Introduction to Laboratory Techniques and Safety

CONTENTS
FOREWORD
iii
PREFACE
UNIT-1 : Introduction
Dos and donts in a chemistry laboratory
Analytical methods
Basic laboratory equipment and procedures
Handling reagent bottles
10
Heating devices
11
UNIT-2 : Basic Laboratory Techniques
16
Cutting of glass tube and glass rod
16
Bending of a glass tube
18
Drawing out a jet
19
Boring a cork
20
Heating solution in a test tube
22
Heating solution in a beaker or a flask
22
Filtration
22
Measuring volume of liquids
25
Weighing technique
30
Experiment 2.1 : Preparation of standard solution of

oxalic acid
34
UNIT-3 : Purification and Criteria of Purity
Experiment 3.1 : Purification of sample of a compound

by crystallisation
38
Experiment 3.2 : Determination of melting point of an organic

compound
40
Experiment 3.3 : Determination of boiling point of an organic

compound
43
UNIT-4 : Chemical Equilibrium (Ionic Equilibrium in Solution)
38
Experiment 4.1 : Study of shift in equilibrium in the reaction

of ferric ions and thiocyanate ions
46
47
UNIT-5 :
Experiment 4.2 : Study of shift in equilibrium in the reaction
between [Co(H2O)6] 2+ and Cl ions
50
pH and pH Change in Aqueous Solutions
53
Experiment 5.1 : To determine the pH of some fruit

juices
Experiment 5.2 :
54
To observe the variation in pH of acid/

base with dilution
56
Experiment 5.3 : To study the variation in pH by common

ion effect in the case of weak acids and
weak bases
58
Experiment 5.4 : To study the change in pH during the

titration of a strong acid with a strong
base by using universal indicator
61
Experiment 5.5 : To study the pH of solutions of sodium

chloride, ferric chloride and sodium
carbonate
63
UNIT-6 :
Titrimetric Analysis
Detection of end point
65
65
Requirement for a reaction in the titrimetric analysis
66
Acidimetry and alkalimetry
66
Indicators in acid base titration
67
Experiment 6.1 : Determination of the concentration

(strength) of a given sodium hydroxide
solution by titrating it against a
standard solution of oxalic acid
69
Experiment 6.2 : Preparation of a standard solution of

sodium carbonate
74
Experiment 6.3 : Determination of the strength of a

given solution of dilute hydrochloric
acid by titrating it against a standard
solution of sodium carbonate
75
Systematic Qualitative Analysis
79
Experiment 7.1 : Detection of one cation and one anion

in the given salt
80
Systematic analysis of anions
81
Preliminary tests with dilute sulphuric acid
Confirmatory tests for anions of dilute sulphuric acid group
Preliminary tests with concentrated sulphuric acid
81
82
86
UNIT-7 :
Confirmatory tests for anions of concentrated sulphuric

acid group
87
Tests for sulphate and phosphate
92
Systematic analysis of cations
93
Preliminary examination of salt for identification of cation
93
Wet tests for identification of cations
99
Analysis of Group-zero cation
99
Analysis of Group-I cations
101
Analysis of Group-II cations
102
Analysis of Group-III cations
105
Analysis of Group-IV cations
106
Analysis of Group-V cations
109
Analysis of Group-VI cations
111
Specimen record of salt analysis
114
PROJECTS
116
APPENDICES
129
xi
UNIT-1
INTRODUCTION
ABORATORY work has special importance in the learning of science as scientific

principles develop and grow on the basis of laboratory work. Chemistry is
an experimental science; the concepts learned in the theory classes are
better understood through experimentation. Laboratory work provides an
opportunity to observe many of the chemical phenomena under controlled
laboratory conditions and workout a problem through the method of inquiry. In
other words, it provides you with ample opportunity to become a keen observer
and to draw inferences and explain results.
The training in laboratory work helps to develop skills for handling apparatus
and equipment and carry out experiments. In this way, the experimental work
helps to promote scientific temper and adopt a cooperative attitude. Working in
the laboratory provides a platform for trying novel and creative ideas and giving
them concrete shape.
Before you become familiar with the scientific procedures and experimental
skills and start working in the laboratory, you should be well acquainted with
the chemistry laboratory. You should notice the facilities provided in the
laboratory and on your working table.
You will notice that your table is provided with a water-tap, gas-tap, Bunsen
burner spirit lamp/kerosene lamp, a reagent shelf and a bin for disposing waste
material. You will find that some reagents are kept on the shelf fixed on the table
while some reagents are kept on the shelf fixed on sidewalls. Reagents kept on
the shelf of the table are frequently required while those on the shelf fixed on
walls are less commonly used. Besides the facilities on the table, you will see
that there are exhaust fans fitted on the upper portion of the wall opposite to the
doors and windows and are placed close to the level of the ceiling. This facilitates
the exhaution of harmful fumes and circulation of fresh air in the laboratory.
For this purpose, there are also enough number of windows in the laboratory.
Keep these open while working. A fume cupboard is provided in the laboratory
for performing those experiments in which fumes are produced.
It is strongly advised that you should become fully familiar with your
chemistry laboratory, laboratory practices and procedures, and more importantly
the precautions to be taken while working in the laboratory.
The environment in the chemistry laboratory is somewhat special in the sense
that it can be a place of joy, discovery and learning. It can also become a place of
frustration and danger. Frustration if you come unprepared and neglect
recording the important data properly, and danger if you do not follow the
precautions properly in conducting the experiments where potential danger exists.
LABORATORY MANUAL CHEMISTRY
In order to become proficient in basic principles underlying

the laboratory work, you must learn to handle the equipment and
familiarise yourself with the safety measures and good laboratory
practices.
You should organise yourself before entering into the laboratory
for work and be aware of the pre-laboratory preparation and
experimental procedures so that your work is not haphazard. You
should work individually unless the experiments require
teamwork. Use your ingenuity and common sense while working.
This attitude is the basic requirement to aquire scientific approach.
Prepare reports of the experiments in the laboratory notebook. Do
not use loose sheets or scraped papers for this purpose. Think
and try to get answers of important questions that give you an
understanding of the principles on which the experimental
procedure is based.
Scientists learn much by discussion. In the same manner,
you too may be benefitted by discussion with your teacher and
classmates. Use books in case of any doubt because books are
more reliable, complete and better source of information than
classmates. Else consult your teacher.
Safety rules are designed to ensure that the work done in the
laboratory is safe for you and your fellow students. Follow the
safety rules and be aware of where the items like first-aid box, fire
extinguisher etc., are kept.
Dont taste anything in the laboratory (Poisonous
substances are not always so labelled in the laboratory) and never
use laboratory as an eating-place. Never use glass apparatus of
the laboratory for eating and drinking purposes. Never work in
the laboratory alone. Seek the permission of your teacher for
working for extra hours, in case it is needed.
1.1 DOS AND DONTS IN A CHEMISTRY LABORATORY

The practices outlined below are designated to guide you in
developing efficient laboratory techniques and to make your
laboratory a pleasant place to work. You should follow the
practices listed below:
Wear safety glasses, lab coat and shoes while working in the
laboratory.
Check and read the label of the reagent bottle carefully before
using its content.
Read procedures and precautions carefully and follow them.
It is a bad practice to leave the reagent bottles on the working
table. Put the stoppers properly on the bottles and keep them
on the shelf immediately after use.
INTRODUCTION
If a reagent bottle on your seat is empty, ask the laboratory

attendant to fill it.
If you require a reagent from the bottle kept on side shelf,
take the test tube or the beaker to the shelf. Do not bring
the bottle to your seat.
Avoid using excessive amounts of reagents unless you
are advised to do so.
Never return unused chemicals to the stock bottles. If
you commit a mistake in putting the material back into the
correct bottle, experiments of other students will be spoiled.
Never mix the chemicals unless it is required in the
experiment. Failure in following this rule may result in
serious accidents.
Use only properly cleaned droppers, spatulas or
pipettes etc. to take out the reagents from the stock
solutions and reagent bottles.
Do not keep the stopper of the bottle on the table.
Impurities may stick to it and the content of the bottle may
be contaminated. Whenever you require a chemical from
the reagent bottle, pick up the bottle with one hand and
remove or replace the stopper with the other hand and keep
it on a clean glazed tile. To take out dry solid reagents use
spatula and keep it on watch glass, never use filter
papers. Do not keep the reagent on your palm or touch
it with your fingers.
Never throw used match sticks, litmus papers, broken glass
apparatus, filter papers or any other insoluble solid
material into the sink or on the floor. Dispose them off in
the waste bin provided at your seat. Only waste liquids
should be thrown in the sink while keeping the tap water
running so that nothing stinks and sticks and the waste
liquid is drained completely.
Do not waste water or gas. Close the taps whenever they
are not in use. Do not leave the lighted burner under the
wire gauze when nothing is being heated. Extinguish it.
Hot apparatus should not be placed on working table directly
because it may spoil the working table. Place it on a glazed
tile or a wire gauze.
Do not heat the apparatus which is made of thick glass, e.g.,
graduated cylinder, bottles, measuring flasks etc., as these
break on heating. Also heating distorts the glass and
calibrations on the measuring apparatus may become invalid.
Test tubes may break if they are heated above the level of the
liquid filled in them. Crucibles may be heated to red-hot.
INTERNATIONAL
HAZARD SYMBOLS
Note : Look for these symbols

on the labels of bottles
of chemicals.
Do not heat the test tube containing solution with its mouth
towards yourself or your neighbour as the spurting of
content may harm you or your neighbour (Fig 1.1). Do not
heat the test tube continuously in one position. Keep it moving
and shaking while heating so that heating is uniform.
Clean every piece of apparatus as soon as the work is finished
and keep these at proper place. A dirty seat and apparatus
indicate careless habit and it hinders successful performance
of the experiment.
Fig. 1.1 : Correct method of heating

solution in a test tube
The indication for cleanliness of glass apparatus is that

after rinsing with water and holding it in position, water flows
out readily and droplets do not stick to the surface. If water
droplets stick to the glass surface it means that apparatus is
greasy. In that case it should be washed with 5% NaOH
solution or with soap and then thoroughly rinsed with water.
If it still remains dirty or some stain remains sticking to it,
then warm concentrated nitric acid can be used for cleaning.
If some stain is still not cleaned then chromic acid, (also called
chromosulphuric acid) can be used for cleaning. To prepare
one litre of chromic acid solution, 100 g of potassium
dichromate is dissolved in one litre of conc. sulphuric acid.
It is highly corrosive liquid and all care should be taken
to avoid its contact with the skin and clothes.
Use fume cupboard for performing experiments in which
poisonous and irritating fumes are evolved.
Keep the doors and windows open and the exhaust fan
on while working in the laboratory, so that poisonous
vapours are quickly sucked out and flow of fresh air is
facilitated.
INTRODUCTION
If you will follow the Dos and Donts outlined above, your
experience of learning basic scientific techniques will surely
be full of joy.
In the following pages you will be introduced to basic

laboratory equipments, procedures and techniques required for
working in a chemistry laboratory. Let us begin with the
introduction to type of analytical methods used in chemistry.
1.2 ANALYTICAL METHODS

Elements and their compounds may be detected by their physical
features such as physical state, colour, odour, lustre, melting
point, boiling point, sublimation, colour imparted to the flame
on heating, hardness, crystalline state or amorphous state,
solubility in water and other solvents, etc., but sometimes it is
impossible to identify the substance on the basis of physical
properties only, therefore, chemical methods such as reaction
with alkalies, acids, oxidising agents, reducing agents and other
compounds are employed for the identification of substances. A
substance is analysed to establish its qualitative and quantitative
chemical composition. Therefore, analysis may be either
qualitative or quantitative. Qualitative analysis is used to detect
the elemental composition of the substance; it may involve
detection of ions formed, and the type of molecules present in
the substance. The methods of qualitative analysis are very
diverse. They not only allow us to determine the elements which
constitute the substances known on the Earth, but also the
composition of celestial bodies which are away from the Earth.
Quantitative analysis helps to establish the quantity of the
constituents of substances. It helps in measurement of energy
changes etc.
1.3 BASIC LABORATORY EQUIPMENT AND PROCEDURES

