Engineering Chemistry Lab Manual

General Instructions

 Before coming to the laboratory, understand the theory behind the reaction you are going to carry

out.

 Keep the workbench and sink neat and clean. Don’t allow filter paper, broken bits of glass,

matchstick etc., to lie on the table or in sink. Put these things in the dustbin placed below worktable.

 Apparatus should be in non-greasy condition.

 Keep the apparatus clean and properly arranged on the workbench.

 If any piece of apparatus is broken, report at once to the staff members / Lab Assistant.

 Once you have transferred a reagent from a reagent bottle, never pour it back even if there is excess

quantity.

 Arrange reagent bottles in their proper places after use and see that they are properly stoppered.

 Handle reagent bottles / chemicals carefully.

 Use only minimum possible quantity of chemicals / reagents for any reaction.

 Close the water tap immediately after use; do not waste water.

 Precautions should be taken to avoid fire accidents.

 After the class, before you leave the laboratory, wash the apparatus clean, wipe the table and keep

the apparatus in proper place.

***

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INTRODUCTION TO ENGINEERING CHEMISTRY LAB

Analytical chemistry plays an important role in recognizing different substances and determining their
constituents. The chemical analysis is mainly divided into qualitative and quantitative analysis.

Qualitative analysis:
It is a method of the detection and identification of the constituents of a compound or a mixture of
compounds or elements.

Quantitative analysis:
It is a process of estimation of exact amount of chemical species present in a sample.

a) Volumetric analysis or Titrimetric analysis:

It is a method of accurate measurement of volume of reagent solution required for complete reaction,
and then the concentration of the sample solution can be calculated.
Ex: Estimation of Calcium in Portland cement using permanganate by volumetric analysis

b) Gravimetric analysis:
In this method, the constituent to be determined is separated from all other components of the sample in
the form of an insoluble precipitate by adding a suitable reagent.
Ex: Estimation of Calcium in Portland cement using ammonium oxalate as calcium oxalate.

Types of titrations in volumetric analysis

I)Acid –Base Titrations or Neutralisation Reactions:

In this titration, an acid is titrated against a base or vice-versa and strength of one of them is known
while that of the other is calculated.
Ex: Estimation of strength of sodium carbonate in soda ash.

Example HCl + NaOH ® NaCl + H 2O

H 2C2O4 + 2NaOH ® ( COONa) 2 + 2H 2O

II) Complexometric Titrations (EDTA Titrations):

In this titration, the ions (metals) are titrated against a complex forming agents like EDTA with aid of
suitable indicator.
Ex: Determination of Hardness of ground water by using EDTA

Example 2CN-+Ag+ [Ag(CN)2]-

EDTA+Mg+2 Mg-EDTA

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III) Redox Titrations:

In this titration, one substance under goes oxidation and other is reduced during titration. The strength
of one of them is known while that of the other is calculated.

Types of Redox reactions:

1. Titrations involving Potassium Permanganate (Permaganometry):

In this titration, Potassium permanganate is a strong oxidant which oxidises other unknown sample.
The strength of potassium permanganate is known and that of other is calculated.
Titrations are usually carried out in an acidic medium and permanganate acts as self indicator.

Ex: Estimation of calcium in Portland cement.

2. Titrations involving Potassium Dichromate (Dichrometry):

In this titration, Potassium Dichromate is a strong oxidant which oxidises other unknown sample. The
strength of potassium dichromate is known & that of other is calculated.
Titrations are usually carried out in an acidic medium. The end point is identified by either using
potassium ferricyanide as external indicator or diphenyl amine as internal indicator.

Ex: Estimation of chromium in potassium dichromate.

3. Titrations using iodine solutions:

a) Iodimetry:
In this titration, a standard iodine solution is taken in an iodine flask and it is titrated with a solution
of a reductant whose concentration is to be determined.

b) Iodometry:

In this titration, iodine is liberated during chemical reactions. An unknown sample solution upon
adding excess amount of KI in the presence of acid medium liberates iodine which is estimated by
using standard sodium thiosulphate solution.
Ex: Estimation of Copper in Copper ore.

IV) Precipitation reactions:

In a precipitation titration, A stoichiometric reaction produces a slightly soluble salt in solution that
precipitates out. To determine the concentration of chloride ion in a particular solution, one could titrate
this solution with a solution of a silver salt, say silver nitrate, whose concentration is known.
Ag+(aq) + Cl-(aq) --> AgCl(s)

A white precipitate of AgCl is deposited at the bottom of the flask during the course of the titration.

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Basic terms used in volumetric analysis

1. Titration: It is a systematic method of determining the strength or concentration of a solute in a

solution using another solution whose strength is known.

2. Titrant: Solution taken in the burette, its concentration is known.

3. Titre: The volume of the titrant required in a titration.

4. Analyte or Titrand: Substance being analyzed to determine its concentration, which is taken in
conical flask.

5. Reagent: To find out concentration of analyte, adding solution of another substance.

6. Standard solution: A solution whose concentration is accurately known is called a standard

solution.

7. Standardization: A process to determine the concentration of a solution of known concentration by

titrating with a primary standard.

8. Primary Standard: A reagent solution of accurately known concentration.

It has the following characteristics:

1. High purity (>99.9%)

2. Stability toward air

3. Absence of hydrate water (non-hygroscopic)

4. Available at moderate cost

5. Soluble

6. Large Molecular weight.

Examples: Sodium carbonate, Potassium dichromate, Sodium oxalate

9. Secondary Standard: A reagent solution of indefinite concentration which is standardized by using

a primary standard solution.

Examples: Acids, Bases, Sodium thiosulphate, Potassium Permanganate.

10. Equivalence Point: During a titration, the point at which the reaction between a titrand and titrant
is just complete is called Equivalence Point.

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11. End Point: The point at which an indicator changes its colour is known as the end point.

Indicator Colour change

Methyl Orange Yellow to Pale red
Phenolpthalein Colourless to pink
Diphenyl amine Colourless to bluish violet
Starch Blue to Colourless
Eriochrome Black-T Wine-red to blue

12. Molarity: It is number of moles per one litre solution.

13. Normality: It is number of gram equivalent moles per one litre solution.

14. Equivalent Weight: The concept of equivalent weight changes according to the type of reaction
involved in the volumetric titration.

a. In an acid base titration, the equivalent weight is calculated by dividing the molecular weight by
the number of replaceable H+ ions or OH¯ ions.
b. In a redox reaction, the equivalent weight is calculated by dividing the molecular weight by the
total number of electrons gained or lost.
c. For example, in the estimation of ferrous ion with standard dichromate solution the equivalent
weight of the oxidizing agent (potassium dichromate) is 1/6 th of its molecular weight since the
number of electrons gained by Cr (VI) is six.
Ex: Cr2O7-2+14H++6e- 2Cr+3+7H2O
6Fe+2 6Fe+3+6e-

d. In the titration of oxalic acid with potassium permanganate, the equivalent weight of
permanganate is 158/5 = 31.6 (since number of electrons gained by Mn(VII) are five). The
equivalent weight of oxalic acid is 126.07 / 2 = 63.035 (Since total number of electrons lost by
oxalic acid is two).
Ex: 2 KMnO4 + 3H 2 SO4 ® K 2 SO4 + 2 MnSO4 + 3H 2O + 5(O )
5H 2C2O4 + 5 (O) ®10CO2 + 5H 2O

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Volumetric apparatus

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1. Calibration of Volumetric Apparatus

Learning objectives:
To learn about

 To avoid systematic
errors in volumetric
experiments
 To maintain quality
of measurements in
Fig: Parallax error experiment
 To retain accuracy
and precision of
Significance: experiment

 Volumetric glassware like burettes,

pipettes, volumetric flask, conical flask
and measuring cylinder are containers Expt. No:
that have been calibrated at a specific
temperature to deliver or contain very
precise amounts of liquid. Date:
 Without proper calibration of volumetric
ware leads to errors and finally absurd
results displayed

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Apparatus: In titrimetric analysis, while using the following apparatus, we should take some precautions to
minimize the practical errors.
1) Burette: Generally a burette has the capacity of holding 50 ml graduated to 1/10 of a milliliter from top
to bottom. At the lower end it is provided with stopcock to regulate the flow of solution.
a) It should always be kept in non-greasy condition. For this reason, the burette is cleaned with
chromic acid and then thoroughly washed with tap water and then distilled water. Then the burette
should be thoroughly rinsed with little of solution that is to be filled in it and reject the rinsed
solution.
b) It is filled with a standard solution. The readings should be noted without parallax error and then it
should be vertically clamped to a burette stand.
While taking the readings, it is better to hold a white paper behind the burette readings and eye must be
placed in the same line of the meniscus. Generally the reading is tangential to lower meniscus in case of
colorless or light colored solutions and upper meniscus in case of concentrated or deeply colored solutions.
2) Volumetric pipette: The pipette is a long narrow tube having cylindrical bulb in the middle and tapping
to a fine nozzle at its lower end and carrying a mark round the glass tube above the bulb. The volume
delivered between the upper mark and lower tip is the volume being titrated (Caution! Don’t blow the
last drop in the nozzle of the pipette). With this we can transfer a definite volume of solution from one
flask to another. The pipette should be washed repeatedly with tap water and then distilled water and
then rinsed with a little of solution which is to be transferred.
3) Graduated pipette: Another type of pipette used in the laboratory is the graduated pipette for
transferring approximate volumes of reagents (such as acids, alkalis, indicators etc.,). These are
graduated in 1/10 of a milliliter, for every milliliter. These are available to measure 1.0, 2.0, 5.0, 10.0
and 20.0 ml. An advantage of these graduated pipettes is that a fraction of milliliter can be measured
and transferred to the conical flask.
4) Measuring jar: This is a cylindrical jar provided with a round base at its one end. It will be graduated
from the bottom to top and has the capacity of holding 50 or 100 ml. and graduated in 1.0 ml units. This
is only used for measuring and transferring the approximate volumes of solutions (generally reaction
medium and other reagents), where accuracy is not important. This should be thoroughly washed with
chromic acid followed by tap water and distilled water. They are also available in the following
capacities 10, 20, 25, 250, 500 and 1000 ml.
5) Conical flask or Erlenmayer flask: It is cone shaped flask and is used in titrations as reaction flask. It
is available in the volume range from 10, 25, 50, 100, 250, 500 and 1000 ml. Generally 250 ml conical
flasks are recommended for class work. During the titration, the neck of the conical flask should hold
using the right hand. It helps to make swirling motion of the solution convenient by rotating the flask.
6) Distilled water bottle / Wash bottle: It is readily available in the range 500, 750 and 1000 ml. It is
made of pyrex glass or corning glass or polyethene. The importance of using wash bottle is to get fine
stream of water to wash down the adhering droplets of the titrant in to the bulk of the titrand in conical
flask.
7) White glazed tile: It is white ceramic tile and helps to see the exact color change at the end point of the
reaction by providing a glossy white background..
***

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2. Estimation of Mohr’s Salt by Potentiometric Method

Learning objectives:
To learn about

 To know about
calculation of iron
content through
potentiometer.
 To assess the amount
of iron without using
indicator
 To understand the
working of
potentiometer by using
redox titration
Significance:
 Potentiometers are used in the manufacture of
electronics equipment that provides a way of Expt. No:
adjusting electronic circuits so that the correct
outputs are obtained.
Date:

 Potentiometer is widely used in various fields:

automotive, medical equipment, robotics, wood
processing machines, molding machines..

