medium as
follows. In this reaction
Mn+7 is reduced to Mn+2 and Fe+2 is oxidized to Fe+3 agent has the
formula
2KMnO4 + 3 H2SO4 K2SO4 + 2MnSO4 + 3H2O + 5 (O)
10 FeSO4 + 5H2SO4 + 5 (O) 5 Fe2(SO4)3 + 5H2O
2KMnO4 + 10 FeSO4 + 8 H2SO4 K2SO4 + 2MnSO4 +5Fe2(SO4)3 + 8H2O
According to this one mole of potassium permanganate is reacting with five
moles of Iron (II). In this all the reactants and products are colourless except
potassium permanganate. So the colour of the permanganate is used to locate
the end point. When once all the Fe(II) ions are completely reacted the excess
trace amount of potassium permanganate can give sufficient colour to the
solution i.e. colour change at the end point is colourless to pale pink.
Potassium permanganate acts as a self-indicator, so it is called self-indictor
reaction.
PROCEDURE
(a) Standardization of potassium permanganate solution
Pipette out 20 ml of the N/20 standard Mohr’s salt solution into a conical

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Experiments in Engineering Chemistry Vimal Jyothi Engineering College
QUESTIONS
1. Give the characteristics of transition metal halide?
2. How we can extract iron from its ore?
3. What is normality?
4. Why this type of estimation is called self-indicator method?
5. Which are the terms used to denote the concentration of solution?
6. Define partial pressure?
7. Give the general steps in metallurgy?

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Experiments in Engineering Chemistry Vimal Jyothi Engineering College
flask and add 10 ml of dilute sulphuric acid. Then, titrate this solution
slowly against the potassium permanganate solution from the burette until a
faint but permanent pink colour persists in the solution. Note down the
volume of the titrant used. Repeat the titrations until a concordant volume is
obtained.

(b) Estimation of Iron in the given ore/alloy

The whole of the given iron ore/alloy solution is transferred into the 100
ml standard flask. Make up the volume of the solution to 100 ml with
distilled water and shake the solution thoroughly. Pipette out 20 ml of the
solution into a conical flask, add 10 ml of dilute sulphuric acid and titrate
against the potassium permanganate solution taken in the burette. The
appearance of a faint but permanent pink colour marks the end point. Note
down the volume of the titrant used. Repeat the titrations until a concordant
volume is obtained.

REPORT
The amount of ferrous iron present in the given 100ml. unknown
Solution is = g

MARKS

SCORING 0.5 1 1.5 2

CRITERIA AVERAGE SATISFACTORY GOOD VERYGOOD TOTAL
ACCURACY OF
RESULT
NEATNESS
PUNCTUALITY
OVERALL
PERFORMANCE
VIVA VOCE
TOTAL MARK

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Experiments in Engineering Chemistry Vimal Jyothi Engineering College
QUESTIONS
1what is thermosetting resin?
2. Mention a few applications of urea-formaldehyde resin.
3. What is high polymer?

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Experiments in Engineering Chemistry Vimal Jyothi Engineering College
Experiment No: Date:
PREPARATION OF UREA-FORMALDEHYDE RESIN

AIM
To prepare urea-formaldehyde (UF) resin
THEORY
Urea-formaldehyde resin is prepared by the condensation polymerisation
reaction between urea and formaldehyde in neutral or acidic condition. Such
resins are water soluble and hence are used as textile finishing. They are also
used in the paper industry to improve the wet strength of paper. In the
plywood industry they are used as adhesives. Such resins find uses in
packaging, accessories, unbreakable dishes, clock cases, etc.
PROCEDURE
Place 10 ml of 40% formaldehyde solution in a beaker. Add about 5g of urea
while stirring until a saturated solution is obtained. Add a few drops of
concentrated sulphuric acid stirring cautiously during the addition. All of a
sudden, a voluminous white solid mass appears in the beaker. When the
reaction is complete, wash the residue with water and dry the product and
determine the yield of the product.