Heating, filtration, decantation, measuring volumes and
weighing solids and liquids are some of the basic laboratory
procedures, which are required frequently during the
experimentations in the chemistry laboratory. Some of the
specific equipment required for this purpose are shown in
Fig. 1.2 and 1.3. You will learn about the use of these while
performing experiments. Guidelines for using some of the
common apparatus are as follows :
Fig. 1.2 : Common laboratory equipments
INTRODUCTION
Fig. 1.3 : Common laboratory glass apparatus
Test Tubes
Test tubes of different volumes are available but usually for this
level of chemistry practical work, test tubes of 125 mm (length)
15 mm (diameter), 150 mm (length) 15 mm (diameter) and 150
mm (length) 25 mm (diameter) are used. Test tubes are available
with or without rim around the mouth. Test tubes of smaller width
are used for carrying out reactions, which do not require heating
or when heating is required for a short period. Only one third of
the test tube should be filled while carrying out a reaction.
The test tube of bigger diameter is called boiling tube. It is used
when large volume of solution is required to be heated. Test tube
holder is used to hold a test tube while heating a mixture or
solution in it. Test tube stand should be used to keep test tubes
containing solutions in the upright position (Fig.1.4).
Fig. 1.4 : Stand carrying boiling tubes and

test tubes of different sizes
Flasks
Mostly round bottom and conical flasks (also called Erlenmeyer
flask) are used in chemistry laboratory. These are available in
various capacities ranging from 5 mL-2000 mL. Choice of the
size and type depends upon the amount of solution to be
handled and the type of reaction to be carried out. Generally,
for heating or refluxing a reaction mixture contained in a round
bottom flask, direct flame / sand bath / water bath, is used.
Conical flasks are employed for carrying out certain reactions
at room temperature or lower temperatures. These are specially
used for carrying out volumetric titrations.
INTRODUCTION
Beakers
Beakers of various capacities ranging from 5 mL to 2000 mL are
available and are employed for the purpose of preparing
solutions, for carrying out precipitation reactions and for
evaporation of solvents etc.
Separating Funnels
These are used for separating immiscible liquids. Separating
funnels of various sizes and shapes are available (Fig. 1.5).
Condensers
Condensers are used to condense the vapour back to the liquid
phase. Generally two types of condensers are used in the
laboratory, (a) air condensers and (b) water condensers. Air
condenser is shown in Fig.1.6 (a). Length and diameter of the glass
tube of air condensers vary. There is a rapid transfer of heat from
the hot vapour to the surrounding air and vapour condenses.
Water condenser has an inner tube surrounded by an outer
jacket [Fig.1.6 (b)] with an inlet and an outlet for circulating water.
Inlet is connected to the tap. Heat is transferred from hot vapour
to the surrounding water.
For refluxing and distillation of solutions or liquids with high
boiling point, air condensers are used. For low boiling liquids water
condensers are used.
(a)
Fig. 1.5 : Separating funnels

of various shapes
(b)
Fig. 1.6 : (a) Air condenser
(b) Water condensers
Ground Glass Joints

Now-a-days ground glass joints are fixed to inlets or outlets of the
apparatus described above to minimize the use of corks. Apparatus
with ground glass joints of various sizes are available.
Fig. 1.7 : Apparatus with ground glass joints
1.4 HANDLING REAGENT BOTTLES
Fig. 1.8 : Method for taking out

solid from the reagent
bottle
10
Correct methods for taking out solid and liquid reagents

from reagent bottles are shown in Fig. 1.8 and 1.9
respectively. Before taking out any reagent from the bottle
one should double-check the name written on label to make
sure that correct reagent is being taken out. Liquid reagents
are stored either in reagent bottle of small mouth with glass
stoppers or dropping bottles. While using reagent bottles
with stopper, put the stopper on a clean glazed tile. Never
put the stopper on the table because dirt from the table may
stick to it and contaminate the reagent. Replace the stopper
immediately after taking out the reagent. The proper way of
pouring liquid from the bottle is shown in Fig. 1.9. When
adding liquids directly from bottles into the beaker, a glass
rod is held against the mouth of the bottle so as to permit
the flow of liquid along the rod without splashing.
INTRODUCTION
Fig. 1.9 : Methods of pouring liquids
If dropper is used for transferring the

liquid, it should not touch the content of the
container while transferring the reagent.
Correct way of transferring liquid with a
dropper is shown in Fig. 1.10. Droppers of
bottles should never be exchanged. Now-adays, use of dropping bottles is considered
more convenient and safe.
1.5 HEATING DEVICES

Heating during the laboratory work can be
done with the help of a gas burner, spirit lamp
or a kerosene lamp. The gas burner used in
the laboratory is usually Bunsen burner
(Fig. 1.11). Various parts of Bunsen burner
are shown in Fig. 1.12. The description of
these parts is as follows :
Fig. 1.10 : Transferring liquid through dropper
11
BUNSEN BURNER
(A) Parts of Bunsen Burner
1. The Base
Heavy metallic base is connected to a side tube called gas tube.
Gas from the source enters the burner through the gas tube and
passes through a small hole called Nipple or Nozzle and enters
into the burner tube under increased pressure and can be burnt
at the upper end of the burner tube.
2. The Burner Tube

It is a long metallic tube having two holes diametrically opposite to
each other near the lower end which form the air vent. The tube can
be screwed at the base. The gas coming from the nozzle mixes with
the air coming through the air vent and burns at its upper end.
3. The Air Regulator

It is a short metallic cylindrical sleeve with two holes diametrically
opposite to each other. When it is fitted to the burner tube, it
surrounds the air vent of the burner tube. To control the flow of
air through the air vent, size of its hole is adjusted by rotating the
sleeve.
Fig. 1.11 : Bunsen burner
Fig. 1.12 : Parts of Bunsen burner
If the air vent is closed and the gas is ignited, the flame will be
large and luminous (smoky and yellow in colour). The light emitted
by the flame is due to the radiations given off by the hot carbon
particles of partially burnt fuel. The temperature of the flame in
this situation is low. If adjustment of sleeve on vent is such that
gas mixed with air is fed into the flame, the flame becomes less
12
INTRODUCTION
luminous and finally turns blue. When the flow of air is correctly
adjusted, the temperature of the flame becomes quite high. This
is called non-luminous flame. Various zones of flame are shown
below in Fig. 1.13.
Three distinctly visible parts of the Bunsen flame are described
below:
Fig. 1.13 : Zones of flame of Bunsen burner
(B) Principal Parts of Bunsen Flame

1. The Inner Dark Cone, A E C
This is innermost dark cone, which is just above the burner tube.
It consists of unburnt gases. This zone is the coldest zone of the
flame and no combustion takes place here.
2. The Middle Blue Cone, A D C E A

This is middle part of the flame. This becomes luminous when the
air vent is slightly closed. Luminosity of this part is due to the
presence of unburnt carbon particles produced by decomposition
of some gas. These particles get heated up to incandescence and
glow but do not burn. Since the combustion is not complete in
this part, the temperature is not very high.
3. The Outer Non-luminous Mantle, A B C D A

This is purplish outer cone. It is the hottest part of the flame. It is
in direct contact with the atmosphere and combustion is quite
complete in this zone.
13
Bunsen identified six different regions in these three

principal parts of the flame:
(i) The upper oxidising zone (f)

Its location is in the non-luminous tip of the flame which is in
the air. In comparison to inner portions of the flame large excess
of oxygen is present here. The temperature is not as high as in
region (c) described below. It may be used for all oxidation
processes in which highest temperature of the flame is not required.
(ii) Upper reducing zone (e)

This zone is at the tip of the inner blue cone and is rich in
incandescent carbon. It is especially useful for reducing oxide
incrustations to the metals.
(iii) Hottest portion of flame (d)

It is the fusion zone. It lies at about one-third of the height of the
flame and is approximately equidistant from inside and outside
of the mantle i.e. the outermost cone of the flame. Fusibility of the
substance can be tested in this region. It can also be employed for
testing relative volatility of substances or a mixture of substances.
(iv) Lower oxidising zone (c)

It is located on the outer border of the mantle near the lower part
of the flame and may be used for the oxidation of substances
dissolved in beads of borax or sodium carbonate etc.
(v) Lower reducing zone (b)

It is situated in the inner edge of the outer mantle near to the blue
cone and here reducing gases mix with the oxygen of the air. It is
a less powerful reducing zone than (e) and may be employed for
the reduction of fused borax and similar beads.
(vi) Lowest temperature zone (a)

Zone (a) of the flame has lowest temperature. It is used for testing
volatile substances to determine whether they impart colour to
the flame.
(C) Striking Back of the Bunsen Burner

Striking back is the phenomenon in which flame travels down the
burner tube and begins to burn at the nozzle near the base. This
happens when vents are fully open.The flow of much air and less
gas makes the flame become irregular and it strikes back.
14
INTRODUCTION
The tube becomes very hot and it may produce burns on touching.
This may melt attached rubber tube also. If it happens, put off the
burner and cool it under the tap and light it again by keeping the
air vent partially opened.
SPIRIT LAMP
If Bunsen burner is not available in the laboratory then spirit
lamp can be used for heating. It is a devise in which one end of a
wick of cotton thread is dipped in a spirit container and the other
end of the wick protrudes out of the nozzle at upper end of the
container (Fig. 1.14). Spirit rises upto the upper end of the wick
due to the capillary action and can be burnt. The flame is non
luminous hence can be used for all heating purposes in the
laboratory. To put off the lamp, burning wick is covered with the
cover. Never try to put off the lighted burner by blowing at
the flame.
Fig. 1.14 : The spirit lamp
KEROSENE HEATING LAMP

A kerosene lamp has been developed by National Council of
Educational Research and Training (NCERT), which is a versatile
and cheaper substitute of spirit lamp. It may be used in laboratories
as a source of heat whereever spirit and gas burner are not
available. Parts of kerosene lamp are shown in Fig. 1.15.
Working of the Kerosene Lamp

More than half of the container is filled with kerosene. Outer sleeve
is removed for lighting the wicks. As the outer sleeve is placed
back in position, the flames of four wicks combine to form a big
soot-free blue flame.
The lighted heating lamp can be put off only by covering the
top of the outer sleeve with a metal or asbestos sheet.
Fig. 1.15 : Parts of Kerosene Heating Lamp
15
UNIT-2
BASIC LABORATORY
TECHNIQUES
HE laboratory apparatus for carrying out reactions, in general, is made up

of glass. It is because glass is resistant to the action of most of the
chemicals. Generally, two types of glass are used for making apparatus
for laboratory work. These are soda-lime glass and borosilicate glass.
Soda-lime glass, which is made by heating soda, limestone and silica, softens
readily at about 300-400C in the burner flame. Therefore, on heating glass
tubings made of soda-lime glass easily softens and can be bent. Coefficient of
expansion of soda glass is very high, therefore on sudden heating and cooling, it
may break. To avoid breaking, it should be heated and cooled gradually. Annealing
by mild reheating and uniform cooling prevents breakage. Such glass should
not be kept on cold surface while it is hot, since sudden cooling may break it.
Borosilicate glass does not soften below 700-800C and requires oxygennatural gas flame for working. Natural gas mixed with oxygen is burnt to get the
oxygen-natural gas flame. Coefficient of expansion of this glass is low and
apparatus made of this glass can withstand sudden changes in temperature.
Therefore, apparatus used for heating purposes is made from borosilicate glass.
On heating, glass apparatus made up of borosilicate glass does not distort.
In the following pages you will learn about some of the techniques of handling
glass tubes and glass rods without injuring yourself. Also, you will learn the
techniques of using laboratory apparatus and equipments.
2.1 CUTTING
OF
GLASS TUBE
AND
GLASS ROD
Material Required
Soda-glass tube
Soda-glass rod
Triangular file
: 15 cm long
: 15 cm long
: One
Procedure
(i)
Place the glass tube or the glass rod on the table and press it with your left
hand.
BASIC LABORATORY TECHNIQUES
(ii)
(iii)
(iv)
(v)
(vi)
Keep the lower end of a triangular file with its sharp edge
perpendicular to the tube to be marked and pull it towards
you to make a single deep scratch on the glass tube or the
glass rod at a desired length (Fig. 2.1 a).
Keep thumbs of your hands on both sides, very close and
opposite to the scratch as shown in Fig. 2.1 b and break the
glass tube or rod by applying pressure from your thumbs
in a direction away from you (Fig. 2.1 c). Break the tube/
rod by holding it with a cloth so that hands are not harmed.
If the glass tube does not break, make a deeper scratch at
the point marked earlier and make a fresh attempt.
Trim any jagged edge by striking with a wire gauge (Fig. 2.2 a).
Heat the freshly cut edge of the tube gently in the flame to
make the edges round and smooth (Fig. 2.2 b). This is called
fire polishing. For fire polishing, first continuously warm the
cut end in the Bunsen flame and then rotate it back and
forth until the edge is rounded. Too much heating may distort
the rounded edge (Fig. 2.2 c).
(a)
(b)
(c)
Fig. 2.1 : (a) Marking a glass rod or a glass tube