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Aim: To estimate the amount of given Mohr’s salt by titrating against standard potassium dichromate
solution potentiometrically.

Apparatus and solutions required: Potentiometer, calomel electrode, platinum electrode, beaker, salt
bridge, N/20 dichromate solution and unknown Mohr’s salt solution.

Theory: It is very well known that the electrode potential of the electrode depends upon the
concentration of its ions in the solution so the potential of an indicator electrode goes on changing with
respect to a standard (reference) calomel electrode by the change of concentration of ions during the
titration. The equivalence point is indicated by fairly a large change in electrode potential value. This
can be found by plotting a graph between the emf of the cell on Y-axis and the volume of titrant and
added on X-axis.

0 . 0591 [ oxidant ]
E=E o + log
n [ reductant ]

Procedure: 10.0 ml of unknown Mohr’s salt solution is pipetted out in to a 100 ml beaker. 5.0 ml of
1:1 sulphuric acid and 35 ml of distilled water are taken in a measuring cylinder and are transferred in
to the beaker. The potentiometer is connected with an indicator electrode (platinum) and a reference
electrode (calomel) in proper direction. The contents of the beaker are then titrated against standard
dichromate solution. A pilot titration is carried out by adding 1 ml portion of dichromate solution each
time. The solution is thoroughly mixed and the corresponding emf values are noted in Table I. At the
equivalence point a large change in potential is noticed. Similarly an accurate titration is carried out by
adding 0.1 ml portions of dichromate solution at the vicinity of the equivalence point. The results are
presented in Table II. A graph is drawn between volume of dichromate solution on X-axis and
potentials on Y-axis for the accurate titration.

Table I: Pilot titration of Mohr’s salt solution with standard solution of potassium dichromate

10.0 ml Mohr’s Salt Solution + 5 ml of 1:1 H2SO4 + 35 ml water

Volume of dichromate
Sl. No. Potentials (mV)
solution (ml)

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Table II: Accurate titration of Mohr’s salt solution with standard solution of potassium
dichromate

10.0 ml Mohr’s Salt Solution + 5 ml of 1:1 H2SO4 + 35 ml water

Volume of dichromate
Sl. No. Potentials (mV)
solution (ml)

Calculations:

According to law of equivalence, V1N1 = V2N2

V1 = Volume of Mohr’s salt solution = ml

N1 = Normality of Mohr’s salt solution = ?

V2 = Volume of dichromate solution = ml

N2 = Normality of dichromate solution = N

V 2N 2
∴ N1 =
V1

Normality of Mohr’s salt solution = N

Amount of Mohr’s salt in 1lit = Normality X Eq. wt.

= N1 X 392.2

N 1  392.2
Amount of Mohr’s salt present in 100 ml = = …….. g.
10

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Report:

Amount of Mohr’s salt present in 100 ml of solution = ……. g.

Precautions:

 The platinum electrode should be activated using spirit lamp before starting the titration.

 The solution should be thoroughly shaken with a stirrer each time.

Table III: Percentage error:

Amount of Mohr’s salt present in 100 ml

of solution
Percentage Signature of
Roll. No Grade/Marks
error
Reported Given Teacher

Inquiry based questions:

1. How do you estimate the iron using dichromate through potentiometrically

2. Explain principle involved in the potentimetric method of estimation of iron using
dichromate.
3. Discuss about Nernst equation and its significance
4. What is redox potential

*****

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3. Determination of Strength of an acid by pH metric Method

Learning objectives:
To learn about

 To know about
calculation of
strength of acid
through pH
metry

 To assess the
Strength of acid
without using
indicator.
Significance:
 To understand
the working of
Knowledge of pH is useful in many situations, including
pH meter
chemical laboratory, water quality for municipal water
supplies, soil measurement analyses in agriculture,
manufacturing, healthcare, clinical and many applications
Expt. No:
Date:

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Aim: To determine the strength of hydrochloric acid with standard sodium hydroxide by pH metric
method.

Apparatus &Chemicals required: pH meter, combined glass electrode, 250 ml beaker, semi-micro
burette, distilled water bottle, 0.1N NaOH, unknown HCl solution and buffer solution of pH 4 and 9.2.

Theory: Hydrochloric acid can be estimated using sodium hydroxide (following pH metric method) as
per the neutralization reaction. The pH meter will give good result between the pH ranges 2 and 10.

The pH meter consists of combined glass electrode and indicator electrode which responds to H +
concentration and a calomel electrode (reference electrode). The electrochemical cell is

H 2 ( Pt )1 atm HCl Salt bridgeSat. KCl ( N ) KCl, Hg2Cl2 ( S ) Hg

The emf of the cell is given by

0 . 0591
E=E o + log [ H + ] at 27 o C
n

Procedure: The unknown solution of hydrochloric acid is made up to the mark with distilled water.
10.0 ml of the solution is pipetted out in to a clean beaker. 40 ml of distilled water is added to this
solution. Meanwhile the pH meter is switched on and is allowed to stabilize for about 10 to 15 min. The
instrument is calibrated with standard buffers of pH 4 and 9.2. A standard solution of sodium hydroxide
is taken in a micro burette. A pilot titration is carried out by titrating the contents of the beaker with 1
ml portions of sodium hydroxide each time. The solution is thoroughly mixed and the corresponding
pH values are noted in Table I. Accurate titration is carried out similarly with 0.1 ml portions of sodium
hydroxide near the neutralization point. The corresponding pH values are recorded in Table II

Table I: Pilot titration of unknown hydrochloric acid solution with standard sodium hydroxide
solution
10 ml of hydrochloric acid + 40 ml of distilled water

Volume of NaOH
Sl. No. pH
solution (ml)

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Table II: Accurate titration of unknown hydrochloric acid solution with standard sodium
hydroxide solution

10 ml of hydrochloric acid + 40 ml of distilled water

Volume of NaOH
Sl. No. pH
solution (ml)

The corresponding pH values are recorded in Table II. 10 ml hydrochloric acid + 40ml distilled water.

Calculations:

According to law of Equivalence, V1N1 = V2N2

V1 = Volume of sodium hydroxide = ml

N1 = Normality of sodium hydroxide = N

V2 = Volume of hydrochloric acid = ml

N2 = Normality of hydrochloric acid = ?

Amount of hydrochloric acid present in 100 ml of the given solution

Normality of HCl  Eq. Wt. of HCl ( 36.5 )

=
10

= g

Report:

Amount of Hydrochloric acid present in 100 ml of the solution = …….. g

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Precautions:

 Whenever electrodes are being removed/immersed from /in any solution, the range selector
switch of pH meter must be kept at zero ( at stand by ) position
 It is advised, always to keep the electrodes dipped in distilled water whenever they are not
being used.

Table III: Percentage error

Amount of Hydrochloric acid present in

100 ml of the solution
Percentage Signature of
Roll. No Grade/Marks
error Teacher
Reported Given

Inquiry based questions:

1. Discuss the principle involved in pH metry

2. Write the method of estimation of acid by using pH metry
3. Define pH and its formula
4. How pH and buffer are related to each other
5. Explain the relation of electrode potential and pH
6. What is pilot titration

*****

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4. Determination of Conductance by Conductometric Method

Learning objectives:
To learn about

 To know about
calculation of
conductance
through
conductometry

 To understand
the difference
Significance: between strong
and weak
electrolytes
Knowledge of measuring conductance is useful in many situations,
including chemical laboratory, water quality for municipal water  To understand
supplies, soil measurement analyses in agriculture, manufacturing, the working of
healthcare, clinical and many applications
conductometer

Expt. No:
Date:
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Aim: To determine the amount of unknown acid solution with standard base solution by
conductometric method.

Apparatus: Conductivity meter (with cell), burette (10ml), volumetric flask (100 ml),
beakers (100 ml), stirrer / glass rod.

Chemicals: Stock acid solution, 0.05 M oxalic acid in100ml volumetric flask and Stock base
solution.
PRINCIPLE: Conductometric titrations works on the principle of Ohm's law. As current is
inversely proportional to Resistance (R) and the reciprocal of resistance is termed as Conductance,
and its unit is Siemen (mho) cm-1. The electrical conductivity of a solution depends on the number
of ions and their mobility. In Conductometric titrations, the titrant is added from the burette, and
the conductivity readings are plotted against the volume of the titrant. Upon adding a strong base
to the strong acids, the conductance falls until the strong acid is neutralized then raised. Such a
titration curve consists of 2 lines which intersect at a particular point, known as the End point or
Equivalence point. The method can be used for titrating coloured solutions or homogeneous,
which cannot be used with normal indicators.

Strong Acid with a Strong Base:

For example, in the titration of HCl versus NaOH, the addition of a strong base (NaOH) to
a strong acid (Hcl). Before NaOH is added, the conductance is high due to the presence of highly
mobile hydrogen ions. When the base is added, the conductance falls due to the replacement of
hydrogen ions by the added cation as H+ ions react with OH- ions to form undissociated water.
This decrease in the conductance continues till the equivalence point. At the equivalence point, the
solution contains only NaCl. After the equivalence point, the conductance increases due to the
large conductivity of OH- ions.
H2C2O4 + 2 NaOH Na2C2O4 + 2H2O

HCl + NaOH NaCl + H2O

Formula:

Procedure:

Step 1: Standardization of sodium hydroxide by using oxalic acid

1. Rinse and fill the burette with the given NaOH solution
2. Pipette out 20 ml of 0.05 M oxalic acid solution into a clean conical flask
3. Add 1 or 2 drops of phenolphthalein indicator to oxalic acid solution.
4. Titrate the solution against sodium hydroxide solution drop wise with shaking till the
solution changes to pale pin
5. Note the volume of NaOH used. It is the end point.
6. Repeat the titration until the concordant readings are obtained
7. Calculate the molarity of NaOH by using the formula mentioned above

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Observations and Calculations: Conductometric titration in between HCl and NaOH

Volume of base added Conductance Corrected conductance

C1= C[(v+V)/V]

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Calculation of Unknown molarity of HCl solution:

Sodium Hydroxide:
M2 = Molarity of NaOH =
V2 = Volume of NaOH =
n2 = Moles of NaOH = 1 mole
HCl:
M3= Molarity of HCl =?
V3= Volume of HCl = 25 ml
n3 = Moles of HCl = 1 mole

Molarity of HCl = ----------------- M

Amount of HCl = ---------------- g/l

Step 2: Determination of molarity of unknown HCl by using standard NaOH through

conductometric titration

1. In 100 ml beaker take 25ml of given unknown HCl solution and add 25ml of distilled
water. The contents are shaken thoroughly.
2. Now, the conductivity cell is immersed in the beaker and the initial conductance of the
solution is taken by stirring the solution and keeping it constant.
3. Then, 0.5 ml portions of base is added from the burette and stirred well. The conductance
of the solution for each addition is to be noted.
4. The conductivity is corrected by multiplying with the factor [(v+V)/V], where 'v' is the
volume of base added and 'V' is the volume of solution initially taken in the beake

5. Plot the graph with respect to the volume of base consumed versus corrected conductance.
From the intersection point on the graph which gives value represents
the equivalence points of acid and base.