RESULT
The yield of the urea-formaldehyde (UF) resin is…………………g
MARKS

SCORING 0.5 1 1.5 2

CRITERIA AVERAGE SATISFACTORY GOOD VERYGOOD TOTAL
ACCURACY OF
RESULT
NEATNESS
PUNCTUALITY
OVERALL
PERFORMANCE
VIVA VOCE
TOTAL MARK

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Experiments in Engineering Chemistry Vimal Jyothi Engineering College
QUESTIONS
1. Define flash point and fire point of lubricating oil.
2. What should be the flash point of a good lubricant?
3. In Pensky Martin’s apparatus what is the purpose of air jacket
surrounding the oil cup.?
4. What are the factors affecting the flash point and fire point?

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Experiments in Engineering Chemistry Vimal Jyothi Engineering College
Experiment No: Date:

DETERMINATION OF FLASH POINT AND FIRE POINT

OF OIL BY PENSKY MARTIN APPARATUS

AIM
To determine flash point and fire point of the given lubricating oil using
Pensky Marten’s apparatus.
CHEMICALS USED
Given lubricating oil, suitable organic solvent like CCl4, ether, petroleum
spirit or benzene
APPARATUS REQUIRED
Pensky Marten’s flash and fire point apparatus, match box, thermometer,
filter paper
PRINCIPLE
Flash point is the lowest temperature at which the lubricating oil gives off
enough vapours that ignite for a moment when tiny flame is brought near it.
Fire point is the lowest temperature at which the vapours of the oil burn
continuously for at least five seconds when a tiny flame is brought near it.
PROCEDURE
Clean and dry all parts of the apparatus with the help of suitable solvent e.g.
CCl4, ether, petroleum spirit or benzene and dry it to remove any traces of
solvent.
Fill the oil cup with the test oil up to the mark. Fix the lids on the top through
which are inserted a thermometer and a stirrer. Ensure that the flame exposure
device is fixed on the top. Light the test flame and adjust it to about 4 mm in
diameter. Heat apparatus as temp. of oil increases by 5 to 60 per min. as stirrer
is continuously rotated. At every 10 C rise of temp. Introduce test flame into
the oil vapour. This is done by operating the shutter. On moving knob of
shutter, test flame is lowered in oil vapours through opening. When test flame
causes a distinct flame in interior cup, note temp. which represent the flash
point. Further heat the oil at the rate of 10C/ min. and continue applying the
test flame as before. The temperature at which the vapours of the oil give a
clear and distinct blue flash for five seconds is recorded as the fire point of
the oil.

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Experiments in Engineering Chemistry Vimal Jyothi Engineering College

RESULT
The flash point of given oil sample=___ C.

The fire point of given oil sample=____ C.

MARKS

SCORING 0.5 1 1.5 2

CRITERIA AVERAGE SATISFACTORY GOOD VERYGOOD TOTAL
ACCURACY OF
RESULT
NEATNESS
PUNCTUALITY
OVERALL
PERFORMANCE
VIVA VOCE
TOTAL MARK

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Experiments in Engineering Chemistry Vimal Jyothi Engineering College

Observation Table
Sl.No Solution pH of Change in Type of
Solution pH meter
Colour Reading Solution
(pH paper)

Unknown Solution-
1
1

Unknown Solution-
2
2

Unknown Solution-
3
3

QUESTION: -
1. Define the term pH value.
2. What is the pH of water?
3. Which different methods are used for determination of pH.
4. Explain the construction and working of pH electrode.