(b) Placing the thumbs together opposite to the scratch
(c) Breaking the glass rod or glass tube
After continuously warming

the cut end in a Bunsen
flame, rotate back and forth
until the edges are rounded
(a)
The cut
end
(b)
Properly
Overheated
rounded edge
end
after fire
polishing
(c)
Fig. 2.2 : (a) Trimming the jagged edges

(b) Rounding the edges
(c) Properly and improperly rounded edges
17
Precautions
(a)
(b)
Make a single deep scratch at the desired length with one stroke of the file.
To avoid injury, carry out the filing and breaking of the glass tube/rod away
from the face as far as possible and hold the glass tube / rod with the help of a
piece of cloth to avoid injury to hands.
Discussion Questions
(i)
Why does glass not possess a sharp melting point?
(ii)
Why is it required to round off the freshly cut edges of the glass tube or the
glass rod?
2.2 BENDING
OF A
GLASS TUBE
Material Required
Glass tube
Triangular file
:
:
20-25 cm long
One
Procedure
(i)
(ii)
(iii)
(a)
Cut a tube of desired length with the help of a triangular file

as described in section 2.1.
Place the tube in the hottest zone of Bunsen burner flame
and heat that portion from where it is to be bent (Fig. 2.3 a).
While heating the tube in the flame keep it rotating slowly until
the portion, which is to be bent, becomes red hot and soft and
starts bending under its own weight. (Fig. 2.3 b).
(b)
Fig. 2.3 : (a) Heating the tube

(b) The tube softens and starts bending under its own weight
(c) Making the bend coplanar
18
(c)
(iv)
(v)
(vi)
Remove the tube from the flame and bend it slowly at a

desired angle by pressing it against a glazed tile to ensure
the coplanarity of the bend (Fig. 2.3 c). Slow process of
bending prevents flattening of glass tube (Fig. 2.4).
Cool it by placing on a glazed tile (Fig. 2.3 c).
Bend the tubes at different angles as shown in Fig. 2.5.
Fig. 2.4 : A glance of proper

and improper bends
Fig. 2.5 : Bend drawn at

various angles
Precautions
(a)
(b)
(c)
Avoid heating the glass tube only on one side, rather rotate it while heating.
Select a glass tube of appropriate length (nearly 30 cm long) to keep your hands
safe from heat.
To avoid flattening of the glass tube while bending, carry out the process slowly.
(i)
Why should the tube be rotated while heating?
(ii)
Why is the red-hot tube bent slowly?
2.3 DRAWING
OUT A
JET
Material Required
Glass tube
Triangular file
Sand paper
:
:
:
20-25 cm long
One
As per need
19
Procedure
(i)
(ii)
(iii)
(iv)
(v)
(vi)
Select a glass tube of appropriate diameter for drawing a jet.

Cut the glass tube of desired length with the help of a
triangular file.
Heat the tube in the hottest portion of the Bunsen burner
flame by holding it at both the ends.
Rotate the tube slowly until the portion, which is kept in the
flame, becomes red hot and soft.
Remove the tube from the flame and pull the ends apart
slowly and smoothly until it becomes narrow in the middle
and then stretches into a fine jet as shown in Fig. 2.6 b.
Cut the tube in the middle (Fig 2.6 c) and make the jet
uniform and smooth by rubbing it with sand paper and by
fire polishing.
(b)
(a)
(c)
Fig. 2.6 : (a) Heating the tube to draw a jet (b) Before cutting (c) After cutting
Precaution
While drawing a jet, pull apart the two ends of the red-hot tube slowly so that it
becomes thin uniformly.
(i)
What type of glass is preferred for drawing out a jet?
(ii)
Why is the glass tube of small diameter chosen for drawing out a jet?
2.4 BORING A CORK

Material Required
Rubber corks
Cork borer set
20
:
:
As per need
One
Glycerine solution
(Shelf reagent)
As per need
Procedure
(i)
(ii)
(iii)
(iv)
(v)
(v)
Mark the rubber cork on both its sides at the place where a
hole is to be drilled (Fig. 2.7 a).
Choose a borer of diameter slightly smaller in size than
that diameter of the tube to be inserted in the hole (Fig. 2.7 b).
Place the rubber cork on the table with its smaller end in the
upward direction as shown in Fig. 2.7 c.
Hold the cork in position with the left hand and put a suitable
borer, lubricated by dipping in water or glycerine, at the
place where the hole is to be drilled (Fig. 2.7 c). By lubricating
the borer with water or glycerine a smooth hole is drilled.
Now hold and push the borer vertically in the downward
direction, and drill the hole by rotating the borer and
simultaneously apply the pressure gently.
For making two holes in the same cork, keep appropriate
distance between the holes and use borers of proper size.
(a)
(b)
(c)
Fig. 2.7 : (a) Marked cork (b) Choosing the borer (c) Boring process
Precautions
(a)
(b)
Make a mark on both sides of the cork and select borer of proper size.
To obtain a smooth hole, drill half the hole from one side and another half from
the other side of the cork.
(i)
What is the role of glycerine in the process of boring?
(ii)
Why should the diameter of the borer be less than the diameter of the tube to be inserted
in the hole?
21
2.5 HEATING SOLUTION IN A TEST TUBE

If a solution contained in a test tube is to be heated on a burner,
hold the test tube with the help of a test tube holder at an angle
and heat just below the surface of the liquid but not at the bottom
(Fig. 2.8).
While heating, shake the test tube occasionally. If the test tube
is heated at the bottom, a bubble may form causing the entire
content to spill out of the test tube violently. This is called bumping.
Fig. 2.8 : Heating solution in This can cause a serious accident, if the mouth of the test tube is
a test tube
pointing towards you or someone working near you. Therefore,
when you heat a test tube over a burner, take care that its mouth
does not point towards anyone. If content of the test tube is to be
heated up to the boiling point, only one third of the test tube should
be filled.
2.6 HEATING SOLUTION
IN A
BEAKER
OR A
FLASK
If liquid is to be heated in a beaker or a flask, the beaker or the

flask is placed on a wire gauze which in turn is placed on a tripod
stand (Fig. 2.9).
For safe boiling, it is advisable to add a chip of broken china
dish or carborundum/marble / a piece of capillary sealed at one
end or any other non-reacting tiny material like pumice stone to
avoid bumping.
Note : (i)
Fig. 2.9 : Heating solution in

a beaker
(ii)
Never heat the apparatus with thick walls because it may

break. Borosilicate glass apparatus is usually used for
heating substances.
The apparatus, which is used for measuring volume, should
also not be heated because heating may distort it and
graduations may become invalid.
2.7 FILTRATION
Filtration involves separation of a solid from a liquid by passing
the liquid through a porous material. In filtration, the porous
filtering material can be a piece of cloth, paper, sintered glass,
asbestos and so on. Filters of various pore sizes are available. If a
filter paper has large pores, the liquid will pass through it more
easily, and the filtration will be fast. However, solid particles of
small size may also pass through the filter. Therefore, choice of the
method of filtration and the filtering material depends on particle
size of material to be retained on the filter paper.
22
Material Required
Funnel
Beaker
Funnel stand
Glass rod
Filter paper
:
:
:
:
:
One
Two
One
One
As per need
Procedure
(i)
(ii)
Fold the filter paper to fit in the funnel as shown in Fig. 2.10.
For this, fold the circular filter paper in half, tear off a small
piece of paper from the corner and once again fold it.
Open the folded filter paper into a cone by keeping three
folds on one side and one on the other such that the torn off
corner is outside. Fit the cone into the funnel. Take care that
filter paper cone fits in one cm below the rim of the funnel.
Fig. 2.10 : Folding the filter paper and placing it in the funnel
(iii)
Wet the paper with the solvent, which is usually

water, and adjust it so that the entire cone tightly
fits on the inner surface of the glass funnel and
there is no air gap in between the paper cone
and the glass.
(iv)
Add more water so that the stem of the funnel is

filled with water. If the filter paper is fitted
correctly, the filter paper will support a column
of water in the funnel stem. The weight of this
column of water produces a mild suction that
expedites filtration (Fig. 2.11).
Fig. 2.11 : Process of filtration
23
Precautions
(a)
(b)
The stem of the funnel should touch the side of the beaker in which filtrate is
collected so that falling drops do not cause splashing.
Filter paper cone should not be filled more than two-thirds. If level of the liquid
being filtered rises above the cone, then some unfiltered solution may pass into
the beaker kept below the funnel to collect the filtrate.
Note : (i) For quick filtration, a fluted filter paper may be used with advantage. The ordinary paper is folded into
6 or 16 folds instead of 4 and the folds are then turned alternately inwards and outwards. On opening
the paper we get a cone of fluted filter paper with series of ridges meeting at the apex. Filtration is
rapid due to the large surface available for filtration (Fig. 2.12).
Fig. 2.12 : Folding the filter paper to get a fluted filter paper cone
(ii) For separating the solid from the liquid, filtration should be done in two stages. First, almost whole
of the liquid should be poured out carefully down a stirring rod (Fig. 2.11). When only a few millilitres
of the mixture remain in the beaker, it should be poured into the funnel after swirling the beaker
gently. The sides of the beaker are then rinsed with a stream of water and the content is again
poured into the funnel. Rinsing is repeated till the beaker and the stirring rod is clean. It is better to
pour down a solid liquid mixture along a glass rod (Fig. 2.11). However, care should be taken that
paper is not punched by the stirring rod.
Suction Filtration : Filtration in the above

manner is a slow process. It can be speeded up
by carrying out filtration under reduced
pressure using suction, which can be applied
by means of water aspirator (Fig. 2.13) or
vacuum pump. Water aspirator can be fitted on
to the tap through a rubber tubing. It uses fast
stream of water to suck in air through the side
arm. Suction is quite strong, therefore a special
funnel called buchner funnel is used for filtration.
It is fixed on to the mouth of the filtration flask
through a rubber cork (Fig. 2.13).
Fig. 2.13 : Suction filtration
24
IMPROVISATION
If you do not have a Buchner funnel or if you have very small amount of substance to be
filtered, try following improvised apparatus for suction filtration. Take a glass rod and check
that it passes through the stem of the funnel freely. Flatten one end of the glass rod by
heating it in a bunsen burner flame and then pressing it against the glazed tile. The flat
portion of the rod will now fit into the upper part of the stem of the funnel.
Cut the length of the rod to a small size so that it forms a button with a small stem. Fit the
button in the funnel as shown in the figure below.
Cut a small circular piece of filter paper of the size such that it covers the flat button and
just touched the sides of the funnel. Moisten the filter paper and use this improvised funnel
in place of a Buchner funnel. Try using shirt button in place of this button.
2.8 MEASURING VOLUME OF LIQUIDS

Usually volumetric flasks, graduated cylinders, pipettes and
burettes are used for measuring volume of liquids. Volumetric
flasks and cylinders are graduated to measure volume of a liquid
at a certain temperature. Pipettes and burettes are calibrated to
deliver certain specific volume of a liquid at a specified temperature.
The capacity mark is usually etched on the glass of the equipment.
Aqueous solutions wet the glass surface, therefore these form
concave meniscus when filled in these equipments. Central part
of the meniscus is rather flat (Fig. 2.14 a). Calibration of the
(a)
(b)
Fig. 2.14 : (a) Water forming curved surface in the glass apparatus
(b) Noting the reading
25
apparatus coinciding with this flat portion of the meniscus gives a

measure of the volume of the liquid. Therefore, while making final
adjustment of volume or noting the reading, the curved surface of
the liquid should appear touching the etched mark when viewed
by keeping the eye level aligned to the etched mark (Fig. 2.14 b).
This helps in avoiding the parallax errors (error caused by the
change in position of the observer). Note that if the liquid forms
convex meniscus or is coloured and opaque e.g. KMnO4 solution
then reading coinciding with upward surface is noted. In flasks
and pipettes capacity mark is etched on the narrow part of the
equipment to minimize the error in noting the level of meniscus.
Graduated cylinders are not used for very precise measurements,
so they need not be narrow. Burettes and pipettes are used to
measure the volume of a liquid accurately.
(a) Using Graduated Cylinder