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Report:

S.No Given Amount of Reported Amount of % Error Marks Signature of the

unknown Acid unknown Acid Faculty

Inquiry based questions:

1 Discuss the principle involved in conduct metry

2 Write the method of estimation of acid by using conductometry
3 What is the difference between conductance of metal and electrolytic solutions?
4 What is specific conductivity ? Give its units
5 Give the factors on which conductance of a given solution depends ?

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5. Determination of Viscosity of a Liquid

Learning objectives:
To learn about

 To know about the

flow measurements
of liquid

 To understand
about various
forces resist the
movement of liquid
Significance:
 Gathering viscosity data on a material gives
manufacturers the ability to predict how the material
will behave in the real world.

 Viscosity measurements are very important in

petroleum, food, concrete, adhesives and cosmetic
Expt.No:
industries.

 Viscosity affects heat generation in bearings, cylinders

and gear sets related to an oil's internal friction Date:

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Aim: To determine the viscosity of the given liquid using Ostwald’s viscometer.

Apparatus and Chemicals: Ostwald’s viscometer, stopwatch, specific gravity bottles, pipette, rubber
tubing, water, organic liquid.

Theory: The Ostwald’s viscometer method is based on Poseuille’s equation. This relates the rate of
flow of a liquid through a capillary tube with the coefficient of viscosity expressed by the equation

r 4t

8vl

Where r = Volume of the liquid of viscosity  flowing in time ‘t’ through a capillary tube of radius ‘r’
and length ‘l’. p- hydrostatic pressure of the liquid.

The determination of absolute viscosity by means of poseuille’s expression, which involves the
determination of v, r, t, l and p. But in practice this method is tedious. Hence a simpler method of
comparing the viscosities of two liquids can be followed.

If t1 and t2 are the flow times required to flow for equal volumes of two liquids through same
length of capillary tube, then

1 P1t1

 2 P2t2

P = hdg

Here h & g are same for the two liquids.

η1 d1 t 1
=
η2 d2 t 2
d1 t 1
⇒ η 1= η
d2 t 2 2

Procedure: The viscometer is cleaned first with chromic acid, water and then with distilled water. It is
finally washed with alcohol and ether and then dried. A piece of clean rubber tube is attached to the end
‘C’ of viscometer and is clamped vertically in air. A sufficient volume of distilled water is introduced
in one of the bulbs (B) so that the bend portion of tube and half or a little more than half bulb (B) are
filled up. With the help of rubber tube attached to the upper arm of bulb (A) water is sucked until it
rises above the upper mark ‘C’ and is allowed to flow under its own weight. The time of flow of water
from ‘C’ to ‘D’ is counted by starting stopwatch as the meniscus just passes lower mark ‘D’. The same
procedure is repeated three times and the mean values are determined. The viscometer is cleaned and

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dried. The same procedure is repeated with the same volume of given liquid and the time of flow of
liquid is measured and the values are recorded in Table I. The relative density of a given liquid is
measured using pycnometer.

Observations

Sl. No. Water Given liquid

Time of flow Mean (t2) Time of flow Mean (t2)

η1 d t
= 1 1
η2 d2 t 2

Where

η1 = Viscosity of the given liquid = ?

η2 = Viscosity of water = poise

d1 = density of the given liquid = gm/cm3

d2 = density of water = gm/cm3

t1 = time of flow of given liquid = sec

t2 = time of flow of water = sec

d 1 t1
(Absolute viscosity) η1 = η2
d 2t 2

Report:

The relative viscosity of the given liquid with respect to water at room temperature =……. poise.

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Precautions:

 The viscometer should be thoroughly cleaned.

 Viscometer must be strictly kept in vertical position
 Same volumes of liquid and water are to be taken while performing the experiment.

Percentage error:

Viscosity of given liquid

Percentage Signature of
Roll. No Grade/Marks
error
Reported Given Teacher

Inquiry based questions:

1. What is viscosity?
2. What is viscosity co-efficient of a liquid?
3. What is specific gravity?
4. How are specific gravity and density of liquid related?
5. What is the unit of viscosity coefficient in SI & cgs systems?
6. What are the factors that affect the viscosity of a liquid?
7. What is the law based on the viscous flow of liquids through capillary tubes?
8. How does viscosity vary with temperature?
9. Why should the viscometer be dried before the measurements are done and which
solvent is used?

*****

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6. Determination of Surface Tension of a Liquid

Learning objectives:
To learn about

 To know about the

origin of surface
tension and nature
of surfactant

 To understand types
Significance: of cohesive forces
 Surface tension is the elastic tendency of a fluid surface
which makes it acquire the least surface area possible.

 Without surface tension, even the smallest objects would

sink underwater. The large particles of dust would not float
on the water, but instead the particles would sink to the Expt.No:
bottom and kill all of the marine life, causing the collapse
of ecosystems.

Date:

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Aim: To determine the surface tension of the given liquid at room temperature by stalagmometer.

Apparatus and chemicals: Stalagmometer, beaker, rubber tubing, pinch cork, relative density bottle,
thermometer, water, given organic liquid.

Theory: When a liquid is allowed to flow through a capillary tube, a drop is formed at its lower end. It
increases to a certain size and falls off. The size of the drop depends on the radius of the capillary and
the surface tension. The surface tension acting along the circumference of the capillary tube supports
the drop in the upward direction.

The measurement of surface tension of a liquid is based on the fact that the drop of the liquid at
the lower end of capillary falls down when the weight of the drop becomes equal to the surface tension.
The surface tension of the given liquid is determined relative to water at room temperature by using
stalagmometer. The number of drops for the same volume of water and the given liquid are counted and
let there be n1 and n2 respectively. Now if the densities of water and given liquid at room temperature
as determined separately using specific gravity bottle, then the surface tension γ 2 of the given liquid
can be calculated using the relationship.

 1 n2 d1
  dynes/cm
 2 n1 d 2

Procedure: The stalagmometer is cleaned thoroughly first with chromic acid solution and finally with
distilled water and then dried. The lower end of stalagmometer is immersed in a beaker containing
distilled water. The water is sucked until the level rises above the mark ‘C’ and the screw is tightened.
The liquid is allowed carefully so that the liquid drops start falling at an interval of about 2-3 sec. in
successive drops. Counting of the drops is started when the meniscus just reaches the upper mark ‘C’
and stopped when the meniscus just passes the lower meniscus ‘D’. The same procedure is repeated
thrice and the mean value is considered. The values obtained are noted in Table I. The stalagmometer is
cleaned and dried. It is then filled until the level rises above the upper mark ’C’ and the number of
drops is counted as described earlier. A specific gravity bottle is cleaned and dried. The density of the
given liquid is measured using the specific gravity bottle.

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Table I: Determination of Surface Tension of the given liquid

Sl. No. Water (n1) Given liquid (n2)

Number of drops Mean Number of drops Mean

γ 1 n2 d 1
= x
γ 2 n1 d 2

1 = Surface tension of water = dynes/cm

2 = Surface tension of the given liquid = ?

n1 = No. of drops of water =

n2 = No. of drops of the given liquid =

d1 = density of water = grams / cm3

d2 = density of the given liquid = grams / cm3

n1 d2 γ 1 x1 x d 2
∴ 2 = n x d x γ 1 = n2 x d 2
2 1

Report:

The relative surface tension of the given liquid with respect to water at room temperature = …….

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Precautions:

 The stalagmometer and the specific gravity bottle should be cleaned properly and dried
before use.
 The stalagmometer should be fixed vertically.
 The number of drops must be between 15-20 per 3 minutes

Percentage error:

Surface tension of given liquid

Percentage Signature of
Roll. No Grade/Marks
error
Reported Given Teacher

Inquiry based questions:

1. Define surface tension.

2. Give the equation for the determination of surface tension.
3. Which instrument is used to find out the surface tension of a given liquid?
4. What are the units of surface tension?
5. What is the value of surface tension of water?
6. Is surface tension an intensive or extensive property?
7.What are the factors affecting the surface tension?
8.What is the effect of temperature on the surface tension?
9. Give some practical applications of surface tension.
10 Why the surface of the slide should not be oily?

*****

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 Engineering Chemistry Lab Manual

7. Determination of amount of sulphuric acid in Lead-Acid storage

cccell

Learning objectives:
To learn about

 To demonstrate the
basic laboratory
technique of
titration

 To learn to
calculate molarity
based on titrations

Significance:

 Not maintaining the required acid concentration in

Lead-Acid battery results in reduction in performance
of the battery and may cause premature battery
failure. Expt. No:
 Low concentration of acid results in drop in output
voltage.
 High concentration of acid causes additional build-up Date:
of lead sulfate at the bottom (sulfation), which
reduces battery storage capacity and battery life.

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Aim: Determination of the amount of sulphuric acid present in lead-acid storage cell by using standard
sodium hydroxide

Theory: Lead-acid storage cell contains 38% sulphuric acid which is a strong acid and is estimated by
using standard sodium hydroxide, a strong base using phenolphthalein indicator. These two reacts as
follows:

H 2 SO4 + 2 NaOH ® Na 2 SO 4 + 2 H 2 O

In this reaction, salt and water are formed, which is an example of neutralization reaction. As
the reactants and products are colorless, so phenolphthalein is used to locate the end point of the
reaction. The color change of Phenolphthalein is from pink in alkaline medium to colorless in acidic
medium (pH range 3.3 to 4.3).

Procedure: The given unknown acid solution is made up to the mark of volumetric flask with distilled
water carefully. The flask is stoppered and shaken thoroughly about 3 to 5 minutes for complete
homogenization.The burette is rinsed with distilled water, rinsed once with the acid solution that is to
be taken in it and finally filled with that acid solution up to zero mark. 10 ml of the alkali solution is
pipetted out into a clean conical flask carefully and 50 ml of distilled water is added with measuring jar.
Two drops of phenolphthalein indicator is added directly to the contents of conical flask. The conical
flask contents are titrated with unknown acid solution after noting the initial reading. The titration is
continued until the color changes from pink to colorless. The final reading of burette is noted. The
titration is repeated for getting concurrent results. The results are tabulated in Table I.

Table I: Titration of unknown acid solution with given standard alkali solution.

Normality of standard alkali solution = N

Indicator: phenolphthalein

Color change at the end point: pink to colorless.

Volume of alkali solution Burette readings Volume of acid solution

Sl. No.
taken in ml (V2) Initial (ml) Final (ml) consumed in ml (V1)
1
2
3

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Calculations:

By the law of equivalence N1V1 = N2V2

N1 = Normality of unknown sulphuric acid solution = ?

V1 = Volume of sulphuric acid solution = ml

N2 = Normality of sodium hydroxide solution = N

V2 = Volume of sodium hydroxide solution = ml

 N1= N2V2 / V1 =

 The normality of sulphuric acid solution = N

Equivalent weight of H 2 SO 4 = molecular weight / 2 = 98/ 2 = 49

Amount of H 2 SO 4 present in 1000 ml of the given unknown sulphuric acid solution = Normality of

H 2 SO 4 solution  equivalent weight of H 2 SO 4 = …….  …49…. = ……… g.

Amount of H 2 SO 4 present in the given 100 ml of solution = Amount present in 1000 ml of solution /
10 = ……. /10 = ……… g.