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Experiments in Engineering Chemistry Vimal Jyothi Engineering College

Experiment No: Date:

DETERMINATION OF pH VALUE

AIM
To determine pH value of solution by using pH meter & pH paper.
APPARATUS
Standard flask., Beaker, pH Meter, pH Paper, Glass Electrode etc.
CHEMICALS
Buffer solution, hydrochloric acid, sodium hydroxide etc.
THEORY
The pH value of solution is defined as negative logarithm of hydrogen ion
concentration. It is expressed in gram/ion lit.
pH = -log [H+] = log10
[ ]
AT 250 the ionic product of water
Kw = [H+] [OH-] =10-14
Also, in pure water [H+] = [OH-]
In neutral solution [H+]= [OH-]
pH of neutral solution = −𝑙𝑜𝑔 10 = 7
Consequently, PH of neutral solution is 7; in acidic solution PH<7, since
[H+]>10 on the other hand PH of the alkaline solution is >7, Since [H+]
<10
pH value of distilled water = 7
pH of the solution is tested by using pH paper. This gives different colour
with different values. pH can also be tested by using pH meter.
PROCEDURE
Dip the pH electrode in the Beaker & note down the pH. Then take another
solution in a beaker dip the electrode & note pH of solution also deep the pH
paper & observe the colour Change& note down the nature of solution. Take
the four different reading of four different solutions & Write the result either
the solution are acidic, basic or neutral.

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Experiments in Engineering Chemistry Vimal Jyothi Engineering College

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Experiments in Engineering Chemistry Vimal Jyothi Engineering College
RESULT
1.pH of first unknown solution is ------ hence the nature of solution is -------
-
2.pH of second unknown solution is ------ hence the nature of solution is ----
----
3.pH of third unknown solution is ------ hence the nature of solution is -------
-

MARKS

SCORING 0.5 1 1.5 2

CRITERIA AVERAGE SATISFACTORY GOOD VERYGOOD TOTAL
ACCURACY OF
RESULT
NEATNESS
PUNCTUALITY
OVERALL
PERFORMANCE
VIVA VOCE
TOTAL MARK

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Experiments in Engineering Chemistry Vimal Jyothi Engineering College
Observation Table
SL NO V E ΔE ΔV 𝚫𝐄
𝚫𝐕
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20

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Experiments in Engineering Chemistry Vimal Jyothi Engineering College

Experiment No: Date:

POTENTIOMETRIC TITRATIONS –REDOX TITRATION

AIM
To estimate the amount of ferrous ion present in the whole of the given
solution, you are being provided with AR K2Cr2O7
APPARATUS
Potentiometer, Pt.-electrode, Calomel electrode, Salt bridge, 150 ml beakers,
Stirrer, Pipette and Burette.
PRINCIPLE
Ferrous solution is taken in a beaker, an inert indicator electrode (platinum
foil) and a reference electrode saturated calomel electrode) are inserted to the
solution in the beaker.
Consider the reduction reaction
Fe3++ e- Fe2+ E˚= +0.77V. The potential of the indicator electrode
is
.
E = E˚ + 𝑙𝑜𝑔
When potassium dichromate solution is added from a burette to Fe2+ solution
in a beaker, the concentration of Fe3+ increases due to oxidation of Fe2+.As a
result the potential of indicator electrode increases. When the end is reached
no more Fe2+ is available for oxidation then dichromate electrode begins to
setup.
Cr2O7 2- + 14 H+ + 6e- 2Cr3++ 7H2O E˚ = +1.33 V
Cell potential shoot up rapidly with further addition of dichromate solution
after end point. In potentiometric titrations, the change in the electrode
potential upon the addition of the point, the rate of change of potential is a
maximum
PROCEDURE
Estimation of ferrous ion:
Making up to a known volume: Transfer the given ferrous sulphate solution into a
100 mL standard flask using a funnel and a glass rod. Wash the solution bottle
with water and transfer the washings to the standard flask. Repeat the washing
three times with small amount of water (about 10 mL). The solution is then made
up to the mark using pure water.
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Experiments in Engineering Chemistry Vimal Jyothi Engineering College

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Experiments in Engineering Chemistry Vimal Jyothi Engineering College

Estimation: Rinse the burette and fill the burette with potassium dichromate
solution, and note the initial burette reading. Pipette 20 mL of ferrous sulphate
solution into a 250 mL beaker. Add 20 mL 4N sulphuric acid. Insert platinum
electrode and calomel electrode in it. Connect the negative lead of the digital
multimeter with calomel electrode using a crocodile clip. The + ve lead is
connected with platinum electrode. The rotatory switch of the multimeter turned
to 2000 mV DC range. The multimeter reading directly gives the cell emf. Note
the emf for every 1 mL potassium dichromate. When the end point is reached rate
of change of emf is a maximum. Note the emf near the end point for every 0.1 mL
dichromate. Plot a graph between emf and volume of dichromate. From the graph
the end point can be determined.