Always a clean graduated cylinder (Fig. 2.15) should be used for
measurement because dirt may chemically contaminate the
substance being measured and it may deter accurate
determination of volume. Dirty glassware does not drain properly
Fig. 2.15 : Measuring Cylinder and the volume delivered may not be equal to that indicated by
calibration mark. Measuring cylinders of 5mL, 10mL, 25mL,
100mL, 250mL, 500mL, 1000mL and 2000mL capacity are
available. Measuring cylinders used for delivering the volume
actually contain slightly more than the volume read. This
compensates for the film of liquid left on the walls when liquid is
poured out.
(b) Using Burette
Fig. 2.16 : Burette
26
A burette is simply a long graduated tube of uniform bore with a

stopcock or a pinchcock at one end (Fig. 2.16). It is used for
measuring volume in a quantitative (titrimetric) estimation. The
burette reading is noted before and after delivering the liquid. The
difference between these two readings is the volume of the liquid
delivered. The liquid should be delivered dropwise. If the liquid is
allowed to run too fast, the walls of the burette will not drain
properly and some liquid may remain sticking to the surface of
the walls. This may lead to faulty reading. Measuring capacity of
the burette usually used in the laboratory is 50 mL.
Before filling the solution to be used, the burette should
be rinsed with the solution to be filled. For rinsing the burette,
few millilitres of solution are taken into it and the whole inner
surface of burette is wetted with the solution by rotating it.
After rinsing, the solution is drained out of the nozzle of the
burette (Fig. 2.17).
Fig. 2.17 : Rinsing the burette
After rinsing, the solution is filled in the burette with the help
of a funnel above zero mark. Stopcock is then opened wide and
the solution is allowed to run through the nozzle till there are no
air bubbles in it (Fig. 2.18).
Fig. 2.18 : Filling the burette
27
In order to read the level of a liquid in the burette,

hold a half blackened white card called anti parallax
card behind the burette at the level of the meniscus, so
that the black area appears to be just touching the
meniscus of the liquid (Fig. 2.19 a, b). The eye must be
levelled with the meniscus of the liquid to eliminate
parallax errors. Read the graduation on the burette
touching the black part of the card (Fig. 2.19 b). Always
remember that for all transparent solutions in the
burette, reading coinciding with the lower meniscus is
noted and for all dark coloured solutions (e.g. potassium
permanganate solution) reading coinciding with the
upper meniscus is noted. Never forget to remove the
funnel from the burette before noting the reading of the
burette and ensure that the nozzle is completely filled.
While noting the reading take care that no drop is
hanging at the nozzle of the burette.
(c) Using Pipette

(a)
(b)
Fig. 2.19 : (a) Mounting anti parallax

card on burette
(b) Using anti parallax card
for noting correct
reading
28
Normally pipettes of measuring capacity 1 mL, 2 mL,

5 mL, 10 mL, 20 mL, 25 mL etc. are used. Graduated
pipettes are also used in the laboratory work (Fig. 1.3).
Pipette (Fig. 2.20 a) is used for measuring volumes
of liquids, when these are to be transferred to a flask or
some other apparatus. Liquids are sucked into the
pipette by applying suction through mouth or by using
a pipette filler bulb or a pipette filler pump. It is always
safe to use pipette filler bulb or pipette filler pump to fill
the pipette. When poisonous and corrosive solutions are
to be drawn into the pipette, never suck by mouth.
Use a pipette filler bulb to draw the liquid up into
the pipette. Hold the pipette in one hand tightly, dip
the jet of the pipette into the solution to be pipetted out,
and squeeze the pipette bulb with the other hand
(Fig. 2.20 b). Now loosen your grip on the bulb so that
the liquid is sucked into the pipette. When the liquid is
above the etched mark on the pipette, remove the bulb,
and put the index finger of the hand at its place holding
the pipette as shown in Fig. 2.20 c. Loosen the finger
carefully to allow the excess liquid to flow out so that
the curvature of the meniscus reaches the mark. Now
carefully remove the finger and let the liquid run into
the flask (Fig. 2.20 d). After emptying the pipette do not
blow out the remaining liquid. Pipettes are so designed
that the little amount of liquid, which remains
untransferred, is not taken into calibration (Fig. 2.20 e).
Fig. 2.20 : (a) Pipette

(b) Using pipette filler bulb
(c) Holding the pipette after
removing the bulb
(d) Transfering liquid to the
flask
(e) Nozzle of the pipette after
measuring solution
(a)
(b)
(c)
To take out the maximum volume

after complete transfer, simply touch
the pipette to the side or base of the
container into which the liquid is being
transferred (Fig. 2.20 d).
The pipette should always be
rinsed with the solution which is to be
measured by it. For this fill the pipette
with few millilitres of solution and wet
the inner surface of the pipette with
the solution by rotating it (Fig. 2.21).
After rinsing, drain out the whole
amount of solution taken in it through
the nozzle. Now it is ready for
measuring the solution. Note that while
handling the pipette, hands should be
dry so that pressure is regulated easily.
Also, nozzle of the pipette being used
should not be broken.
(d)
(e)
Fig. 2.21 : Rinsing the pipette
29
(d) Using Measuring Flask
Fig. 2.22 : The measuring

flask
These are employed for making specific volumes of solutions. This

is also called graduated flask or volumetric flask. It is a pear shaped
vessel with a long narrow neck and flat bottom (Fig. 2.22). A thin
circle etched around the neck indicates the volume of the liquid
that it holds at a definite temperature.
The temperature and the capacity of the flask at that
temperature are marked on the flask. The mark around the neck
helps in avoiding errors due to parallax when making the final
adjustment of meniscus. The lower edge of the meniscus of the
liquid should be tangential to the graduated mark. While making
final adjustment of the meniscus, the front and the back portion
of the circular mark should be observable in single line. The neck
of the flask is made narrow to reduce error in adjustment of the
meniscus. In narrow space small change in volume makes large
effect on the height of the meniscus.
Measuring flasks of various capacities are available. Usually
at this level of experimentation flasks of capacity 50 mL, 100 mL
and 250 mL are employed in the work. The method of preparation
of solution by using measuring flask has been described in the
Experiment 2.1 later in this unit.
2.9 WEIGHING TECHNIQUE

(a) Acquaintance with Analytical Balance (Chemical
Balance)
The construction and
principle of working of a
chemical balance are same as
that of a physical balance.
However, due to its higher
sensitivity, its accuracy is
more. With the help of a
chemical balance, one can
weigh accurately up to 4
places of decimal. Analytical
balance can be used to weigh
the mass of a substance upto
0.0002 g accuracy. It is
called the least count of the
balance. A full view of a twopan analytical chemical
balance is shown in Fig. 2.23.
Fig. 2.23 : Analytical balance
30
In this type of balance, the beam is made up of a hard but

light weight material. The beam pivots at its centre on a knifeedge, which rests upon a plate made of very hard material such as
agate or corundum. The plate is attached to the central beam
support (central pillar). The two terminal agate knife-edges are
fixed at equal distance from the central edge and each of these
supports a suspension called stirrup from which the pans are
hung. A sharp pointer is attached to the centre of the beam
(Fig. 2.24 a). The pointer moves over a scale fixed at the bottom of
the pillar and serves to point out the deflection of the beam from
central position when the balance is in operation (Fig. 2.24 b). There
are two adjusting screws on both sides of the beam, which are meant
for adjusting the beam in the horizontal position. There are three
leveling screws at the base of the balance to make it horizontal. A
plumb line hangs near the central pillar, which helps in keeping the
balance horizontal. In order to operate the balance there is a knob
at the centre of the base.
(a)
(b)
Fig. 2.24 : (a) Pointer attached to the beam

(b) Movement of pointer
(b) Weight Box Including Fractional Weights and Riders

The weight box of a chemical balance generally contains the
following weights.
(a) Weights for weighing in grams :100, 50, 20, 20, 10, 5, 2, 2, 1
(b) Weights for weighing in milligrams : 500, 200, 200, 100, 50,
20, 20, 10
(c) Rider : To weigh 0.2 mg to 10 mg.
The three categories of weights for weighing in a chemical balance
are shown in Fig. 2.25. Materials used for making the weights
are as follows :
31
Gram Weights : Made of copper and nickel with or without coating

of chromium.
Milligram Weights : Made of Aluminium/German silver/Stainless
steel.
Rider : A loop made of aluminum or platinum wire weighing
10.0 mg.
(a)
(b)
(c)
(d)
Fig. 2.25 : (a) Weight box (b) Fractional weights (c) Rider and
(d) Forceps
(c) Setting of a Chemical Balance and Weighing

Material Required
Chemical balance
One
Weight box
One
Set of fractional weights including rider
One
Weighing bottle/watch glass
One
Procedure
Following steps are followed while using a chemical balance:
(i) Level the balance with the help of leveling screws and plumb
line.
(ii) Ensure that the beam is horizontal. Adjust the pointer at
zero point with the help of screws provided on both sides of
the beam. If it is adjusted on releasing the beam arrest, the
pointer moves equal divisions on both the sides of the zero
of the base scale.
32
(iii)
(iv)
(v)
Place a watch glass/weighing bottle on the left pan in which

weighing material is kept. Put approximate weights from
the weight box with the help of forceps on the right pan.
Release the beam arrest slowly and note the movement of
the pointer on the scale. If its weight is not appropriate, the
pointer will move towards the lighter side. Add or remove
weights according to the requirement after bringing the pans
to rest by arresting the beam with the help of the knob located
near the base. When weight on both the pans becomes equal,
the pointer moves equal divisions on both sides of the zero
of the base scale.
Use the rider for adjustment of weight below 10mg.
Using Rider
Maximum weight that can be weighed with the help of rider is
10 mg and the weight of the rider itself is 10 mg (i.e. 0.01g). It can
be easily placed in the grooves of the balance beam (Fig. 2.26).
When placed at the terminal position of the beam, which is marked
10, it will weigh 10 mg (i.e 0.01g). Principle of moment is applied
for weighing by using the rider. Weight is equal to the arm length
from the centre of the beam multiplied by the weight of the rider.
Length of the beam from the centre to one side of the beam is
taken as unit length.
On both sides from the centre, the balance beam is divided
into ten equal parts through equidistant marks, each of which
corresponds to 1/10 of the length of the beam. Hence, each big
1
0.01g = 0.001 g or 1 mg weight. Each
division corresponds to
10
big division is further divided into five parts. Thus, each small
division corresponds to only 1/5 milligram i.e. 0.2 mg or 0.0002 g.
Thus, the rider placed at the 4.2 mark will weigh 0.0044 g
(i.e. 4 0.001 + 2 0.0002 = 0.0044 g) (Fig. 2.26).
Fig. 2.26 : Rider resting

on grove of
balance beam
Precautions
(a)
(b)
(c)
(d)
(e)
(f)
(g)
Pans must be properly cleaned before and after weighing. Chemicals should never
be placed directly on the pans for weighing.
Always release the beam gently.
Avoid overloading the balance.
Always transfer the weights from one place to another with the help of forceps.
Do not allow the weights to get spoiled by corrosion.
Never weigh a hot/cold object on the balance.
Always keep weights on the right pan and object on the left pan of the balance
(if you are a right handed person).
33
(h)
(i)
(j)
Always make necessary adjustments in the balance before weighing.