Report:

Amount of sulphuric acid present in the given 100 ml of solution = …….. g.

Precautions:

 II:
Table Care should beerror
Percentage taken while handling the acid and base
 Don’t add excess amount indicator

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Table II: Percentage error

Amount of H 2 SO 4 present in 100 ml of

the given sulphuric acid solution (g) Percentage
Flask No. Grade/Marks Signature of
error
Reported Given Teacher

Inquiry based questions:

1) Give the principle involved in titration of sulphuric acid against NaOH

2) How you will find out the strength of sulphuric acid in lead acid storage cell
3) Apply modern quinoid theory to explain the action of phenolphthalein?
4) Can you directly prepare standard solution of HCl, HNO 3 and H2SO4

***

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8. Estimation of Chromium (VI) in Potassium Dichromate

Learning objectives:
To learn about

 To understand
about dichrometry
reactions of redox
titrations.
 To know the action
of external
indicator and its
structural changes
Significance: during the course
of reaction.
 Chromium is used to harden steel, to manufacture
chromium steels (stainless steel), namely Nickel-
Chromium steels of high tensile strength, more resistant to  To identify the
corrosion and shocks. importance of
phosphoric acid in
 Chromium plating can be used to give a polished mirror
finish to steel. the reaction

 Chromium compounds are used as industrial catalysts and

pigments.
Expt.No:
 Chromium is important in the metabolism of fats and
carbohydrates. Date:

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Aim: Estimation of Chromium (VI) in potassium dichromate by titration against standard solution of
Mohr’s salt.

Theory: Potassium dichromate (K2Cr2O7) acts as an oxidizing agent in the presence of sulphuric acid
or hydrochloric acid oxidizes ferrous iron to ferric iron, getting it self reduced to a green colored
chromic (Cr+3) salt. Mohr’s salt is a reducing agent with the formula (NH 4)2SO4.FeSO4.6H2O. In acid
solution, the reduction of potassium dichromate may be represented as:

K 2Cr2O7 + 4H 2 SO4 ® K 2 SO4 + Cr2 ( SO4 ) 3 + 4H 2O + 3(O)

K 2Cr2O7 + 8HCl ® 2KCl + 2CrCl3 + 4H 2O + 3 (O )

From either of these equations it follows that the equivalent weight of potassium dichromate is one
sixth of the molecular weight. The nascent oxygens so liberated oxidize iron (II) to iron (III).

K 2Cr2O7 + 4H 2 SO4 ® K 2 SO4 + Cr2 ( SO4 ) 3 + 4H 2O + 3(O)

6FeSO4 + 3H 2 SO4 + 3(O ) ® 3Fe2 ( SO4 ) 3 + 3H 2O

K 2Cr2O7 + 7H 2 SO4 + 6FeSO4 ® K 2 SO4 + Cr2 ( SO4 )3 + 3Fe2 ( SO4 )3 + 7H 2O

Diphenylamine (DPA) is used as an external indicator to locate the end point in this titration. Potassium
dichromate, being an oxidizing agent, will also oxidize diphenylamine.

The oxidation of iron (II) to iron (III) imparts green color to the iron (II) solution due to the formation
of chromic sulphate, which deepens to blue green color shortly before the end point of the titration. The
oxidation of DPA imparts intense purple or bluish violet color and it represents the end point of the
titration.

oxidation
NH NH NH
H2
Diphenylamine, DPA colorless

N N

oxidized form of DPA

bluish violet color

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The standard reduction potential values of the active species involved in this titration are as follows.

Species E0Reduction Values

Cr6+/Cr3+ +1.33V
Fe3+/Fe2+ +0.77V
DPA(oxidized)/DPA +0.76V

Following the potential values, it is clear that dichromate having highest value (+1.33V) acts as an
oxidizing agent and it will first oxidize DPA preferentially and then Fe 2+. As a result, the solution in the
conical flask first gets a bluish violet color which then turns to unclear green color. This leads to
ambiguity in sharp detection of the end point. To avoid this, syrupy phosphoric acid is added, which
reacts with Fe3+ forming stable ferric phosphate. In other words, the Fe 3+ ion gets stabilized and more
Fe2+ ions gets oxidized to Fe3+, as a result of which the oxidation potential value of iron increases or, its
reduction potential values decreases. The reduction potential value of iron drops from +0.77V to
+0.62V. As a result, dichromate oxidizes Fe2+ first and then DPA. This facilitate in clear visualization
of the end point.

Species E0Reduction Values

Cr6+/Cr3+ +1.33V
DPA(oxidized)/DPA +0.76V
Fe3+/Fe2+ +0.62V

When once all the ferrous ions completely oxidized with dichromate, an excess drop of dichromate will
oxidize the indicator DPA. This gives a purple or bluish violet color to the solution and it is the
endpoint.

Procedure:

Standardization of Mohr’s salt solution by titrating against a standard solution of potassium

dichromate

10.0 ml of Mohr’s salt solution is pipetted out into a clean conical flask carefully. 40.0 ml of
distilled water, 5.0 ml of 1:1 dilute sulphuric acid and 3.0 ml of syrupy phosphoric acid are added with
measuring flask. One or Two drops diphenylamine indicator is added directly to the conical flask
contents. The burette is rinsed and then filled with standard potassium dichromate solution, the initial
reading is noted, which coincides with the lower meniscus, after removing the air gap from the nozzle.
Now the contents are titrated against potassium dichromate solution with constant thorough shaking
until the color changes from colorless - pale green, - dark green – bluish green to bluish violet, which is
the end point of the reaction. The final reading of the burette is noted without parallax error. Titrations
are repeated until 2 or 3 concurrent results are obtained. The results are tabulated in Table 1.

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Table I: Titration of standard potassium dichromate solution with Mohr’s salt solution.

Normality of standard solution of potassium dichromate = N

Indicator: 1 % diphenylamine solution

Color change at the end point: Bluish green to bluish violet

Volume of Mohr’s salt Burette readings Volume of K2Cr2O7 solution

Sl. No.
solution taken in ml (V1) Initial (ml) Final (ml) consumed in ml (V2)
1
2
3

Calculations:

By the law of equivalence, N1V1 = N2V2

N1 = Normality of Mohr’s salt solution = ?

V1 = Volume of Mohr’s salt solution = ml

N2 = Normality of potassium dichromate solution = N

V2 = Volume of potassium dichromate solution = ml

 N1 = N 2 V2 / V1 =

Report: The normality of Mohr’s salt solution = N

Estimation of chromium (VI) in the given 100 ml of potassium dichromate solution by titrating
against a standard solution of Mohr’s salt.

Procedure: The given potassium dichromate solution is diluted up to the mark of volumetric flask with
distilled water carefully. The flask is stoppered tightly and is shaken thoroughly about 3 to 5 minutes
for complete homogenization. 10.0 ml of standard Mohr’s salt solution is pipetted out into a clean
conical flask carefully. 40.0 ml of distilled water, 5.0 ml of 1:1 dilute sulphuric acid and 3.0 ml of
syrupy phosphoric acid are added with a measuring cylinder. One or Two drops diphenylamine
indicator is added directly to the conical flask contents. The burette is filled with the above potassium
dichromate solution after rinsing with the same solution and then initial reading is noted. Now the
conical flask contents are titrated against potassium dichromate solution with constant thorough
shaking until the color changes from colorless - pale green, - dark green – bluish green to bluish violet,

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which is the end point of the reaction. The final reading of the burette is noted without parallax error.
Titrations are repeated until 2 or 3 concurrent results are obtained. The results are tabulated in Table II.

Table II: Titration of potassium dichromate solution with a standard solution of Mohr’s salt.

Normality of standard solution of Mohr’s salt is = N

Indicator: 1 or 2 drops of diphenylamine solution

Color change at the end point: Bluish green to bluish violet

Volume of Mohr’s salt Burette readings Volume of K2Cr2O7 solution

Sl. No.
solution taken in ml (V3) Initial (ml) Final (ml) consumed in ml (V4)
1
2
3

Calculations:

By the law of equivalence, N3V3 = N4V4

N3 = Normality of Mohr’s salt solution = N

V3 = Volume of Mohr’s salt solution = ml

N4 = Normality of potassium dichromate solution = ?

V4 = Volume of potassium dichromate solution = ml

 N4 = V3 N3 / V4 =

Normality of unknown potassium dichromate solution = N

Eq.wt.of chromium (VI) in potassium dichromate = At. wt./6 =104/6 =17.33

Amount of chromium (VI) present in 1000 ml of solution = Normality of an unknown dichromate

solution  equivalent weight of chromium (VI) = ………  ………= ………. g.

Amount of chromium (VI) present in the given 100 ml solution = Amount present in 1000 ml of
solution / 10 = ……./10 = ……….. g.

Report: The amount of chromium(VI) present in a given 100 ml of an unknown solution is..... g.

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Precautions:
 Care should be taken while preparing cement solution
 There should not be any leakage from burette.
 Before using any solution, shake it properly.
 While noting burette reading for permanganometry much care should be taken since
permanganate is violet colour.

Table III: Percentage error

Amount of calcium present in 100 ml

of cement solution (g)
Percentage
Flask No. Grade/Marks Signature of
error
Reported Given Teacher

Inquiry based questions:

1. Write & explain theory for estimation of chromium (VI) in Potassium dichromate.
2. Write & explain procedure for standardization of Mohr’s salt solution by titrating against a
standard solution of potassium dichromate.
3. Briefly write & explain procedure for estimation of chromium (VI) in the given 100 ml of
Potassium dichromate solution by titrating against a standard solution of Mohr’s salts.
4. Write chemical formula of Potassium dichromate, Mohr’s salt, Sulphuric acid and Hydrochloric
acid.
5. Write chemical structure of diphenylamine indicator.
6. Write structure changes into diphenylamine indicator during colour change.
7. Explain oxidation states changes related to Fe ion and Cr ion in reactant and product during
titration.
8. Define oxidation state and calculate for Mohr’s salt, potassium dichromate, chromic sulfate,
chromic chloride, ferrous sulfate and Ferric sulfate.
9. How to calculate equivalent weight of Chromium (VI) in Potassium dichromate solution.
10. What is the role of using syrupy phosphoric acid in this experiment

*****

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9. Estimation of Copper (II) in a Copper Ore

Learning objectives:
To learn about

 To learn about
iodometric reactions
of redox titrations

 To know role of
starch as an
indicator
 To understand the
Significance: reaction between
copper sulphate
 Copper is a mineral by both the geological and with hypo
nutritional definitions.

 Copper is the most effective conductor of electricity,

used in making of electrical wires, electric circuits, etc.

 Copper is corrosion resistant, ductile and malleable, used

in making industrial machinery and alloys such as Expt.No:
bronze - an alloy of copper and tin and gun metal - an
alloy of copper, zinc and tin. Date:

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Aim: Estimation of copper in the copper ore by titration against a standard solution of hypo through
Iodometric method.

Theory: Copper sulphate has the formula CuSO4.5H2O and hypo with the formula Na2S2O3.5H2O.
Copper sulphate cannot be titrated directly with hypo, (because there is no direct reaction between
them) it can be estimated indirectly via the liberation of iodine from potassium iodide. Copper sulphate
liberates Iodine quantitatively from the solution of potassium Iodide when freed from mineral acids.
The liberated Iodine reacts with hypo. This method is known as indirect Iodometric titration method
(Iodometry). In Iodometric titrations starch is used as an indicator, which gives blue colored complex
even at very low concentrations of iodine. The two redox reactions involved are given below.