RESULT
1.Endpoint from the ΔE Vs ΔV Graph = ……………..
2.Endpoint from the E Vs V Graph = ……………….
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Experiments in Engineering Chemistry Vimal Jyothi Engineering College

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Experiments in Engineering Chemistry Vimal Jyothi Engineering College
QUESTIONS
1. Basic principle of potentiometric titration.
2. What is single electrode potential?
3. What is potentiometric titration?
4. What are the advantages of potentiometric titrations?
5. Give the application of Potentiometric titrations?
6. Explain acid base Potentiometric titration.

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Experiments in Engineering Chemistry Vimal Jyothi Engineering College

MARKS

SCORING 0.5 1 1.5 2

CRITERIA AVERAGE SATISFACTORY GOOD VERYGOOD TOTAL
ACCURACY OF
RESULT
NEATNESS
PUNCTUALITY
OVERALL
PERFORMANCE
VIVA VOCE
TOTAL MARK

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Experiments in Engineering Chemistry Vimal Jyothi Engineering College
Observations and Calculation
Conductance of 0.1 M KCl solution =

.
Cell constant = = =

Conductivity of sample water =Conductance of sample water × cell constant

=…………………..

QUESTIONS
1. What is conductometry?
2. Write applications of conductometry?

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Experiments in Engineering Chemistry Vimal Jyothi Engineering College
Experiment No: Date:
MEASUREMENTS OF CONDUCTIVITY OF A SAMPLE
OF WATER

AIM
To measure the conductivity of given sample of water using a conductivity
bridge and conductivity electrode assembly. You are being provided with AR
KCl crystals

PRINCIPLE
Salinity, acidity etc. of water can be easily monitored by conductivity
measurements. Conductance is the reciprocal of resistance. The conductance
of a solution can be measured using a conductivity meter. Specific
conductance or conductivity is defined as conductance of 1 cm3 of a
conductor or solution held between two electrodes of 1 cm2 area placed on
the opposite pairs of the faces of a cube of 1 cm length.

Specific conductance = conductance × cell constant

The cell constant is measured by filling the conductivity cell with a solution
of known conductivity like 0.1 M KCl solution. The conductivity of 0.1 M
KCl solution is 0.01288 ohm-1cm-1 at 298 K. By measuring conductance of
0.1 M KCl solution in the given cell, the cell constant can be determined.
Conductivity of the given sample of water can be calculated by knowing
conductance of the sample water and the cell constant.
PROCEDURE
Preparation of standard KCl solution (0.1 M)
745 mg of KCl is weighed accurately using wax paper and transferred using
a funnel into a 100 ml standard flask. Wash wax paper using distilled water
and transfer all the contents into the flask and solution is made up to the mark
using distilled water.
Determination of Cell constant: -
Take a 100 ml of dry beaker, the conductivity electrode is inserted in it and
sufficient amount of 0.1 M of KCl solution is poured into it, so that the
electrode is in full contact with the solution. Measure the conductance by
selecting the proper range switch (milli mho or micro mho).