To insert or remove weights and to keep the object on the pans always use the
side doors. Never use the front shutter.
Keep the doors shut while relasing the beam arrest to note the movement of the
pointer on the scale.
(i) How is an analytical balance different from a physical balance?
(ii) On what principle, is weighing by using rider based?
(iii) What is the maximum weight that can be weighed on a chemical balance?
(iv) Which weights are called fractional weights?
(v) Why are forceps always used for handling the weights?
(vi) The rider rests at a reading of 3.4 on the left side of the beam. What contribution does this
make to the weight of the material being weighed when weights are placed on the right
pan?
(vii) Can you weigh 0.0023 g using chemical balance? Give reason for your answer.
EXPERIMENT 2.1
Aim
Oxalic acid
Preparation of 250 mL of 0.1M standard solution* of oxalic acid.
Theory
A solution of exactly known concentration is considered to be a
standard solution. There are various ways of expressing the
concentration of a standard solution. Standard solution of an acid/
base is used to determine the unknown concentration of a solution
of bases / acids by volumetric analysis. For example, a standard
solution of oxalic acid can be used to determine the unknown
concentration of an alkali solution. The strength of a standard
solution is usually expressed in moles per litre. The formula of
hydrated crystalline oxalic acid is
* Learn more about standard solution in Unit-6.
34
and its molar mass is 126 g. If 126 g of oxalic acid is present in one
litre of the solution, it is known as one molar (1.0 M) solution.
For the preparation of one litre of 0.1 M oxalic acid solution, we
126
=12.6g of hydrated oxalic acid. Therefore, for preparing
require
10
250 mL of 0.1 M oxalic acid solution, we require:
12.6 g 250 mL
= 3.1500 g of hydrated oxalic acid.
1000 mL
In general for preparing a solution of required molarity, the amount
of substance to be weighed can be calculated by using the formula
given below :
Molarity (M) =
Mass of solute is grams 1000

Molar mass of solute
(volume of solution to
be prepared in mL)
Material Required
Measuring flask (250 mL)

Funnel
Weighing tube/Watch glass
Wash bottle
Iron stand with ring clamp
:
:
:
:
:
One
One
One
One
One
Oxalic acid
: As per need
Procedure
(i)
(ii)
(iii)
Weigh an empty, clean and dry watch glass/weighing tube

accurately (Weight 1).
Weigh 3.1500 g oxalic acid by placing it on the above watch
glass/in a weighing tube (Weight 2). Always note weight up to
the fourth decimal place and clean the balance before and after
weighing the chemical.
Transfer oxalic acid carefully from the watch glass/weighing
tube into a clean and dry measuring flask using a funnel.
Weigh the empty watch glass again (Weight 3) and find out the
mass of oxalic acid transferred to the measuring flask by
substracting this mass (Weight 3) from the combined mass of
watch glass and oxalic acid (Weight 2). Calculate the exact
molarity of solution from this mass. Wash funnel several times
with distilled water by using a wash bottle to transfer the
sticking particles if any into the measuring flask. While washing
the funnel, add water in small amounts so that its volume in
the flask does not exceed th of the volume of the measuring
flask as shown in Fig. 2.27 a, b.
Oxalic acid
35
(iv)
(a)
Swirl the measuring flask till solid oxalic acid is completely

dissolved. Add more distilled water with shaking. Make up
the volume with distilled water to the etched mark by
adding last few mL dropwise. Stopper the flask and shake it
thoroughly to make the solution uniform throughout
(Fig. 2.27 c, d). Label it as 0.1 M oxalic acid solution.
(b)
Fig. 2.27 : Making standard a solution

(a) Transfering oxalic acid
(c) Adding last few mL dropwise
(c)
(d)
(b) Diluting the solution

(d) Standard solution
Precautions
(a)
(b)
(c)
(d)
(e)
(f)
(g)
(h)
(i)
(j)
36
The pan of the balance should be cleaned before and after weighing.
Never touch the weights with hand. Use forceps to transfer weights from the weightbox to the pan of the balance.
Always use spatula to transfer the reagent from the bottle on to the watch glass.
Stopper the reagent bottle immediately after withdrawing the substance.
Always use distilled water to prepare the standard solution.
Always check the adjustment of the balance before weighing the substance.
Care should be taken while weighing the chemicals. These should not be spilled
on the pan of the balance.
Watch glass/weighing bottle and funnel should be washed several times by using
small amounts of distilled water each time.
While making the solution, water should be added carefully so that the lower
part of the meniscus just touches the etched mark of the measuring flask.
To ensure uniform composition of the solution, stopper the flask and shake it
carefully and thoroughly.
(i)
What is the formula and the basicity of hydrated oxalic acid and anhydrous oxalic acid?
(ii)
What do you mean by a molar solution?
(iii)
Why are the standard solutions always prepared in a volumetric flask?
(iv)
How will you prepare 250 mL of 0.05 M oxalic acid solution?
(v)
Can solid NaOH be used to prepare its standard solution?
(vi)
What type of substance can be used for preparing standard solution?
(vii)
What is meant by weighing by transfer? When is this used?
37
UNIT-3
PURIFICATION AND
CRITERIA OF PURITY
the identification of a compound, qualitative analysis of pure substance

is required. Therefore, first we have to purify the substance and then check
its purity. There are many techniques namely, crystallisation, distillation
sublimation, chromatography etc. available for purification of a compound. In
this unit you will learn about crystallisation as a technique for purification of a
compound. The purity of a compound may be checked by determining its melting
or boiling point. The technique for determination of melting and boiling points
will also be described in this unit. Pure solid and liquid compounds possess
sharp melting and boiling points. Therefore, melting and boiling points of a
compound can be used as a criteria of purity.
OR
EXPERIMENT 3.1
Aim
Purification of sample of any one of the following Potash alum, Copper sulphate
or Benzoic acid by crystallisation.
Theory
Crystallisation is one of the techniques for the purification of an impure compound
particularly when the original crude material obtained after a reaction is in a
very impure condition. First step of the process involves choosing a single solvent
or a mixture of solvents, which dissolves the crude material readily when hot,
but only to a small extent when cold. The crude substance is then dissolved in
the minimum amount of boiling solvent to obtain a saturated solution. Insoluble
impurities are removed by filtering the hot solution. It is then checked for
crystallisation point and then cooled slowly when the solute crystallises out leaving
the greater part of impurities in the solution. The crop of crystals is collected by
filtration and the process is repeated until the crystals of pure substance are
obtained. Sometimes during cooling minute quantity of the substance (solid which
is being purified) is added to the solution to facilitate the initial crystallisation.
This is called seeding. The added tiny crystal acts as a nucleus for the growth
of new crystals. Growth of crystals depends upon the conditions in which
crystallisation is carried out. For obtaining good crystals, rapid cooling should
be avoided because it results into small or disfigured crystals.
Purity of crystals is often judged from the colour of the crystals. For example,
pure crystals of alum, copper sulphate and benzoic acid are white, blue and
PURIFICATION AND CRITERIA OF PURITY
greenish white respectively. Impurities impart colour to the crystals;

therefore, impure crystals have a colour different from pure crystals.
Material Required
Beaker (250 mL)

Glass funnel
Tripod stand
Porcelain dish
Glass rod
Sand bath
:
:
:
:
:
:
One
One
One
One
One
One
Potash alum,
Copper sulphate
and Benzoic acid
: As per need
Procedure
(i) Take 30-50 mL distilled water in a beaker and prepare a
saturated solution of potash alum/copper sulphate in it at
room temperature by adding the impure solid sample in
small amounts with stirring. Stop adding the solid when it
does not dissolve further. To prepare saturated solution of
benzoic acid use hot water.
(ii) Filter the saturated solution so prepared and transfer the
filtrate into a porcelain dish. Heat it on a sand bath till nearly
th of the solvent is evaporated. Dip a glass rod into the
solution, take it out and dry it by blowing air from the
mouth. If a solid film deposits on the rod, stop heating.
(iii) Cover the porcelain dish with a watch glass and keep the
content of the dish undisturbed for cooling.
(iv) When crystals are formed, remove the mother liquor (liquid
left after crystallisation) by decantation.
(v) Wash the crystals of potash alum and copper sulphate, thus
obtained first with very small quantity of alcohol containing
small amount of cold water to remove the adhering mother
liquor and then with alcohol to remove moisture. Wash the
crystals of benzoic acid with cold water. Benzoic acid is
soluble in alcohol. Do not use alcohol to wash its crystals.
(vi) Dry the crystals between the folds of a filter paper.
(vii) Store the dry crystals thus obtained at a safe and dry place.
(viii) Repeat steps (ii-vii) for obtaining maximum amount of pure
substance.
Copper sulphate
Precautions
(a)
(b)
(c)
Do not evaporate the entire solvent while concentrating the solution.

Do not disturb the solution while it is being cooled.
Use the washing liquid in 3-4 very small installments rather than in one installment.
39
(i) Which one of the following formula is correct representation
of potash alum(phitkari)? Explain.
+
3+
(a) K (H2O)6 Al (H2O)6( SO 4 )2

(b) K2SO4.Al2(SO4)3 . 24H2O
(ii) What are isomorphous compounds?
(iii) What is meant by the term, water of crystallisation?
(iv) Describe the effect of strong heating on each type of crystal
prepared by you.
(v) What do you understand by the term mother liquor?
(vi) Which thermodynamic function favours the process of
crystallisation?
(vii) Explain the term-saturated solution?
(viii) Why is the preparation of a saturated solution essential for
making crystals?
(ix) Name the processes involved in crystallisation?
(x) What is Kipps waste? How can we obtain crystals of ferrous
sulphate from Kipps waste?
EXPERIMENT 3.2
Aim
Determination of melting point of a solid organic compound.
Theory
The kinetic energy of molecules of a substance increases on heating.
When it becomes high enough to overcome the attractive forces
operating between the molecules, the lattice structure of the solid
breaks, the solid melts and comes into the liquid state. Melting
point of a substance is the temperature at which solid state of a
substance begins to change into the liquid state, when the pressure
is one atmosphere.
40
Material Required
Thieles tube
/Kjeldhals flask/beaker
Thermometer
Capillary tubes
Iron stand with clamps
:
:
:
:
One
One
As per need
One
Liquid paraffin
: As per need
/Conc. H2SO4
Organic Compound
(Naphthalene/
p-Dichlorobenzene/
p-Toluidine)
: As per need
Procedure
(i)
(ii)
(iii)
(iv)
(v)
(vi)
Take a capillary tube of approximately 8 cm in length. Seal

its one open end by heating it in a Bunsen flame. Rotate the
capillary while sealing to ensure complete closure of the
opening.
Crush the desired substance (about 100 mg) into fine
particles and fill the substance in the capillary tube up to
nearly 1cm length. For filling the capillary, dip its open end
in to the powder. Hold the sealed end between the index finger
and the thumb and tap the upper end gently with the other
hand so that solid particles are tightly packed and capillary
is prevented from breaking.
Moisten the capillary tube with liquid paraffin and stick it to
the thermometer. It will stick to the thermometer by cohesive
forces. See that the lower ends of the capillary tube and the
thermometer bulb are at the same level. The thermometer is
fitted into a rubber cork, which has a groove on its side for
the escape of air and vapours.
Take a Thieles tube (Fig. 3.1 a) and fill it with 50 to 60 mL
liquid paraffin so that it crosses the bent portion of the Thieles
tube. Alternatively, Kjeldahl flasks may be used in place of
Thieles tube.
Dip the thermometer along with the capillary tube in liquid
paraffin and adjust the rubber cork in such a way that the
thermometer bulb and the filled portion of the capillary is
completely dipped in the liquid paraffin and the open end of
the capillary remains in the air as shown in Fig. 3.1 a. The
thermometer and the capillary tube should not touch the
sides of the Thieles tube.
Now start heating the side arm of the Thieles tube with a low
flame from the side opposite to that of the capillary tube and
note the temperature when the solid starts melting.
p-Dichlorobenzene
p-Toluidine
Naphthalene
Hazard Warning
Avoid contact with skin

and eyes and dont inhale
vapours
of
these
chemicals.
41
Fig. 3.1 : (a) Determination of melting point using Thieles tube
Beaker
Kjeldahls flask
Fig. 3.1 : (b) Different apparatus used for determining melting point
This temperature is the melting point of the solid. If you
have taken Kjeldahl flask, heat it by revolving the flame
around the bottom of the flask to ensure uniform heating.
For this, hold the burner in your hand and also keep a
sand bath below the flask while heating. It will prevent
spilling of acid in case of accident. Repeat the experiment
with other solids.
42
Precautions
(a)
(b)
(c)
(d)
(e)
(f)
Note :
Keep the lower end of the capillary tube and the thermometer at the same level.
Capillary tube should not be very thick.
Packing of the powder should be uniform without any big air gaps in between
the solid particles.
Thieles tube should be heated at the side arm by using a low flame.
The cork of the Thieles tube or Kjeldhal flask holding the thermometer should
have a side groove so that vapours can escape through it during the process of
heating to prevent bursting of the tube or flask.
Never fill the bulb of Kjeldahl flasks more than half.
Paraffin can be safely heated upto 220C. Therefore for determination of melting point of a substance
possessing melting point higher than this, conc. H2SO4 may be used which can be heated upto 280C.
Sulphuric acid has been suggested for use but is not recomended. Silicone oils are most satisfactory
liquids and can be used in place of sulphuric acid.
(i) Why do pure solids possess sharp melting point?
(ii) What is the effect of impurities on the melting point of a solid?
(iii) Why is the melting point of benzamide more than acetamide?
(iv) Can any other liquid be used in place of liquid paraffin to determine the melting point?
(v) Can we heat the capillary directly for the determination of melting point?
(vi) Why is liquid paraffin filled in the Thieles tube/Kjeldahls flask?
(vii) Why is Thieles tube heated at the side arm?
EXPERIMENT 3.3
Aim
Determination of boiling point of a liquid organic compound.
Theory
The boiling point of a liquid is the temperature at which vapour
pressure of the liquid becomes equal to the atmospheric pressure,
which the surface of the liquid experiences. At 1.013 bar
atmospheric pressure the boiling point of the liquid is termed as
normal boiling point. Different liquids have different boiling point.
The difference in the boiling points of liquids is essentially due to
the difference in the intermolecular forces operating between the
molecules of the liquid.
43
Material Required
Thieles tube/Kjeldahls flask