2CuSO4 + 4KI ® 2CuI + 2K 2 SO4 + I 2

I 2 + 2Na2 S2O3 ® 2NaI + Na2 S4O6

2CuSO4≡I2≡2Na2SO4

The copper sulphate solution may contain mineral acid impurities, which interfere with the
above reaction by oxidizing iodide to iodine in the presence atmospheric oxygen. Also acid impurities
may interfere with starch indicator making it hydrolyzed.

4I-+O2+4H+ 2I2+2H2O

So adding sodium carbonate can neutralize the above acids. Sodium carbonate also precipitates some of
copper sulphate as copper carbonate. It can be re-dissolved with dilute CH 3 COOH (1:1) (non-mineral
acid).

Procedure:

Standardization of Hypo solution by titrating against a standard solution of copper sulphate.

Procedure: 10.0 ml of standard copper sulphate solution is pipetted out into a clean conical flask
carefully. To this sodium carbonate solution is added drop wise until the solution becomes turbid and
then dilute acetic acid (1:1) is added by drop wise to re-dissolve the precipitate obtained and the
solution becomes clear. Then 10.0 ml of 10% potassium iodide solution is added to the conical flask
with gentle swirling and it is covered with watch glass immediately. After 2 minutes, the solution is
diluted with 30.0 ml of distilled water and the resultant solution is dark brown in color. The burette is
filled with the given hypo solution after rinsing with the same solution. Hypo solution is added drop
wise to the conical flask with constant shaking until the color of solution changes from dark brown –
dark yellow – yellow – pale yellow to wheatish yellow / straw yellow. At this stage 1.0 ml of freshly
prepared starch solution is added and the solution becomes blue in color. The titration is continued drop
wise until the blue color just disappears due to cuprous iodide formation (flesh white), which is the end
point of the titration. The final reading of the burette is noted. A number of titrations are carried out
until 2 or 3 concurrent readings are obtained. The results are tabulated in Table I.

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Table I: Standardization of Hypo solution with standard copper sulphate solution.

Normality of standard copper sulphate solution = N

Indicator: 1 % freshly prepared starch solution

Color change at the end point: Blue to flesh white

Volume of CuSO4 Burette readings Volume of hypo solution

Sl. No.
solution taken in ml (V2) Initial (ml) Final (ml) consumed in ml (V1)
1
2
3

Calculations:

By the law of equivalence, N1V1 = N2V2

N1 = Normality of hypo solution = ?

V1 = Volume of hypo solution = ml

N2 = Normality of copper sulphate solution = N

V2 = Volume of copper sulphate solution = ml

 N1 = N2V2 / V1 =

Report: The normality of hypo solution = N

Estimation of copper in a copper ore by titrating against a standard hypo solution

Procedure: The given copper ore solution (as sulphate) is diluted upto the mark of volumetric flask
with distilled water carefully. The flask is stoppered tightly and is shaken thoroughly about 3-5 minutes
for complete homogenization. 10.0 ml of the copper ore solution is pipetted out into a clean conical
flask carefully. To this sodium carbonate solution is added by drop wise until the solution becomes
turbid. Then dilute acetic acid (1:1) is added by drop wise until the solution becomes clear. Then 10.0
ml of 10% potassium iodide solution is added to the conical flask contents with gentle swirling and
then flask is covered with watch glass immediately for two minutes for complete liberation of iodine.
The solution is then diluted with 30.0 ml of distilled water and the resultant solution is dark brown in
color. The burette is filled with standard Hypo solution. Hypo solution was added drop wise with
constant shaking until the color of solution changes from dark brown – dark yellow – yellow – pale
yellow to wheatish yellow / straw yellow. At this stage 1.0 ml of freshly prepared starch solution is
added to the conical flask and the solution becomes blue in color. Now the titration is continued drop
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wise with thorough shaking until the blue color just disappears (flesh white) which is the end point of
the reaction. The final reading of the burette is noted. A number of titrations are carried out until 2 or 3
concurrent readings are obtained. The results are tabulated in Table II.

Table II: Titration of standard Hypo solution with copper ore solution.

Normality of standard solution of hypo = N

Indicator: 1 % freshly prepared starch solution

Color change at the end point: Blue to flesh white

Volume of copper ore Burette readings Volume of hypo solution

Sl. No.
solution taken in ml (V4) Initial (ml) Final (ml) consumed in ml (V3)
1
2
3

Calculations:

By the law of equivalence, V3 N3 = V4 N4

N3 = Normality hypo solution = N

V3 = Volume of hypo solution = ml

N4 = Normality of copper ore solution = ?

V4 = Volume of copper ore solution = ml

 N4 = N3V3 / V4 =

The normality of copper ore solution= N

Equivalent weight of copper = atomic weight / 1 = 63.6 / 1 = 63.6

Amount of copper present in 1000 ml of solution = normality of copper ore solution  equivalent
weight of copper = ……..  ……. = ……. g.

Amount of copper present in the given 100 ml of copper ore solution = amount present in 1 liter of the
solution / 10 =………/10 = …….. g.

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Report:

The amount of copper present in the given 100 ml of an unknown solution is ……. g

Precautions:

 After the addition of potassium iodide the flask is covered with watch glass for about one /
two minutes for complete liberation of Iodine.
 Starch indicator should be added before the end point.
 Minimum quantities of Na2CO3 solution and CH3COOH are to be added.

Table III: Percentage error

Amount of copper present in 100 ml of

copper ore solution (g)
Flask Percentage Signature of
Grade/Marks
No. error
Reported Given Teacher

Inquiry based questions:

1. Write briefly theory for estimation of copper (II) in a copper ore (5-6 lines).
2. Write briefly procedure for standardization of hypo solution by titrating against a standard
solution of copper sulfate (5-6 lines).
3. Write the chemical formula for copper sulfate and sodium thiosulfate solution (hypo
solution).
4. What is Iodometric (Iodometry) titration?
5. Write name of indicator for experiment.
6. Write name of mineral acids and role in this experiment.
7. What is 10% Potassium iodine solution? Explain
8. Why to wait for 2-3 minute after addition of potassium iodine.
9. Write about all chemical equations involved in this experiment.
10. What is meaning of standard CuSO4 solution.

*****

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10. Determination of Zinc by EDTA Method

Learning objectives:
To learn about

 To understand the
behaviour of EDTA as
chelating agent

 To know the method of

complexometric titration
and estimation of metal in
materials.

Significance:
 To know the stability of
 Zinc is a mineral by both the geological and nutritional complexes at particular
definitions. pH’s

 Zinc is the good material used in galvanisation process,

making of coating of bolts, screws, alloys, etc.
Expt.No:
 Zinc is corrosion resistant, ductile and malleable, used in
making industrial machinery and alloys
Date:

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Aim: Determination of the Zinc (Zn+2) by titrating against a standard EDTA solution using Eriochrome
Black-T (EBT) as indicator.

Theory: Zinc present in a given sample can be determined by using the complexometric method, in
which the disodium salt of EDTA is employed (soluble in water) and it can be represented as follows.

(EDTA – Ethylene Diamine Tetra Acetic acid)

HOOCH2C CH 2COOH
N-CH2-CH 2-N
NaOOCH2C CH 2COONa

EDTA forms complexes with zinc when the pH is in the range of around 9.5 to 10.5 and to maintain the
pH, a basic buffer solution is used (NH4OH + NH4Cl buffer serves pH 9.5 to 10.5). The complexes of
Zinc with EDTA are colorless, therefore it is necessary to use indicator to locate the end point. In this
titration Eriochrome black – T is used as indicator, which forms an unstable wine red colored complex
with Zinc, calcium and magnesium.. So the color change at the end point is wine red to blue. (M
=Metal ions, Zn+2 )

pH=10 EDTA
M + EBT M-EBT M-EDTA + EBT
(Blue colour) (Unstable complex) ( Stable complex) (Blue colour)
Wine red colour Colourless

The di-sodium salt of EDTA solution can be standardized by using standard zinc sulphate solution in
presence of ammonia – ammonium chloride buffer (pH 10) using Eriochrome Black – T as indicator.

Zn+2+H2Y -2 ZnY -2+2H+

Procedure: a) Standardization of EDTA solution using known zinc solution :10 ml of Zinc solution is
pipetted out into a clean conical flask. To this 2 or 3 ml of ammonia - ammonium chloride buffer
solution (pH 9.5 – 10.5) and 2 or 3 drops of Eriochrome Black – T indicator are added. (If necessary 2
drops of 0.1 M Mg-EDTA complex is added in order to get the clear end point). The burette is filled
with 0.01 M EDTA solution, after rinsing with it and the initial reading is noted. Now the contents in
conical flask are titrated with EDTA solution until the color changes from wine red to blue, which is
the end point of the reaction. The final reading of the burette is noted. Titrations are repeated until 3 or
4 concurrent readings are obtained. The results are tabulated in Table I.

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Table I: Titration of standard Zinc solution with EDTA

Molarity of standard solution of Zinc = 0.1 M

Indicator: Eriochrome black-T.

Color change at the end point: Wine red to blue

Volume of Zinc solution Burette readings Volume of EDTA solution

Sl. No.
taken in ml (V2) Initial (ml) Final (ml) consumed in ml (V1)
1
2
3

Calculations:

By the law of equivalence, M1V1 = M2V2

M1 = Molarity of EDTA solution = ?

V1 = Volume of EDTA solution = ml

M2 = Molarity of Zinc solution = 0.1 M

V2 = Volume of Zinc solution = ml

 M1 = M2V2 / V1 =

Report: The Molarity of EDTA solution, M1 = M

b) Standardization of EDTA solution using known zinc solution :10 ml of unknown zinc solution is
pipetted out into a clean conical flask. To this 2 or 3 ml of ammonia - ammonium chloride buffer
solution (pH 9.5 – 10.5) and 2 or 3 drops of Eriochrome Black – T indicator are added. (If necessary 2
drops of 0.1 M Mg-EDTA complex is added in order to get the clear end point). The burette is filled
with 0.01 M EDTA solution, after rinsing with it and the initial reading is noted. Now the contents in
conical flask are titrated with EDTA solution until the color changes from wine red to blue, which is
the end point of the reaction. The final reading of the burette is noted. Titrations are repeated until 3 or
4 concurrent readings are obtained. The results are tabulated in Table II

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Table II: Titration of standard EDTA solution with Unknown zinc solution

Molarity of standard solution of EDTA = M

Indicator: Eriochrome black-T.

Color change at the end point: Wine red to blue

Volume of unknown Burette readings

Sl. No. Volume of EDTA solution
Zinc solution taken in ml
Initial (ml) Final (ml) consumed in ml (V1)
(V2)
1
2
3

Calculations:

By the law of equivalence, M3V3= M4V4

M3 = Molarity of EDTA solution = M

V3 = Volume of EDTA solution = ml

M4 = Molarity of Zinc solution = M

V4 = Volume of Zinc solution = ml

 M3 = M4V4 / V3 =

Report: The Molarity of Zinc solution, M4 = M

Equivalent weight of Zinc = atomic weight / 1 = 65.38 / 1 = 65.38

Amount of zinc present in 1000 ml of solution = molarity of zinc solution (M 4)  equivalent weight of
zinc = ……..  ……. = ……. g.