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Experiments in Engineering Chemistry Vimal Jyothi Engineering College

Determination of conductivity of sample water: -

After rinsing the 100 ml beaker with sample water, pour sufficient amount
of sample water into the 100 ml beaker, insert the conductivity electrode in
it, measure the conductance.
RESULT
Conductivity of the given sample water =

MARKS

SCORING
0.5 1 1.5 2
AVERAGE SATISFACTORY GOOD VERYGOOD TOTAL
CRITERIA
ACCURACY OF
RESULT
NEATNESS
PUNCTUALITY
OVERALL
PERFORMANCE
VIVA VOCE
TOTAL MARK

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Table 1
Calibration of device using standard solutions
S Dilution Concentration of Flame Photometer
l. Factor(i) standard solution (ppm) reading(ppm)
n
o
Entered Displayed Na=[x * i] K=[y * i]
Na/K(p/q) Na/K(x/y)
1 1
2 9
3 10
4 50
5 100
6 Blank
(H2O)
Table. 2
*Determination of concentration of unknown solution for Na/K
s.no Dilution Concentration of Flame photometer
factor(i) solution(ppm) reading(ppm)

1
2
3
4

Mean concentration of Na (ppm) = …………………………

Mean concentration of K (ppm) = …………………………..

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Experiments in Engineering Chemistry Vimal Jyothi Engineering College
Experiment No. Date.
DETERMINATION OF ALKALI METALS (Na & K) IN
WATER SAMPLE USING FLAME PHOTOMETER
AIM
To determine the amount of alkali metals (Na & K) in water sample by
using Flame photometer.
THEORY
Flame Photometry now more properly called “Flame Atomic Emission
Spectrometry”, is used to analyse the metal in all types of sample solutions
of minerals, metals, Ferro alloys. In a typical flame photometric
experiment, a solution containing the relevant substance to be analysed is
aspirated into the burner and dispersed into the flame as a fine spray. This
process is called Nebulization. When a solution of metallic salt is sprayed
on to a flame, fine droplets are formed. Due to the thermal energy of the
flame, the solvent in the droplets evaporates, leaving the fine residue,
which is converted to the neutral atoms. These neutral atoms are converted
into the excited state atoms by the thermal energy of the flame. As the
excited state is not stable, these excited atoms return to the ground state,
with the emission of radiation of specific wavelength. The wavelength of
the radiation emitted is characteristic of the element and is used to identify
the element (Qualitative Analysis). The intensity of the radiation emitted
depends upon the concentration of the element analysed (Quantitative
Analysis). Fraction of free atoms thermally excited = N* / No = A e-
ΔE/kT
where N* = no. of atoms in excited state
No = no. of atoms in ground state
A = Constant for element
ΔE = difference in energy level of excited and ground state
k = Boltzmann constant
T = Flame Temperature
The wavelength of light emitted depends upon the difference in the
energy levels of atoms in the excited and ground state. Since atoms of
each element have a specific wavelength of radiation, the colour of the
emitted radiation is different for different elements. For example, alkali
metal elements like 'Na' emits yellow (589nm), 'K' emits purple(767nm),
'Li' emits violet (670nm). Alkaline earth metals like 'Ca' emits brick red
(422nm, 554nm and 626nm) colored radiations. The wavelength of the
radiation emitted is given by the following equation: hc
Wavelength of light emitted (λ) = -----------

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Experiments in Engineering Chemistry Vimal Jyothi Engineering College

QUESTIONS
1. What is the basic principle of Flame Photometer?
2. What are the basic components of Flame Photometer?
3. Which are the functions of flame used in flame photometer?

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Experiments in Engineering Chemistry Vimal Jyothi Engineering College