Thermometer 110C or 360C
Iron stand with clamp
Ignition tube
Capillary tube
:
:
:
:
:
Concentrated H2SO4
Fig. 3.2: Determination of boiling point
One
One
One
One
One
Organic liquid : 1 mL
Liquid paraffin/
: As per need
Conc. H2SO4
Procedure
(i)
Fill Thieles tube with the liquid

paraffin so that it crosses the bent
portion of the Thieles tube.
(ii)
Take 1-2 drops of the given liquid

in an ignition tube and tie the
ignition tube with the thermometer
with a rubber band as shown in
Fig. 3.2. Note that the lower end of
the ignition tube and the
thermometer bulb are at the same
level.
(iii)
Seal one end of the capillary tube

of approximately 8 cm length by
heating in the flame.
(iv)
Place the capillary tube with its

open end dipped in the liquid
present in the ignition tube.
(v)
Heat the side arm of Thieles tube

with a low flame.
(vi)
Observe the escape of bubbles at

the lower end of the capillary
dipped in the liquid organic
compound. Note the temperature
at which bubbles start coming
briskly and continuously. This
temperature is the boiling point of
the liquid.
Note : For determination of boiling point of high

boiling liquids, paraffin cannot be used
as heating medium.
44
Precautions
(a)
(b)
(c)
(d)
Record the temperature as the boiling point at which brisk and continuous
evolution of the bubbles starts from the lower end of the capillary dipped in the
liquid organic compound.
Keep the lower end of the ignition tube and the thermometer bulb at the same
level.
Heat the side arm of the Thieles tube gently.
Boiling point of the liquid filled in Thieles tube should be 50-60C higher than
that of the liquid, of which boiling point is to be determined.
(i)
Suggest a suitable liquid, which can be filled in the Thieles tube for the determination of
the boiling point of carbon tetrachloride?
(ii)
In place of liquid paraffin, can any other liquid be used for the purpose of determination of
boiling point?
(iii)
Suppose boiling point of a liquid in Delhi is 100C. At hill station, will it be the same or
different? Give reasons.
(iv)
Why is food cooked more quickly in a pressure cooker?
(v)
How would the boiling point of water vary with the addition of equimolar quantities of
urea, potassium chloride and potassium sulphate?
(vi)
Why do different isomers of alcohol represented by the formula C4H10O differ in their boiling
points?
Do you know?
Learning technique of crystallisation is not only important from the point of view of
purification of compounds but also from the point of developing large single crystals; because
studies on single crystals have shown them to have many optical and electrical properties
of great use. For example, slices from large crystals of silicon containing traces of certain
impurities are used in making solar batteries used for the operation of instruments in
satellites. Frequency control in radar, television and radio is done by making use of slices of
some crystals. Also, use of crystals of some compounds is made in microphones and
earphones. You can now realize how important it is for chemist to learn these techniques.
45
UNIT4
CHEMICAL EQUILIBRIUM
(IONIC EQUILIBRIUM
IN
SOLUTION)
reactions can be classified into two categories; namely reversible

and irreversible reactions. Reversible reactions take place in the same
reaction vessel and can proceed in the forward and backward direction
simultaneously under the same conditions of temperature and pressure. Further
in the case of reversible reactions a state is reached, when the rate of the forward
reaction becomes equal to the rate of the reverse reaction and it appears as though
the reaction has come to a stand still. This state is referred to as the state of
dynamic equilibrium. Consider the following simple reversible reaction at the
given temperature, T.
HEMICAL
A+B
C+D
According to the law of mass action, rate of forward reaction, r1, will be directly
proportional to the product of concentrations of A and B and the rate of backward
reaction, r2, will be directly proportional to the products of concentrations of C
and D.
Thus, r1 = k1[A][B] and r2 = k 2 [C][D]
where k1 and k2 are the rate constants for the forward and the backward
reactions respectively and [A], [B], [C] and [D] are the molar concentrations of A,
B, C and D respectively.
At equilibrium, r1 will be equal to r2
k1 [A][B] = k 2 [C][D]
k1
k2
[C][D]
[A][B]
k1
Putting k = Kc we have
2
Kc =
[C][D]
[A][B]
Kc is called equilibrium constant. Its value is independent of initial

concentration of reactants and is a function of temperature but remains constant
at a constant temperature. At a given temperature, if the concentration of any
one of the reactants or products is changed, then equilibrium is disturbed and
according to Le Chatelier principle, reaction proceeds in that direction which
counteracts the change in concentration , so as to maintain the equilibrium.
CHEMICAL EQUILIBRIUM (IONIC EQUILIBRIUM IN SOLUTION)
The state of equilibrium in any reaction is recognised by the

constancy of an observable property (macroscopic property) like
colour intensity of the solution. In this unit we will study about
the shift in equilibrium in various reactions.
EXPERIMENT* 4.1
Aim
Study of shift in equilibrium in the reaction of ferric ions and
thiocyanate ions by increasing the concentration of any one of
these ions.
Theory
The equilibrium reaction between ferric chloride and potassium
thiocyanate is conveniently studied through the change in the
intensity of colour of the solution.
3+
2+
Fe (aq) + SCN (aq)
[Fe(SCN)] (aq)
(Blood red colour)
The equilibrium constant for the above reaction may be

written as:
2+
[[Fe (SCN)] (aq)]

3+
[Fe (aq)] [SCN (aq)]
Here K is constant at a constant temperature. Increasing the

concentration of either Fe3+ ion or thiocyanate ion would result in
2+
a corresponding increase in the concentration of [Fe(SCN)] ions.
In order to keep the value of K constant, there is a shift in
equilibrium, in the forward direction and consequently an increase
2+
in the intensity of the blood red colour which is due to [Fe(SCN)] .
At equilibrium colour intensity remains constant.
Material Required
Beakers (100 mL)

Beaker (250 mL)
Boiling tubes
Burettes
Glass droppers
Test tube stand
Glass rod
:
:
:
:
:
:
:
Two
One
Six
Four
Two
One
One
Ferric chloride
Potassium thiocyanate
:
:
0.100g
0.100g
* The very nature of the experiment is purely qualitative. therefore, preparation of solution in terms of molarity has
not been stressed.
47
Procedure
Ferric chloride
Hazard Warning
Avoid contact with skin

and eyes.
(i) Dissolve 0.100 g ferric chloride in 100 mL of water in a beaker

and 0.100 g potassium thiocyanate in 100 mL of water in
another beaker.
(ii) Mix 20 mL of ferric chloride solution with 20 mL of potassium
thiocyanate solution. Blood red colour will be obtained. Fill
this solution in a burette.
(iii) Take five boiling tubes of same size and mark them as a,b,c,
d and e.
(iv) Add 2.5 mL of blood red solution to each of the boiling tubes
from the burette.
(v) Add 17.5 mL of water to the boiling tube a so that total volume
of solution in the boiling tube a is 20 mL. Keep it for reference.
(vi) Now take three burettes and label them as A, B, and C.
(vii) Fill burette A with ferric chloride solution, burette B with
potassium thiocynate solution and burette C with water.
(viii) Add 1.0 mL, 2.0 mL, 3.0 mL and 4.0 mL of ferric chloride
solution to boiling tubes b, c, d and e respectively from
burette A.
(ix) Now add 16.5 mL, 15.5 mL, 14.5 mL, and 13.5 mL of water
to boiling tubes b, c, d and e respectively from burette C so
that total volume of solution in each boiling tube is 20 mL.
Fig. 4.1 : Set up of experiment for observing equilibrium,

each boiling tube contains 20 mL solution
Note : Colour intensity of the solution will decrease very much on dilution.
It will not be deep blood red colour.
Total volume in each test tube is 20 mL.
Each test tube has 2.5 mL equilibrium mixture.
Amount of FeCl3 is increasing from test tubes b to e.
48
(x) Compare the colour intensity of the solution in each boiling tube
with the colour intensity of reference solution in boiling tube a.
(xi) Take another set of four clean boiling tubes. Add 2.5 mL of
blood red solution to each of the boiling tubes from the
burette. Repeat the experiment by adding 1.0 mL, 2.0 mL,
3.0 mL and 4.0 mL of potassium thiocynate solution from
burette B to the boiling tubes b, c, d, and e respectively
followed by addition of 16.5 mL, 15.5 mL, 14.5 mL and
13.5 mL of water respectively to these test tubes. Again
compare the colour intensity of the solution of these test tubes
with reference equilibrium solution in boiling tube a.
(xii) Record your results in tabular form as in Tables 4.1 and 4.2.
(xiii) You may repeat the observations with different amounts of
potassium thiocyanate and ferric chloride solution and
compare with the reference solution.
Table 4.1 : Equilibrium shift on increasing the concentration of ferric ions
Boiling Tube
Volume of ferric
chloride solution taken
in the system in mL
Change
in
colour
intensity as matched
with reference solution in
boiling tube a
Reference solution for matching colour containing

2.5 mL blood red solution + 17.5 mL water
(20 mL equilibrium mixture)
1.0
2.0
3.0
4.0
Direction of shift in
equilibrium
Equilibrium
position
Table 4.2 : Equilibrium shift on increasing the concentration of thiocyanate ions
Boiling Tube
Volume of thiocyanate
solution taken in the
system in mL
Change
in
colour
intensity as matched
with reference solution in
boiling tube a
Reference solution for matching colour containing

2.5 mL blood red solution + 17.5 mL water
(20 mL equilibrium mixture)
1.0
2.0
3.0
4.0
Direction of shift in
equilibrium
Equilibrium
position
49
Precautions
(a)
(b)
(c)
(d)
Use very dilute solutions of ferric chloride and potassium thiocyanate.

Compare the colour of the solutions by keeping the boiling tube and the reference
test tube side by side.
To judge the change in colour of the solution in an effective manner, note the
colour change in diffused sunlight.
Use boiling tubes of the same size.
(i)
Explain why representing the ionic reaction between ferric and thiocyanate ions as given
in the text viz.
3+
2+
Fe (aq) + SCN (aq)
[Fe (SCN)] (aq)
is more appropriate in the following form ?