Amount of copper present in the given 100 ml of zinc solution = amount present in 1 liter of the
solution / 10 =………/10 = …….. g.

Report: The amount of zinc present in given unknown sample = ……

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Precautions:
 The fumes from the NH3/NH4Cl buffer at pH 10 are toxic, corrosive, and irritating. Wash
hands thoroughly before leaving the lab.
 Eriochrome black-T is a dye stuff and avoid direct contact since it cause eye irritation and
skin irritation.
 Don’t add excess amount indicator to avoid error.

Table III: Percentage error

Amount of zinc present in 100 ml of

unknown zinc solution (g)
Flask Percentage
Grade/Marks Signature of
No. error
Reported Given Teacher

Inquiry based questions:

1. Write the theory behind the determination of hardness of a ground water sample by EDTA method?
2. Write the procedure behind the determination of hardness of a ground water sample by EDTA method?
3. What are complexometric titrations?
4. Write the structure of EDTA? How many binding sites are there for EDTA?
5. What is buffer? How it maintains the constant pH of any solution?
6. What is basic buffer? Give one example for basic buffer?
7. Write the colour of the following compounds?
a) EDTA b) EBT c) (M) EDTA d) (M) EBT e) EBT (M=Zn)
8.EDTA is forming complexes efficiently with Ca and Mg metal mixtures in hard water but not efficient
with the individual metals why?
9. What observations you found when the colour of the complexes changes from wine red to blue?

***

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11. Determination of Hardness of a Ground Water Sample

Learning objectives:
To learn about

 To understand the chemical

basis of water hardness and
how it originates and way it
can affect other parameters
 To know the method of
measuring and expressing
hardness and its
relationship with other
water quality parameters.
Significance:  To know the significance of
 Water hardness can be a really hassle if it exceeds the
water hardness in
permissible amounts. environmental engineering.

 Hard water requires more soap and synthetic

detergents for home laundry and washing and
contributes to scaling in boilers and industrial Expt.No:
equipment.
Date:

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Aim: Determination of the total hardness of the given sample of water by titrating against a standard
EDTA solution using Eriochrome Black-T (EBT) as indicator.

Theory: Hardness present in a given sample of water can be determined by using the complexometric
method, in which the disodium salt of EDTA is employed (soluble in water) and it can be represented
as follows.

(EDTA – Ethylene Diamine Tetra Acetic acid)

HOOCH2C CH 2COOH
N-CH2-CH 2-N
NaOOCH2C CH 2COONa

EDTA forms complexes with calcium and magnesium when the pH is in the range of around 9.5 to
10.5 and to maintain the pH, a basic buffer solution is used (NH 4OH + NH4Cl buffer serves pH 9.5 to
10.5). The complexes of calcium and magnesium with EDTA are colorless, therefore it is necessary to
use indicator to locate the end point. In this titration Eriochrome black – T is used as indicator, which
forms an unstable wine red colored complex with calcium and magnesium. Calcium ions complexed
first with EDTA, but the color change does not occur until all the magnesium has also completely
reacted. It is thus possible to determine the total amount of these metals in the solution and the total
hardness can be calculated. Calcium itself does not give a satisfactory end point with Eriochrome black
– T indicator unless the solution also contains magnesium. When once all the calcium and magnesium
ions are completely removed by EDTA,free indicator is left in the solution which imparts blue color to
the solution. So the color change at the end point is wine red to blue. (M =Metal ions, Ca+2 and Mg+2)

pH=10 EDTA
M + EBT M-EBT M-EDTA + EBT
(Blue colour) (Unstable complex) ( Stable complex) (Blue colour)
Wine red colour Colourless

The di-sodium salt of EDTA solution can be standardized by using standard zinc sulphate solution in
presence of ammonia – ammonium chloride buffer (pH 10) using Eriochrome Black – T as indicator.

Zn+2+H2Y -2 ZnY -2+2H+

Procedure: 50.0 ml of sample of hard water is pipetted out into a clean conical flask. To this 2 or 3 ml
of ammonia - ammonium chloride buffer solution (pH 9.5 – 10.5) and 2 or 3 drops of Eriochrome
Black – T indicator are added. (If necessary 2 drops of 0.1 M Mg-EDTA complex is added in order to
get the clear end point). The burette is filled with 0.01 M EDTA solution, after rinsing with it and the
initial reading is noted. Now the contents in conical flask are titrated with EDTA solution until the

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color changes from wine red to blue, which is the end point of the reaction. The final reading of the
burette is noted. Titrations are repeated until 3 or 4 concurrent readings are obtained. The results are
tabulated in Table I.

Table I: Titration of standard EDTA solution with unknown water sample

Morality of standard solution of EDTA = M

Indicator: Eriochrome black-T.

Color change at the end point: Wine red to blue

Volume of water sample Burette readings Volume of EDTA solution

Sl. No.
taken in ml (V1) Initial (ml) Final (ml) consumed in ml (V2)
1
2
3

Calculations:

1 gram mol.weight of EDTA = 1 gram mol.weight of calcium carbonate

1 gram mol.weight of EDTA dissolved in 1000 ml of solution gives one molar solution

1000ml of 1 M EDTA = 100 g of calcium carbonate

1.0 ml of 1 M EDTA = 0.1 g of calcium carbonate

1.0 ml of 0.01 M EDTA = 0.001 g of calcium carbonate

1.0 ml of 0.01 M of EDTA equivalent to 1.0 mg of calcium carbonate equivalent hardness

50.0 ml of hard water samples consumes ‘X’ ml of 0.01 M EDTA solution

 Total hardness of water sample per liter = X  1000 / 50 = X  20 mg/l or ppm.

Report: The total hardness of the given water sample = ……. mg/l or ppm.

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Precautions:
 The fumes from the NH3/NH4Cl buffer at pH 10 are toxic, corrosive, and irritating. Wash
hands thoroughly before leaving the lab.
 Eriochrome black-T is a dye stuff and avoid direct contact since it cause eye irritation and
skin irritation.
 Don’t add excess amount indicator to avoid error.

Roll No Report on water quality Grade/Marks Signature of

Teacher

Inquiry based questions:

1. Write the theory behind the determination of hardness of a ground water sample by EDTA method?
2. Write the procedure behind the determination of hardness of a ground water sample by EDTA method?
3. What are complexometric titrations?
4. Write the structure of EDTA? How many binding sites are there for EDTA?
5. What is buffer? How it maintains the constant pH of any solution?
6. What is basic buffer? Give one example for basic buffer?
7. Among the following complexes A, B which one is stable and Why?
O M
O
HO3S
N N

O2N

A B M=Ca +2, Mg+2

8. Write the colour of the following compounds?

a) EDTA b) EBT c) (Mg, Ca) EDTA d) (Mg, Ca) EBT e) EBT
9. EDTA is forming complexes efficiently with Ca and Mg metal mixtures in hard water but not
efficient with the individual metals why?
10. What observations you found when the colour of the complexes changes from wine red to blue?

***

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 Engineering Chemistry Lab Manual

12. Estimation of Calcium in Portland cement

Learning objectives:
To learn about

 To understand the
role of self
indicator in
permanganometry

 To know the
composition of
cement and role of
Significance: calcium content.
 Calcium constitutes the major component of cement,
contributing to about > 65% of the total composition
 To know the
of cement. nature of
permanganate ion
 Calcium (in the form of oxides and silicates) gives in redox titrations
the desired high strength and hardness to cement.

Expt. No:
Date:

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Aim: Estimation of calcium (as oxide) in the given sample of portland cement by using potassium
permanganate solution.

Theory: Metals like calcium, copper, lead and zinc which can be estimated by dissolving their
sparingly soluble oxalates in dilute sulphuric acid and titrating with standard potassium permanganate
solution. This method is widely used for the estimation of calcium. Calcium is precipitated as oxalate
by the addition of ammonium oxalate solution to a dilute hydrochloric acid solution of the cement
followed by the neutralization of the acid with dilute ammonia solution. The precipitated calcium
oxalate is acidified with dilute sulphuric acid to liberate oxalic acid.

Cement + HCl ® CaCl2 + Excess HCl

Excess HCl + NH 4OH ® NH 4Cl + H 2O (Neutralization)

CaCl2 + ( NH 4 ) 2 C2O4 ® CaC2O4 + NH 4Cl

CaC2O4 + H 2 SO4 ® CaSO4 + H 2C2O4

Potassium permanganate is an oxidizing agent with the formula KMnO 4 and oxalic acid is a
reducing agent with the formula H2C2O4.2H20. Potassium permanganate is standardized by titrating
with standard oxalic acid solution in acidic medium. Calcium from Portland cement is estimated by
tirating the liberated oxalic acid solution from calcium oxalate with standard potassium permanganate
solution.

2KMnO4 + 3H 2 SO4 ® K 2 SO4 + 2MnSO4 + 3H 2O + 5 (O)

5H 2C2O4 + 5 (O) ®10CO2 + 5H 2O

2KMnO4 + 3H 2 SO4 + 5H 2C2O4 ® K 2 SO4 + 2MnSO4 + 8H 2O +10CO2

In these reactions all the reactants and products are colorless except potassium permanganate.
The color of potassium permanganate is used to locate the end point and one of the products i.e., Mn +2
ions act as catalyst to catalyze the preceding reaction. So this is an example of self indicator and auto
catalytic reaction.

Procedure:

1. Extraction of calcium as calcium oxalate from cement: About 5.0 g. of portland cement are
accurately weighted into a 600 ml beaker, covered with a watch glass, and dissolved in 1:4
hydrochloric acid. The contents of the beaker are heated to boiling. The solution is now filtered and the
residue on the filter paper is washed a number of times with a little acid. The filtrate and washings are
boiled and made ammonical with 1:4 ammonia. The precipitate formed is allowed to settle and the
solution is filtered. The precipitate is then washed with hot water. Both filtrate and washing are diluted
to 1000 ml. Then the solution is boiled and from this hot solution calcium is precipitated as the calcium
oxalate by the addition of strong ammonium oxalate solution. Boiling is continued for 10 minutes and
the precipitate is allowed to settle. A drop of ammonium oxalate is added to the supernatant solution to

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ensure that precipitation is completed. Now the solution is filtered through whatmann filter paper
followed by washing with cold water until it is free from oxalate and chloride. Filtrate is tested for the
presence of calcium with ammonium oxalate solution. A hole is pierced in the filter paper with a
pointed glass rod, and the bulk of precipitate is washed with little amount of hot water into the
volumetric flask. The filtrate is treated with dilute sulphuric acid (1:8) and finally filter paper is washed
with hot water. If necessary some more dilute sulphuric acid is added to dissolve completely.