E2 – E1
Where h = Planck’s constant
c = velocity of light

E2, E1 = energy levels of excited and ground states respectively. The

intensity of the radiation emitted depends upon the concentration of
The element presents in the solution. Higher the concentration, more is
The flame intensity and lower the concentration, less is the flame
intensity. The intensity of the spectral emission line is given by the
Following equation:
Intensity of spectral V AT h ro No ga
Emission line (Iv) = --------------- e-E/kT
B(T)
Where E= energy of excited state; k = Boltzmann constant
T = absolute temperature; h = Planck's constant
ro = freq. of radiation; V= flame volume (aperture ratio)
AT = no. of transitions each excited atom undergoes per second
No = no. of free metal atoms in ground state per unit volume
ga = statistical wt. of excited atomic state
B ( T ) = partial function of the atom overall states
MATERIALS REQUIRED
Flame photometer with cuvette cells, compressor and flame, Weighing
balance, standard volumetric flasks (100 ml, 50 ml); Burette; Graduated
pipette (25ml / 10ml / 5 ml), 1000 ppm NaCl/KCl Stock solution , 1000 ppm
CaCO3/LiCO3 Distilled Water.
PROCEDURE
Step 1: Calibration of flame photometer
1. Prepare the standard solutions of 1 ppm, 9 ppm (for low concn. Mode) and
10 ppm, 50 ppm, 100 ppm (for high concn.mode) in 100ml / 50 ml
volumetric flasks from the stock solution of NaCl /KCl.
2. Similarly prepare the standard solutions for Ca / Li in low and high
concentrations using the stock solution of CaCO3/LiCO3.
3. Switch on the instrument by following the instructions written on the
instrument and choose a setup number.
4. Set the instrument to low or high concentration mode and start calibration
in each mode by aspirating the standards. Use distilled water as blank.
5. Now, after calibration, aspirate the standards and check whether they are
in proper range and note the readings displayed.
6. From the supplied unknown solution of Na / K and Ca / Li, prepare the

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Experiments in Engineering Chemistry Vimal Jyothi Engineering College
Sample solutions in low or high concentration modes in 100 ml /50 ml
volumetric flask or by diluting them 100,200, 300 times (A, B, C etc.) and
again calibrate the instrument with the sample solutions by choosing
different setup number.

7. Now the samples are aspirated and analysed under flame photometer and
the readings are noted.
8. The concentrations of the respective solutions (A, B & C) for Na/K and
Ca/Li are multiplied by the respective dilution factors to get the mean
concentration of Na/K and Ca/Li which gives the original concentration of
Unknown Solution.
9. Save your calibration file in the directory and note the set-up number for
low and high conc. Modes.
RESULTS
Solutions Concentration in ppm
Unknown solution Na K Ca Li

MARKS

SCORING
0.5 1 1.5 2
AVERAGE SATISFACTORY GOOD VERYGOOD TOTAL
CRITERIA
ACCURACY
OF RESULT
NEATNESS
PUNCTUALITY
OVERALL
PERFOMANCE
VIVA VOCE
TOTAL MARK

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OBSERVATIONS AND CALCULATIONS
Standardisation of thiosulphate solution
Standard dichromate solution X thiosulphate solution
Indicator: starch

Volume of std. dichromate solution, V1 = 20 mL

Volume of thiosulphate solution, V2 = …………….mL
Normality of K2Cr2O7 solution N1 = ………………..
Volume of
Thiosulphate
Volume of Burette Readings in ml ( V2 mL)
SL.No std.dichromate solution
( V1 mL) Initial Final
1 20

2 20

At the end point

No. of equivalents of dichromate = No. of equivalents of thiosulphate solution
ie., V1N1 = V2N2
×
Normality of thiosulphate solution N2 = = = …………………………………..
Estimation of Copper in Brass
Cu2+ or brass solution X std. thiosulphate solution
Indicator: Starch

Volume of Cu2+ Burette Readings in ml Volume of

solution Thiosulphate
SL.No ( V2 mL)
( V1 mL) Initial Final
1 20

2 20

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Experiments in Engineering Chemistry Vimal Jyothi Engineering College
Experiment No: Date:

ESTIMATION OF COPPER IN BRASS

AIM
To estimate the amount of copper in brass, being provided with
approximately 0.01sodium thiosulphate and AR potassium dichromate
crystals, and a solution f brass dissolved in acid
APPARATUS
Pipette, Burette, Conical flask, Measuring jar, Standard flask
PRINCIPLE
Conical flask, A standard solution of potassium of dichromate solution is
prepared first, then using that standard solution the given thiosulphate
solution is standardised. It is done by adding excess potassium iodide
solution. From the standard reduction potential data
Cr2O7 2- + 14 H+ + 6e- 2 Cr3+ +7H2O E0 = +1.33 V (1)
I2 + 2e- E0 = +0.54V (2)
Since the reduction potential of dichromate is higher it is capable of
oxidising iodide(I-) ions from potassium iodide to iodine(I2). The liberated
iodine is then titrated against thiosulphate (S2O3 2-) solution using starch
indicator. Starch gives an intense blue colour on adsorption of I2.
S4O6 2- + 2e- 2 S2O3 2- E0 = +0.09 V
From reduction potential data it is seen that the liberated iodine is capable of
oxidising thiosulphate ions to tetra thionate S4O6 2- ions.
In this estimation of copper, potassium iodide solution is added to neutral
copper sulphate solution which is also capable of liberating iodine. During
the oxidation of I- ion to I2 Cu2+ ion is reduced to Cu+ ion.
2CuSO4 + 4 KI Cu2I2+ K2SO4 + I2 ; or Cu2+ + e- Cu+ ; E0 = +0.56 V
Here also the liberated iodine is then titrated against thiosulphate solution
using starch indicator. 1 ml of Ammonium thiocyanate (10%) solution is also
added along with starch to remove the adsorbed I2 from Cu2I2 precipitate.
PROCEDURE
Standardisation of thiosulphate solution: 20 mL of standard dichromate
solution (about 0.01N) is pipetted into a conical flask, add about 5 mL 5% KI
solution and 3 mL con. HCl and titrated against thiosulphate solution taken
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Experiments in Engineering Chemistry Vimal Jyothi Engineering College

Volume of Thiosulphate solution, V2 = ………………………. mL

Volume of Cu2+ Solution, V1 = 20 mL
At the end point
No. of equivalents of Cu2+ = No. of equivalents of thiosulphate solution
Ie., V1N1 = V2N2

×
Normality of Cu2+ in brass solution N1 = = = ………………………….
Weight of copper per litre of the given solution (x) = normality x eq. wt.
= N1 x 63.54 =………………
Weight of brass per litre of the given solution (y) = …………………… g/L (1g/L given
in Aim)

% of copper in the given brass = × 100 = ……………………………………………

QUESTIONS
1.What is Brass?
2. How is brass solution prepared?
3. What is the purpose of adding urea to the brass solution?
4. Why is KI added to brass solution although copper in brass is determined?
5. Why is starch indicator added towards end point?

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Experiments in Engineering Chemistry Vimal Jyothi Engineering College

in the burette. When the solution becomes pale yellow add 4 drops of freshly
prepared starch solution, then the solution becomes blue in colour. The titration is
continued by adding thiosulphate solution drop by drop till the blue colour
disappears.

Estimation of Copper: Pipette out 20 mL of the brass solution into a 250 mL

conical flask. It is then neutralised by adding NH4OH solution drop by drop till
the blue turbidity persists; dissolve this turbidity by adding glacial acetic acid drop
wise. To this neutral Cu2+ solution add about 5 mL 5% KI solution and stir well. It
is then titrated against standard thiosulphate solution taken in the burette. When
the solution becomes pale yellow 4 drops of starch solution and 1 mL 10%
ammonium thiocyanate solution are added and continue the titration till the blue
colour disappears. Repeat the titrations for concordant values.

Result: Percentage of copper in the given brass = …………………………

MARKS

SCORING
0.5 1 1.5 2
AVERAGE SATISFACTORY GOOD VERYGOOD TOTAL
CRITERIA
ACCURACY OF
RESULT
NEATNESS
PUNCTUALITY
OVER ALL
PERFORMANCE
VIVA VOCE
TOTAL MARK

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Experiments in Engineering Chemistry Vimal Jyothi Engineering College

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Experiments in Engineering Chemistry Vimal Jyothi Engineering College
Experiment No: Date:

DETERMINATION OF WAVELENGTH OF ABSORPTION

MAXIMUM AND CALORIMETRIC DETERMINATION
OF Fe3+ SOLUTION
AIM
To determine wavelength of absorption maximum and the determination of
unknown concentration of Fe3+ ion in the given sample solution. You are being
provided with a standard solution containing 1000 ppm ferric ion
PRINCIPLE
In UV-Visible spectroscopy, absorption of wave length from 200 to 800 nm is
observed. (200 to 380 nm UV region and 380 to 800 Visible region) In the
colorimeter a suitable monochromatic wavelength in the visible region (380 to
780 nm) is sent through a colored solution of the sample. The amount of
transmitted radiation depends on the extent of absorption of light. Let ‘I0’ be the
intensity of light transmitted through the blank solution and ‘I’ be the intensity
of light transmitted through the coloured sample solution.
Then, Absorbance A= log , The absorbance ‘A’ can be directly read out from
the instrument.
According to Beer-Lambert’s law A= ɛ c t , where ‘ɛ’ is the molar absorption
coefficient of the coloured substance, ‘c’ is the concentration of the solution and
‘t’ is the thickness of the absorption medium. Here ‘ɛ’ and ‘t’ are constants for the
given coloured molecule and for given cell. Therefore, absorbance A is
proportional to concentration ‘c’, When we plot a graph between ‘A’ and ‘c’ we
must get a straight line passing through origin. The unknown concentration can be
read out from the graph by noting its absorbance.
The calorimetric determination of Fe3+ is based on the formation of red coloured
complex with thiocyanate ion. The complex shows an absorption maximum at 490
nm.
Fe3+ + 3CNS- [ Fe(CNS)3]
PROCEDURE
Preparation of 100 ppm standard solution
10 mL of the given standard (1000ppm) is pipetted into a 100 mL standard flask.
The solution is the made up to the mark using distilled water.
Preparation of standard coloured solutions and the blank
Take six,100 mL standard flasks. Pipette 2 mL,4mL,6mL,8mL,10mL standard
Fe3+ solutions(100ppm) into each flask using a 10mL graduated pipette
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Concentration 2 4 6 8 10 unknown
(ppm)
Absorbance
(A)

The Unknown
concentration

2 4 6 8 10
Concentration (ppm)

Unknown concentration = concentration from the graph x 10 = …………… ppm

QUESTIONS
1. What is the formula of ferrous ammonium sulfate hexahydrate?
2. Over what range of iron concentrations does the iron-bipyridyl complex
obey the Beer-Lambert law?
3. What is colorimeter?

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Add 10mL 4% potassium thiocyanate solution into each standard flask

including the blank flask. The solutions are then made up to the marks using
distilled water. Keep the flask at rest for about 5 minutes.
Determination of wavelength of absorption maximum
Switch on the UV-Visible spectrometer; activate the scan mode by mouse click.
Select the wavelength range from 200 to 800 nm. Fill the cuvette with any on
the standard coloured solution prepared above and place it in the spectrometer.
Scan the spectral range and print the spectrum. Note the wavelength of
absorption maximum.
Verification of Beer-Lamberts law
Switch on the colorimeter. Adjust the wavelength of the filter of the calorimeter
to 490 nm(wave length of absorption maximum obtained above.)Note the
absorbance at 490 nm for all these solutions after setting zero with blank
solution. Plot absorbance against concentration, then a straight line passing
through origin is obtained.
Determination of Un-known concentration
10 mL of the sample solution is pipette out into a 100 mL standard flask add 10
mL 4% potassium thiocyanate solution and made up to the mark using distilled
water. Keep the solution at rest for about minutes. Note the absorbance of this
solutions at 490nm after setting zero with the blank solution. The unknown
concentration can be read out from the graph its absorbance.

Result: Wavelength of a absorption maximum =………………………. nm

The concentration of Fe3+ in the given sample solution = ………………ppm

MARKS

SCORING
0.5 1 1.5 2
AVERAGE SATISFACTORY GOOD VERYGOOD TOTAL
CRITERIA
ACCURACY OF
RESULT
NEATNESS
PUNCTUALITY
OVER ALL
PERFORMANCE
VIVA VOCE
TOTAL MARK

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