3+
2+
[Fe (H2O)6] + SCN (aq )
[Fe (H2O)5 (SCN)]
+ H2O.
(ii)
Does the constancy in colour intensity indicate the dynamic nature of equilibrium? Explain
your answer with appropriate reasons.
(iii)
What is equilibrium constant and how does it differ from the rate constant?
(iv)
It is always advisable to carry out the present experiment with dilute solutions. Why?
(v)
What will be the effect of adding solid potassium chloride to the system at equilibrium?
Verify your answer experimentally.
(vi)
Why boiling tubes of same size are used in the experiment?
EXPERIMENT 4.2
Aim
Study of the shift in equilibrium in the reaction between
2+
[Co(H2O)6] and Cl ions, by changing the concentration of any

one of these ions.
Theory
In the reaction between [Co (H2O)6]
displacement reaction takes place.
2+
[Co(H2O)6] + 4Cl
Pink
50
2+
and Cl ions, the following

2
[CoCl4] + 6H2O
Blue
This reaction is known as ligand displacement reaction and

the equilibrium constant, K, for this is written as follows:
Hydrochloric acid
K=
[[CoCl 4 ] ]
2+
Acetone
[[Co(H2 O)6 ] ] [Cl ]
Since the reaction occurs in the aqueous medium, it is believed

that concentration of H2O is almost constant and is included in
the value of K itself and is not shown separately in the expression
for equilibrium constant.
2+
Now if at equilibrium the concentration of either [Co (H2O)6]
ion or Cl ions is increased, then this would result in an increase

2
in [CoCl4] ion concentration thus, maintaining the value of K as
constant. In other words we can say that equilibrium will shift in
the forward direction and will result in a corresponding change
in colour.
Conical flask (100 mL)

Beakers (100 mL)
Burettes
Test tubes
Test tube stand
Glass rod
Hazard Warning
Material Required
Alcohol
:
:
:
:
:
:
One
Three
Three
Six
One
One
Acetone and alcohol are

inflamable, do not let the
bottles open when not in
use.
Keep the bottles away
from flames.
Wash your hands after
use.
Wear safety spectacles.
Acetone/alcohol
Concentrated
hydrochloric acid
Cobalt chloride
60 mL
:
:
30 mL
0.6000 g
Procedure
(i)
(ii)
(iii)
(iv)
(v)
Take 60 mL of acetone in a 100 mL conical flask and dissolve

0.6000 g CoCl2 in it to get a blue solution.
Take 5 test tubes of same size and mark them as A, B, C, D
and E. Add 3.0 mL of cobalt chloride solution in each of the
test tubes from A to E respectively. Now add 1.0 mL,
0.8 mL, 0.6 mL, 0.4 mL and 0.2 mL of acetone respectively in
these test tubes. Add 0.2 mL, 0.4 mL, 0.6 mL and 0.8 mL of
water to test tubes B, C, D and E respectively, so that the total
volume of solution in each of the test tubes is 4.0 mL.
Note the gradual change in colour of the mixture from blue
to pink with an increase in the amount of water.
Take 10 mL cobalt chloride solution in acetone prepared
above and add 5 mL distilled water to it. A solution of pink
colour will be obtained.
Take 1.5 mL of pink solution from step (iv) in five different
test tubes labeled as A B, C, D and E. Add 2.0 mL,
1.5 mL, 1.0 mL and 0.5 mL of water to the test tubes labelled
Note : In the first set

of experiments
concentration of
chlorocomplex is
constant
and
concentration of
water is changing.
In the second set
concentration of
aqua complex is
constant
and
concentration of
chloride ions is
increasing.
51
(vi)
from A to D and 0.5 mL, 1.0 mL, 1.5 mL, 2.0 mL and 2.5 mL
concentrated HCl respectively in the test tubes A to E so that
total volume of solution in the test tubes is 4 mL.
Note the gradual change in colour of pink solution to light
blue with increasing amounts of hydrochloric acid. Record
your observations in tabular form (Tables 4.3 and 4.4).
Table 4.3 : Shift in equilibrium on adding water

Sl.
No.
Test
tube
Volume of acetone
Volume of CoCl2
Volume of water
Colour
added in mL
solution added in mL added in mL
of mixture
1.
1.0
3.0
0.0
2.
0.8
3.0
0.2
3.
0.6
3.0
0.4
4.
0.4
3.0
0.6
5.
0.2
3.0
0.8
Table 4.4 : Shift in equilibrium on adding Cl ions

Volume of conc. Volume of aquo complex Volume of water
HCl added in mL solution added in mL
added in mL
Sl.
No.
Test
tube
1.
0.5
1.5
2.0
2.
1.0
1.5
1.5
3.
1.5
1.5
1.0
4.
2.0
1.5
0.5
5.
2.5
1.5
0.0
Colour
of mixture
Precautions
(a)
(b)
(c)
Take all the precautions of experiment 4.1.

Use distilled water for the experiment.
Use burette or graduated pipette for adding water or solutions.
(i)
What will be the effect of increasing the temperature of the reaction mixture at equilibrium?
(ii)
Can an aqueous solution of sodium chloride replace concentrated HCl? Verify your answer
experimentally.
(iii)
Why should the total volume of the solution in each test tube be kept same?
52
UNIT-5
PH AND PH
CHANGE
IN
AQUEOUS SOLUTIONS
have already performed experiments on dynamic equilibrium between

unionised salt and the ions produced by it on dissolving in a solvent. In
this unit we will learn about shift in ionic equilibrium between unionised
+
water molecules and H and OH ions. The conductivity experiments prove that
even pure water ionises to some extent although it has very low conductivity. On
this basis it can be concluded that ionic equilibrium exists in pure water also.
This ionic equilibrium can be represented as
OU
H2O(l)
H (aq) + OH (aq)
Since H+ ion cannot have independent existence in water because of its positive
charge and small ionic radius, a better representation of this equilibrium is
2H2O(l)
H3O (aq) + OH (aq)
This is self ionisation of water. Equilibrium constant for this chemical

equation can be written as follows:
+
K=
[H3 O ] [OH ]
2
[H2 O]
Since water is in large excess, its concentration can be assumed to be constant

and combining it with K provides a new constant Kw, which can be written as follows:
+
Kw = [H3O ] [OH ]
Kw is self ionisation constant of water or simply ionization constant of water.
14
It remains constant at constant temperature. At 25C value of Kw is 1.010 .
Thus, it is quite evident that at a given temperature in any aqueous solution,
+
this product i.e. [H3O ] [OH ] remains constant whether acidic, alkaline or neutral
in nature. If dissolution of a substance shifts the equilibrium in such a way that
at equilibrium the hydronium ion concentration is more than hydroxyl ion
concentration then the solution is acidic in nature. If dissolution of a substance
shifts the equilibrium in such a way that at equilibrium concentration of OH

ions is greater than the concentration of hydronium ions, then the solution is
alkaline in nature. Thus, concentration of hydronium ion in an aqueous solution
can provide information about acidic, basic and neutral nature of the solution.
+
The concentration of H3O ions in a solution is measured in terms of pH which is
defined as the negative logarithm of hydronium ion concentration and is given
by the following expression.
+
pH = log [H3O ]
At room temperature pH of neutral water is 7. A solution with

pH less than this is acidic while the solution with pH greater than
this is basic in nature.
EXPERIMENT 5.1
Aim
To determine the pH of some fruit juices.
Theory
Several dyes show different colours at different pH. These act as
acid-base indicators. Solution of a mixture of dyes can be used to
obtain approximate pH value of a solution. A solution of a mixture
of dyes can be obtained to measure pH values from zero to 14. It
is called universal indicator. Some universal indicators can
measure the pH change of even 0.5. In fact, dyes themselves are
weak acids or bases. Colour change occurs as a result of change
in the structure of dye due to acceptance or release of protons.
Different forms of a dye have different colours and hence, colour
change is observed when pH of the solution changes. A standard
chart for the colour change of the universal indicator with pH is
supplied with the indicator paper or solution and the comparison
of observed colour change with the chart provides a good estimate
of the pH of the solution.
54
PH AND PH
CHANGE IN AQUEOUS SOLUTIONS
Material Required
Beakers (100 mL) :
Four
Glass droppers
Four
Test tubes
Four
pH chart
One
Fruit juice
: Lemon,orange,
apple,pineapple
pH papers/universal
indicator solution
:
As per need
Procedure
(i) Procure fresh juices of lemon, orange, apple and pineapple
in separate beakers of 100 mL capacity each.
(ii) Transfer nearly 2 mL of the fresh juice (20 drops) with the
help of a separate dropper for each juice in four different
test tubes marked 1, 2, 3 and 4 respectively.
(iii) Add two drops of the universal indicator in each test tube
and mix the content of each test tube thoroughly by shaking.
(iv) Match the colour appearing in each test tube with the
standard pH chart.
(v) Record your observations in Table 5.1.
(vi) Repeat the experiment using pH papers to ascertain the pH
of different juices and match the colour in each case with
the one obtained with universal indicator.
(vii) Arrange the pH value of the four juices in increasing order.
Table 5.1 : pH value of different fruit juices

Name of the
Juice
Colour with universal

indicator
pH
Inference
Lemon
Orange
Apple
Pineapple
Result
Increasing order of pH value of juices is ____________.
55
Precautions
(a)
(b)
(c)
(d)
Add equal number of drops of universal indicator to equal volumes of solutions

in each of the test tubes.
Match the colour of the solution with pH chart carefully.
Store pH papers at a safe place to avoid contact with acidic and basic reagents
kept in the laboratory.
Use only fresh juice for the experiment.
(i)
Out of the four juices, which one is least acidic? Explain.
(ii)
If we dilute each of the juices, what effect is likely to be observed on the pH values?
(iii)
On mixing any two juices, would the pH alter or remain the same? Verify your answer
experimentally.
(iv)
How can you ascertain the pH of a soft drink ?
EXPERIMENT 5.2
Aim
To observe the variation in pH of acid/base with dilution.
Theory
Hydrogen ion concentration per unit volume decreases on dilution.
Therefore, change in pH is expected on dilution of the solution.
Material Reqiured
Boiling tubes
Glass droppers
Test tubes
:
:
:
Eight
Four
As per need
0.1 M HCl solution

0.1 M NaOH solution
0.05 M H2SO4 solution
pH paper/universal
indicator
: 20mL
: 20mL
: 20mL
: As per need
Procedure
(i)
(ii)
56
Take four boiling tubes and mark them as A, B, C and D.

(Fig. 5.1).
Take 2mL of 0.1 M HCl in boiling tube A.
PH AND PH
(iii) Take 2mL of 0.1 M HCl in boiling tube B and add 18 mL

water to it and mix thoroughly.
(iv) Take 5mL of dilute HCl solution from boiling tube B in boiling
tube C and add 15mL water to it.
NaOH
H2SO4
HCl
Hazard Warning
Never add water to the

acid.
For dilution add acid
slowly into water.
Fig. 5.1 : Set up for experiment 5.2
(v) Take 5mL of diluted HCl from boiling tube C in boiling tube
D and add 15 mL water to it.
(vi) Cut a pH paper into small pieces and spread these on a clean
glazed tile.
(vii) Take out some solution from boiling tube A with the help of
a dropper and pour one drop on one of the pieces of pH
paper kept on the glazed tile. Compare the colour of the pH
paper with the standard chart.
(viii) Similarly test the pH of solutions of boiling tubes B, C, and
D respectively and record your results as in Table 5.2.
(ix) Calculate the hydrogen ion concentration of solution B, C
and D.
(x)
Take out 1mL of solution from each boiling tube and

transfer in separate test tubes. Add 2 drops of universal
indicator to each of these test tubes. Shake the test tubes
well and match the colour of these solutions with the
standard pH chart to estimate the pH.
(xi)
Similarly observe the change in pH of 0.05 M H2SO4 and

0.1M NaOH solution with dilution as detailed in steps (i) to
(ix) above.
(xii)
Record your observations in Table 5.2.
(xiii) Compare the result obtained by using universal indicator

paper and that obtained by using universal indicator
solution.
57
Table 5.2 : pH change on dilution

HCl
Boiling tube
Colour
NaOH
H2SO4
pH
Colour
pH
Colour
pH
A
B
C
D
Result
(i)
(ii)
Concentration of solutions of test tube B, C and D are ____________.