2. Standardization of potassium permanganate solution by titrating against a standard oxalic

acid solution

10.0 ml of standard oxalic acid is pipetted out into a clean conical flask carefully and to this 45.0 ml
of distilled water followed by 5.0 ml of 1:1 dilute sulphuric acid are added with a measuring jar. The burette
is filled with potassium permanganate solution after rinsing with the same. Now the conical flask contents
are heated to just boiling which will be indicated by commencement of bubbles from the bottom of the
flask. After noting the initial reading of the burette a small portion (~ 0.5 ml) of potassium permanganate is
added to the hot solution of conical flask and the flask is kept in undisturbed position until the
permanganate solution is decolorized to produce the sufficient amount of Mn +2 ions, which catalyze the
preceding reaction. Now the titration is continued while hot with permanganate solution until the pale pink
color is obtained. The final reading of the burette is noted which coincides with upper meniscus. A number
of titrations are carried out until 2 or 3 concurrent readings are obtained. The results are tabulated in Table I.

Table I: Titration of potassium permanganate solution with standard oxalic acid solution.

Normality of standard solution of oxalic acid = N

Indicator: Self indicator (color of the potassium permanganate)

Color change at the end point: Colorless to pale pink.

Volume of oxalic acid Burette readings Volume of KMnO4 solution

Sl. No.
solution taken in ml (V1) Initial (ml) Final (ml) consumed in ml (V2)
1
2
3

Calculations: By the law of equivalence, N 1V1 = N 2V2

N1 = Normality of oxalic acid solution = N

V1 = Volume of oxalic acid solution = ml

N2 = Normality of potassium permanganate solution = ?

V2 = Volume of potassium permanganate solution = ml

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 N2 = N1V1 / V2 =

Report: The normality of potassium permanganate solution = .......... g

3. Estimation of calcium present in a given 100 ml of unknown cement solution by titrating

against a standard solution of potassium permanganate

Procedure: The Potassium permanganate solution is standardized using standard oxalic acid solution
(refer Part-I of experiment No. 4). The given cement solution is diluted up to the mark of volumetric
flask with distilled water carefully. The flask is stoppered tightly and is shaken thoroughly about 3 to 5
minutes for complete homogenization. 10.0 ml of cement solution is pipetted out into a clean conical
flask carefully and to this 45.0 ml of distilled water followed by 5.0 ml of 1:1 dilute sulphuric acid are
added. The burette is filled with standard potassium permanganate solution. Now the conical flask
contents are heated to just boiling. After noting the initial reading of the burette a small portion (~ 0.5
ml) of potassium permanganate is added to the hot solution and kept it in undisturbed position until the
de-colorization of the permanganate solution. Now the titration is continued while hot with
permanganate solution until the color changes from colorless to pale pink. The final reading of the
burette is noted. Titrations are repeated until 2 or 3 concurrent readings are obtained. The results are
tabulated in Table II.

Table II: Titration of standard potassium permanganate solution with an unknown cement
solution.

Normality of standard solution of potassium permanganate = N

Indicator: Self indicator (Color of the potassium permanganate)

Color change at the end point: Colorless to pale pink.

Volume of cement Burette readings Volume of KMnO4 solution

Sl. No.
solution taken in ml (V3) Initial (ml) Final (ml) consumed in ml (V4)
1
2
3

Calculations:
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By the law of equivalence, N 3V3 = N4V4

N3 = Normality of unknown cement solution = ?

V3 = Volume of unknown cement solution = ml

N4 = Normality of potassium permanganate solution = N

V4 = Volume of potassium permanganate solution = ml

 N3 = N4V4/ V3 =

The normality unknown cement solution = N

Equivalent weight of calcium in cement = Molecular weight /2= 40 / 2=20

Amount of calcium present in 1000 ml of solution = Normality of unknown calcium in cement solution
 equivalent weight of calcium = ……..  ………. = ………. g.

Amount of calcium present in a given 100 ml of cement solution = Amount present in 1000 ml solution
/10 = ……./10 = ……… g.

Report:

The amount of calcium present in the 100 ml of the given unknown cement solution = ……. g.

Precautions:
 Care should be taken while preparing cement solution
 There should not be any leakage from burette.
 Before using any solution, shake it properly.
 While noting burette reading for permanganometry much care should be taken since
permanganate is violet colour.

*****

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Table III: Percentage error

Amount of calcium present in 100 ml

of cement solution (g)
Percentage
Flask No. Grade/Marks Signature of
error
Reported Given Teacher

Inquiry based questions:

1. Write & explain theory for estimation of calcium in Portland cement.

2. Write & explain procedure for standardization of calcium present in cement solution by titrating
against a standard solution of potassium permanganate.
3. How to make cement solution.
4. Why the name ‘Portland cement’ was given?
5. What is the catalyst used in the reactions?
6. What indicator is used in the reactions?
7. What type of reactions does it belong to and why?.
8. What colour change if observed at the end of the reactions.
9. Explain oxidation states changes related to Mn ion during titration.
10. Why the contents of the conical flask is heated to boiling during titration.
11. Why a small portion of KMnO4 is added to hot solution of the conical flask.
12. What is the equivalent weight of calcium in Portland cement solution.

*****

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 Engineering Chemistry Lab Manual

13. Estimation of available Chlorine Content in Bleaching Powder

Learning objectives:
To learn about

 To understand how
chlorine was estimated
after mix of bleaching
powder with water
 To know the method of
measuring and
expressing available
chlorine in water
 To know about
Significance: iodometric titrations

 Proper application of chlorine in the form of

bleaching powder will produce bacteria-free water
and eliminate algae and slime.

 Bleaching powder used for domestic should have

1–2% of available chlorine and for the one used Expt. No:
for commercial purposes must contain 40%
available chlorine. Date :
 Exposure to water having higher amounts of
chlorine causes gastrointestinal problems, cancer,
etc.

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Aim: Determination of the amount of available chlorine in the given sample of bleaching powder by
using standard Hypo solution through Iodometric method.

Theory: Bleaching powder consists essentially of a mixture of Ca(OCl) Cl and basic chloride [CaCl 2,
Ca(OH)2. H2O]. The active constituent of the bleaching powder is hypochlorite, which is responsible for
the bleaching action of the material. This is very good disinfectant in water, which is due to the
formation of nascent oxygen.

CaOCl2 + H 2O ® Ca (OH ) 2 + Cl2

Cl2 + H 2O ® HOCl + HCl (HOCl is a germicide)

HOCl ® HCl + [O] (nascent oxygen is responsible for bleaching action)

In the evaluation of bleaching powder the result is usually expressed in terms of available chlorine,
which is the chlorine liberated in acidic solution. Available chlorine can be determined iodometrically
by adding potassium iodide and acetic acid to the suspension of the material.

OCl-+Cl-+2H+ H2O+Cl2
Cl2 + 2KI ® 2KCl + I 2

In acetic acid medium the reaction proceeds slowly. The liberated chlorine in presence of acid liberates
iodine quantitatively from the solution of potassium iodide. This liberated iodine can be titrated with
the standard solution of sodium thiosulphate.

I 2 + Na2 S2O3 ® 2NaI + Na2 S4O6

In iodometric titrations starch is used as an indicator to locate the end point. Starch forms soluble blue
colored complex with iodine even at low concentrations.

Procedure:

Preparation of Bleaching powder solution: The given sample of bleaching powder is weighed out
accurately into clean glass mortar. A little water is added and the mixture is ground in to a smooth paste
with a pestle. Then little more water is added to this paste and mixed thoroughly, allowed to settle, and
the milky liquid is poured into a 100 ml volumetric flask. Then the residue is grounded well with a little
more water and the operations are repeated until the whole of the sample has been transferred into the
flask either in solution or in a state of very fine suspension. The flask is then filled up to the mark with
distilled water and is shaken thoroughly.

The given bleaching powder solution is diluted up to the mark with distilled water carefully and
stoppered well. The solution is shaken thoroughly for 3 to 5 minutes for complete homogenization. 10.0
ml of well shaken bleaching powder solution or suspension is pipetted out into a clean conical flask and

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to this 50.0 ml of distilled water, 10.0 ml of 10% potassium iodide solution are added using a
measuring flask. Then the above solution is acidified by adding 10.0 ml of glacial acetic acid and the
flask is covered with watch glass for about 5 minutes for complete liberation of iodine. The burette is
filled with standard hypo solution and the initial reading is noted. The brown colored solution (liberated
iodine) is then titrated with standard hypo solution drop wise with constant shaking until the brown
color becomes pale yellow. At this stage 1.0 ml of 1% freshly prepared starch solution is added to this
solution and the color changes to blue. The titration is continued until an excess drop of hypo solution
changes the color of the solution from blue to colorless (disappearance of blue color), which is the end
point of the reaction. The final reading of the burette is noted. Titrations are repeated until 2 or 3
concurrent readings are obtained. The results are tabulated in Table I.

Table I: Titration of bleaching powder suspension with a standard hypo solution.

Normality of standard solution of hypo = N

Indicator: 1 % freshly prepared starch solution

Color change at the end point: Blue to colorless (disappearance of blue)

Volume of bleaching Burette readings

Sl. No. Volume of hypo solution
powder solution taken in
Initial (ml) Final (ml) consumed in ml (V2)
ml (V1)
1
2
3

Calculations:

According to the law of equivalence

1000 ml of 1 N hypo solution = 35.46 g. of chlorine

1.0 ml of 1 N hypo solution = 0.03546 g. of chlorine

1.0 ml of 0.1 N hypo solution = 0.003546 g. of chlorine

10.0 ml of bleaching powder suspension of consumed ‘X’ ml of 0.1 N hypo solution. 

Amount of chlorine present in the given 100 ml of solution = 10  X  0.003546 g.

10  X  0.003546  100
The percentage of available chlorine =
Weight of bleaching powder taken

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Report:

The percentage of available chlorine in given bleaching powder sample = ………

Precautions:
 Starch solutions should be freshly prepared
 In each titration same amount of indicator, KI and acetic acid should be added.
 There should not be any leakage from burette
 While taking reading from burette, eye should be parallel to it.
 Before using any solution, shake it properly

Table II: Percentage of error

Roll No Report on water quality Grade/Marks Signature of

Teacher

Inquiry based questions:

1. Write the theory behind the estimation of chlorine in bleaching powder?

2. Write the procedure behind the estimation of chlorine in bleaching powder?
3. What are Iodometric titrations?
4. Write the composition of bleaching powder?
5. What is the active species of beaching powder when we subject it for hydrolysis?
6. What type of media is required for the liberation of Iodine and Why?
7. Why people are closing the lid after acidifying the reaction mixture in chlorine experiment?
8. Which form of Iodine species is involving in the formation of Iodine Starch complex?
9. Write the reaction between hypo with Iodine?
10. What is law of equivalence? How many grams of hypo is equivalent to one chlorine atom

***

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14. Preparation of Phenol-Formaldehyde resin

Learning objectives:
To learn about

 To understand the
polymerisation process

 To learn behaviour of
phenol and formaldehyde
in organic reaction

Significance:  To know the role of acid

catalyst in formation of
polymer

Expt.No:
Date:

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AIM:- To prepare phenol formaldehyde resin.

Apparatus:- Beaker, glass rod, funnel, filter paper, and chemical balance.

Chemicals:- Phenol formaldehyde, conc. HCl, glacial acetic acid, distilled water.

Theory:- Phenolic resins are condensation polymerization of phenolic derivatives (like

phenol, resorcinol) with aldehyde (like formaldehyde, furfural). Most important member of this
class is bakelite or phenol formaldehyde resin.
Phenol formaldehyde is prepared by condensing phenol with formaldehyde in presence of acidic or
alkaline catalyst. The initial reaction result in the formation of o- and p-hydroxy methyl phenol, which

react to form linear polymer novalac. During moulding hexamethyline tetramine [ (CH 2)6N4] is added
which convert the fusible novalac in to hard infusible and insoluble solid of cross – linked structure
known as Bakelite.

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Procedure:-
1. Place 5 ml of glacial acetic acid and 2.5 ml of 40% formaldehyde solution in a 100 ml
beaker .
2. Add 2 g of phenol to it.
3. Wrap a cloth loosely round the beaker. Add a few ml of conc. HCl in to the mixture
carefully and heat it slightly.
4. A large mass of plastic pink in colour is formed.
5. A residue is washed with water and filtered.
6. The product dried and yield is weighed.

Precautions:-
1. While adding conc. HCl, it is better to stay little away from the beaker since the reaction
sometimes becomes vigorous.
2. The reaction mixture should be stirred continuously.

Observations:-
Mass of the beaker (W1) = ---------g.
Mass of the beaker with phenol formaldehyde (W2) = --------g.
Therefore mass of phenol formaldehyde (W2 – W1) = --------g.

Percentage of error:
Roll No Reported value Given value Grade/Marks Signature of
Teacher

Result: - The yield of phenol formaldehyde is = --------g

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15. Preparation of Urea-Formaldehyde resin

Learning objectives:
To learn about

 To understand the
polymerisation process

 To learn behaviour of urea

and formaldehyde in organic
reaction

 To know the role of acid

catalyst in formation of
polymer

Expt.No:
Date:

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AIM:- To prepare urea formaldehyde resin.

Apparatus required:- Beaker, glass rod, funnel, filter paper and chemical balance.
Chemicals:- Urea, formaldehyde sol., conc. H2SO4, distilled water.
Theory:- Amino resins are condensation products obtained by the reaction of formaldehyde with
nitrogen bearing compounds such as aniline, amides for ex:- melamine formaldehyde, urea
formaldehyde etc. Urea formaldehyde is prepared by condensation reaction between urea and
formaldehyde in acidic or alkaline medium.
The first product formed during the formation of resin is monomethylol and dimethylol ureas.

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Procedure:-
1. Place about 5 ml of 40% formaldehyde solution in 100 ml beaker.
2. Add about 2.5 g of urea with constant stirring till saturated solution is obtained.
3. Add a few drops of conc. H2SO4, with constant stirring.
4. A voluminous white solid mass appears in the beaker.
5. Wash the white solid with water and dry it in the folds of filter paper.
6. Weight the yield of product
Precautions:-
1. While adding concentrated H2SO4, it is better to stay little away from the beaker since the
reaction sometimes becomes vigorous.
2. The reaction mixture should be stirred continuously.
Observations:-
Mass of the beaker (W1) = ---------g.
Mass of the beaker with urea formaldehyde (W2) = --------g.
Therefore mass of urea formaldehyde (W2 – W1) = --------g.
Percentage error:

Roll No Reported value Given value Grade/Marks Signature of

Teacher

Result:- The yield of urea formaldehyde = -------g

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16. Thin Layer Chromatography

Learning objectives:
To learn about

 To understand the
principle involved in
chromatography

 To identify impurity
present in materials
Significance:

 To know the behaviour of

mobile phase and
stationary phase

Expt.No:
Date:

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Aim: To separate the aminoacids using thin layer chromatography method

Apparatus: TLC jar (An alternative is a beaker covered by a watch glass or aluminum foil), Spotting capillaries ,
Measuring cylinder100 cm3, TLC plates (Either arranged from a supplier or prepared by the teacher) and Spraying
bottle

Chemicals:
Propanol-1, Conc. Ammonia solution
Any three amino acid from the following:L-alanine, L-Leucine, L-Lysine, L-Aspartic acid, Methionine

Preparation of TLC Plates

TLC plates can be prepared by one of the following methods:
A. Dipping: Combine 33cm3 of methanol and 67 cm3 of chloroform in a 125 cm3 screw-cap jar, stir in 35g of Silica
Gel G, and shake the capped jar vigorously for about a minute, Stack two clean microscope slides back-to-back,
holding them together at the top. Without delay dip them into the slurry for about 2 seconds, Touch the bottom of the
stacked slides to the jar to drain off the excess slurry, let them air dry a minute or so to evaporate the solvent, separate
them and wipe the excess adsorbent off the edges with a tissue paper. Activate the slides by heating them in oven at
ll0°C for 15 minutes, or by placing them in a covered beaker heated to that temperature.

B. Spreading: Take a clean glass plate Mix about 10 g of Silica Gel G with 20 cm3 of water (stirring and shaking
well to get out any lumps) and pour on the glass plate. Spread it out with the help of TLC applicator. Let the plate air
dry for ten minutes and put plate at 110°C in a oven for at least 30 minutes to activate the adsorbent

Solutions provided

1. Sample Solution:
Provide solution of any three amino acid as above. Make one of amino acid solution as unknown sample. Their
solution can be prepared by dissolving 15 mg of each amino acid separately in 1 cm3 of distilled water. Warm if a
particular amino acid is not soluble in cold.
2. Detector:
Ninhydrin Reagent (0.2%): Take 100 cm3 of I-butanol and 100 cm3 of water in a separatory funnel. Shake gently and
allow it to from the layers. Remove the lower aqueous layer. Transfer the upper organic layer to a sprayicg.bottle and
to this add 0.2 g of ninhydrin; shake well and use as the detector for amino acids.

Procedure:

1. Preparation of Developer: Prepare the developer by mixing 1- propanol and concentrated ammonia in the
proportion of 7:3 respectively by measuring the required volumes with the help of a measuring cylinder.

2. Take 4 silica gel coated TLC plates from your teacher.

3. Dry the plates in an oven for 30 minutes at 100"C, so that they have been activated for adsorption
chromatography.
4. Take a plate and make a light pencil line across it, 1 cm above the bottom of the plate and put a short mark at
the line centre where a known or unknown amino acids will be spotted.
5. Label the plate at the top end to indicate known or unknown amino acids.

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6. Hold the plate in the left hand cautiously, so that the fingers do not touch the adsorbent layer. Take a capillary
and place in the solution of amino acid to be spotted, let the solution rise into the capillary, take out the capillary
from the solution and gently touch the capillary to the layer side of the TLC plate at the marked centre. Allow to
flow the solution on the plate for a short duration so that a spot of the solution is formed but not larger than 2 mm
in diameter.(Note: The teacher is supposed to demonstrate this technique).

7.Allow the spot to dry. You can blow in order to aid evaporation. Apply more solution at the same place (if
required). The aim is to apply a small but visible and built up spot.

8. Apply lhe unknown solution on a separate TLC plate in a similar manner.

9. After spotting all the known and unknown solutions, insert the plates into the developing jars (one plate in
each jar).

10. Pour the mobile phase into the chamber, with the help of a pipette till the developer level reaches nearly at 1
cm height of the lower edge of the adsorbent layer on the plate (Remember that the spot should be above this
level).

11. Cover the jar and allow the devloper to ascend along the plate. The position of the solvent front can be seen
visually as the damp portion of the plate appears darker than the dry portion.

12. When the developer ascends to a required height on the plate, remove the plate from the developing chamber,
mark the solvent front and dry the plate at 100°C for about 10 minutes.

13. After the plates have been dried, spray the detector on the plates with the help of a spraying bottle. The
detector is 0.2% ninhydrin solution in butanol saturated with water.

14. Heat the plates at llO°C, either in an oven or on a hot plate, for 5-10 minutes, till the zones of amino acids
appear as coloured spots on the plates.

15. Mark the periphery of the coloured spots and their centres.

16. Measure the distance of each spot-centre from the starting line and also the distance by which the solvent
front, has moved. Calculate the Rf values.

17. From the comparison of Rf values of known and unknown samples you can determine which amino acids are
present in your unknown.

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Observations and calculations:

Observe the colour of the spots of various amino acids on TLC plates. Measure the distance to which the centre
of the amino acid has moved from the original (ds), and the distance which the solvent front has moved from the
point of application (dm) on the chromatoplate. Calculate the Rf values by the relation. Rf = ds/dm, for table
below. Each known amino acid and for the unknown.

Percentage of error:

Roll No Report on aminoacids Grade/Marks Signature of

Teacher

Report: The Rf value of unknown amino acid and reported as________________

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17. Preparation of ZnO nanoparticles

Learning objectives:
To learn about

 To learn the method of

preparation of ZnO
nanoparticles

Significance:  To understand the

working principles of
electric furnace and
centrifuge

 To know the method of

precipitation in
preparation of
nanoparticles

Expt.No:
Date:
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Aim: To Prepare the nanoparticles of zinc oxide using direct precipitation method

Apparatus: Beakers-250ml, Heating mantle, Centrifuge and furnace

Chemicals required : Zinc nitrate, Potassium hydroxide, absolute alcohol

Principle: Zinc oxide, with its unique physical and chemical properties, such as high chemical
stability, high electrochemical coupling coefficient, broad range of radiation absorption and high
photostability, is a multifunctional material.. ZnO nanoparticles were synthesized by different methods.
It is confirmed that the various applications of ZnO nanoparticles depend upon the control of both
physical and chemical properties such as size, size dispersity, shape, surface state, crystal structure,
organization onto a support, and dispensability. This has led to the development of a great variety of
techniques for synthesizing the compound. By using the precipitation method, nanoparticles of ZnO
was prepared as follows

Method: ZnO nanoparticles were synthesized by direct precipitation method using zinc nitrate and
KOH as precursors. In this work, the aqueous solution (0.2 M) of zinc nitrate (Zn(NO3)2.6H2O) and
the solution (0.4 M) of KOH were prepared with deionized water, respectively. The KOH solution was
slowly added into zinc nitrate solution at room temperature under vigorous stirring, which resulted in
the formation of a white suspension. The white product was centrifuged at 5000 rpm for 20 min and
washed three times with distilled water, and washed with absolute alcohol at last. The obtained product
was calcined at 500 °C in air atmosphere for 3 hr. In this method , the ZnO nanoparticles were
successfully synthesized by direct precipitation method using zinc nitrate as zinc source and KOH as
precipitating agent in aqueous solution. The size range of the generated ZnO powder was
approximately 20–40 nm. Finally the size, structure and morphology of ZnO nanoparticles was
determined by XRD, SEM and TEM techniques

Report: The amount of ZnO nanoparticles are ________grams has 20-40nm in size

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18. SEM (Scanning Electron Microscope) analysis of nanomaterials

Learning objectives:
To learn about

 To understand the
underlying principle of
SEM

 To interpret the
Structure, composition
and morphology of a
material at nano level
Significance: SEM was used to using SEM image

 Identify the structure and morphology of

Nanowires for gas sensing  To know the average
particle size of nano
 Inspection of semiconducting materials used particle
in solar cells etc.

 Assembly of microchips for effective design

of low power chips used in IoT (Internet of
Things ) etc for fast accessing data
Expt.No:
 Resolving samples related to forensic, Date:
biological and geological aspects

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Concentrations of aqueous solutions of common acids and bases at 25 0C

Molecular Weights of Primary Standards

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Notes

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