Write your conclusion about the variation of pH with dilution.
Precautions
(a)
(b)
Add equal number of drops of the universal indicator to equal amounts of solution
in each of the boiling tubes.
Match the colour of the solution with pH chart carefully.
(i)
What trend is observed in the variation of pH with dilution for acidic as well as for basic
solutions?
(ii)
How do you explain the results of variation in pH with dilution?
(iii)
If any two acidic solutions (say A and C) are mixed, what would happen to the pH of the
mixture? Verify your answer experimentally.
(iv)
For each acidic solution, whether we use HCl or H2SO4, pH is same to a reasonably good
extent, even though HCl is 0.1M, and H2SO4 is 0.05M. How do you explain this result?
(v)
Will the pH of 0.1M acetic acid be the same as that of 0.1M hydrochloric acid? Verify your
result and explain it?
EXPERIMENT 5.3
Aim
To study the variation in pH by common ion effect in case of weak
acids and weak bases.
58
PH AND PH
Theory
It is a known fact that the ionisation in the case of either a weak acid
or a weak base is a reversible process. This can be represented as:
(1) HA
H +A
(2) BOH
B + OH
(weak acid)
(weak base)
The increase in concentration of A ions in case (1) and that of B

ions in case (2) would shift the equilibrium in the reverse direction
+
thereby decreasing the concentration of H ions and OH ions in

cases (1) and (2) respectively so as to maintain the constancy of
+
equilibrium constant K. This change either in H ion concentration
or OH ion concentration brings a change in the pH of the system,

which can be judged either with the help of a pH paper or by using
a universal indicator solution.
Material Required
Beakers (100 mL)
: Four
Pipettes (25 mL)
: Two
Test tubes
: Four
pH chart
: One
Sodium ethanoate
Ammonium chloride
Ethanoic acid (1.0 M)
Ammonia solution (1.0 M)
pH paper and
universal indicator
:
:
:
:
2g
2g
50 mL
50 mL
As per need
Procedure
(i) Take four 100 mL beakers and mark them as A, B, C and D.
(ii) Transfer 25 mL of 1M ethanoic acid in beaker A and 25 mL
of (1M) ammonia solution in beaker B.
(iii) Similarly transfer 25 mL of (1 M) ethanoic acid in beaker C
and 25 mL of (1.0 M) ammonia solution in beaker D. Now
add 2 g sodium ethanoate in beaker C and dissolve it.
Likewise add 2 g of ammonium chloride in beaker D and
dissolve it by shaking the content of the beaker thoroughly.
(iv) Take approximately 2 mL (20 drops) of the solution from
beakers A, B, C and D respectively into test tubes marked
as 1, 2, 3 and 4.
(v) In each of the test tubes add 2 drops of universal indicator
solution. Shake the content of the test tubes well and match
the colour in each case with the standard pH chart.
(vi) Record your observations as given in Table 5.3.
(vii) Compare pH of the solution in test tubes 1 and 3 and record
the change in pH.
(viii) Similarly compare pH of the solution in test tubes 2 and 4
and record the change in pH.
Ammonia solution
Ethanoic acid
Ammonium chloride
59
Table 5.3 : Comparison of pH of acid/base and its buffer

Sl. No. of
Test Tube
Composition of the
system
CH3COOH in water
NH4OH (NH3 in water)
CH3COOH + CH3COONa
NH4OH+NH4Cl
Colour
of pH paper
pH
Result
(a)
(b)
(c)
(d)
(e)
pH of acetic acid is _______

pH of buffer of acetic acid and sodium acetate is ________ than acetic acid.
pH of ammonia solution is _______
pH of buffer of ammonia solution and ammonium chloride is _________ than the
ammonia solution.
Common ion effect ________ ionization of acid/base.
Precautions
(a)
(b)
(c)
(e)
Try only weak acid/weak base and its salt for the study of the common ion effect.
Handle the bottle of ammonium hydroxide with care.
Add equal number of drops of the universal indicator in each of the test tubes.
Store pH papers at a safe and dry place.
(i)
The addition of sodium acetate to acetic acid increases the pH whereas, the addition of
NH4Cl to aqueous NH3 solution (NH4OH) decreases the pH of the system. How do you
explain these observations?
(ii)
Suggest suitable replacement for CH3COONa for system 3 and NH4Cl for system 4.
(iii)
Suggest other pairs of weak acid and its salt and weak base and its salt to carry out the
present investigations.
(iv)
In salt analysis/mixture analysis, point out the situations where the variation in pH is
carried out by common ion effect.
(v)
How do buffer solutions resist change in the pH? Explain with a suitable example.
60
PH AND PH
EXPERIMENT 5.4
Aim
To study the change in pH during the titration of a strong acid
with a strong base by using universal indicator.
Theory
It is assumed that strong acids and strong bases are completely
dissociated in solution. During the process of neutralisation,
H+ ions obtained from the acid combine with the OH ions produced
by base and form water. Therefore, when a solution of strong acid
is added to a solution of strong base or vice versa, the pH of the
solution changes. As the titration proceeds, initially there is slow
change in the pH but in the vicinity of the equivalence point there
is very rapid change in the pH of the solution.
Material Required
Burette
:
Beakers (250 mL)
:
Conical flask (100 mL) :
Dropper
:
pH chart
:
One
Two
One
One
One
Hydrochloric acid
(0.1 M)
Sodium Hydroxide
solution (0.1 M)
Universal indicator
: 25 mL
: 50 mL
: As per requirement
Procedure
(i)
Take 25 mL hydrochloric acid solution (0.1 M) in 100 mL

conical flask.
Hydrochloric acid
(ii)
Add five drops of universal indicator solution to it.
Sodium hydroxide
(iii)
Add (0.1 M) sodium hydroxide solution from the burette as

given in Table 5.4.
(iv)
Shake the content of the flask well after each addition of

sodium hydroxide solution. Note the colour of the solution
in the conical flask each time and find out the pH by
comparing its colour with the pH chart.
(v)
Note down your observations in Table 5.4.
(vi)
Plot a graph of pH vs. total volume of NaOH added.
61
Table 5.4 : pH change during the neutralisation of

25 mL of HCl (0.1 M) with NaOH (0.1 M) solution
Sl. No.
Volume of NaOH
added in lots (mL)
Total volume of NaOH added

to the solution in flask (mL)
1.
2.
12.5
12.5
3.
10.0
22.5
4.
2.3
24.8
5.
0.1
24.9
6.
0.1
25.0
7.
0.1
25.1
8.
0.1
25.2
9.
0.1
25.3
10.
0.1
25.4
11.
0.5
25.9
pH
Precautions
(a)
(b)
(c)
To get good results perform the reaction with solutions of strong acid and strong
base of same concentration.
Handle the bottle of acid and base with care.
Use small amount of indicator.
Result
Write down your result on the basis of data.
(i)
What trend of pH change will you observe in the neutralisation of strong acid with strong
base?
(ii)
Do you expect the same trend of pH change for neutralisation of weak acid (acetic acid)
with a strong base (sodium hydroxide)?
(iii)
In which pH range should the indicator show colour change if the hydrochloric acid is to be
neutralised by sodium hydroxide? Give answer after looking at the graph of the experiment.
(iv)
Explain how does the study of pH change help in choosing the indicator for neutralisation
reaction.
62
PH AND PH
EXPERIMENT 5.5
Aim
To study pH of solutions of sodium chloride, ferric chloride and
sodium carbonate.
Theory
Salts of strong acid and strong base form neutral solutions while
salts of weak acid/base and strong base/acid are basic and acidic
respectively in nature. Salts of weak acid/base with strong base/
acid are hydrolysed in water while salts formed by neutralization
of strong acid and strong base do not hydrolyse in solution. You
have already learnt about this in your chemistry textbook.
Material Required
Boiling tubes
Test tubes
Glass droppers
: Three
: Three
: Three
pH paper/universal indicator :
0.1 M NaCl solution
:
:
0.1 M FeCl3 solution
:
0.1 M Na2CO3 solution
As per need
As per need
As per need
As per need
Procedure
(i)
(ii)
Take three boiling tubes and mark them as A, B and C.

Take 20 mL of 0.1 M solution(s) of NaCl, FeCl3 and Na2CO3
in boiling tubes A, B and C respectively.
(iii) Cut the pH paper in small pieces and spread the pieces on a
clean glazed tile.
(iv) Test the pH of the solution in boiling tubes A, B and C as in
the experiment 5.1.
(v) Arrange three clean test tubes in a test tube stand.
(vi) Number the test tubes as 1, 2 and 3.
(vii) Pour 4 mL solution from boiling tube A in each of the test
tubes.
(viii) Add 5 mL, 10 mL and 15 mL water in the test tubes 1, 2 and
3 respectively.
(ix) Note the pH of the solutions of test tubes 1, 2 and 3 with the
help of pH paper and universal indicator.
(x) Repeat the experiment with the solutions of boiling tubes B
and C.
(xi) Note your results in tabular form as in Table 5.5.
63
Table 5.5 : pH of NaCl, FeCl3 and Na2CO3 solutions of different concentrations

pH of solution
Solution
Test tube 1
Test tube 2
Test tube 3
NaCl
FeCl3
Na2CO3
Result
Write down the result on the basis of your observations.
Precautions
(a)
(b)
(c)
(d)
Use freshly prepared solutions.

Do not leave the bottles open after taking out salt.
Use separate and clean test tube for each solution.
Store the pH paper at a safe and dry place.
(i)
Why are FeCl3 and Na2CO3 solutions not neutral?
(ii)
Why are the salts of strong acid and strong base not hydrolysed? Explain.
(iii)
How is the phenomenon of hydrolysis useful in salt analysis?
(iv)
What is the effect of dilution on pH of salt solution? Verify and explain your results.
64
UNIT-6
TITRIMETRIC ANALYSIS
OU are already aware that a substance is analysed to establish its qualitative

and quantitative chemical composition. Thus, chemical analysis can be
categorised as qualitative analysis and quantitative analysis. In this unit
you will learn about determination of the amount of substance in solution. Depending
upon the method adopted for determining the amount of chemical substances in
solution, there are two methods of analysis namely, titrimetric analysis and
gravimetric analysis. In titrimetric analysis measurement of only volumes is involved
while in gravimetric analysis measurement of volumes as well as mass is involved.
Titrimetric analysis involves determination of the volume of a solution of
accurately known concentration, which is required to react quantitatively with
the measured volume of the solution of a substance, concentration of which is to
be determined. The solution of accurately known concentration is called standard
solution. The mass of the substance dissolved in the solution of unknown
concentration is calculated from the volume of the standard solution used, the
chemical equation and the relative molecular masses of the reacting compounds.
The reagent of known concentration is called titrant and the substance being
titrated is termed as titrand.
To carry out titrimetric analysis, standard solution is usually added from
the long graduated tube called burette. The process of adding the standard
solution to the solution of unknown concentration until the reaction is just
complete is called titration. The point at which reaction is completed is called
equivalence point or the theoretical or stoichiometric end point. It is not
possible all the time to take standard solution in the burette. You will come to know
about it later in this unit in the titration of sodium hydroxide with oxalic acid.
6.1 DETECTION OF END POINT

The end point is detected either by some physical change produced in the reaction
mixture itself or by the addition of an auxiliary reagent, known as indicator;
alternatively some other physical measurement may be used. At the completion
of the reaction, the indicator shows a visible change e.g. (colour change or turbidity)
in the solution being titrated. In an ideal titration, the visible end point coincides
with the stoichiometric or theoretical end point; but in practice usually some
small difference occurs. This represents titration error.
Indicator and the experimental conditions selected should be such that the
difference between the visible end point and the theoretical end point is
minimum.Requirements for a Reaction in the Titrimetric Analysis
6.2 REQUIREMENT FOR A REACTION IN THE TITRIMETRIC ANALYSIS

(i)
(ii)
The substance of which amount is to be determined by

titrimetric analysis must react completely and rapidly with
the other reagent in stoichiometric proportion.
The reaction should be fast and there must be alteration in
physical or chemical property of the solution at the
equivalence point, which can be detected by an indicator, or
by measuring the potential difference or current etc.
6.3 ACIDIMETRY AND ALKALIMETRY

Titrimetric analysis can be carried out for various types of reactions.
In this unit you will learn only about neutralisation reactions.
These involve titrations of acids and bases. Standard solutions of
acids (acidimetry) and bases (alkalimetry) are used in these
titrations. In quantitative estimation through titrimetric analysis,
concentration of solution is expressed in terms of molarity. It is
number of moles of solute dissolved in 1 litre of solution.
Molarity, M =
number of moles of solute

volume of solution in litres
Standard Solution
A solution of exactly known concentration is called standard
solution. Any substance, which is stable at room temperature and
does not react with solvent in which it is dissolved, can be directly
weighed to prepare its standard solution. Description and
preparation of these solutions is given below:
Primary and secondary standards

A primary standard is a compound of sufficient purity in which
total amount of impurities does not exceed 0.01-0.02%. The
standard solution can be prepared by direct weighing of a sample
of primary standard followed by its dissolution in water (or solvent)
to obtain a definite volume of solution. The substance to be used as
a primary standard should also satisfy the following requirements:
1. It must be easily available in pure and dry form.
2. It should not undergo change in air i.e. it should not be
hygroscopic, oxidised by air or affected by gases such as
carbon dioxide present in the atmosphere or lose water of
crystallization, so that it can be stored safely.
3. It should be easy to detect the impurities present in it.
4. It should have high relative molecular mass so that weighing
errors are neglible.
5. Its reaction with another substance should be instantaneous
and stoichiometric.
6. The substance should be readily soluble in water.
66
It is difficult to obtain an ideal primary standard.

Therefore, substances having characteristics nearer to the
primary standards are usually employed.
Unstable hydrated salts, as a rule, should not to be used as
primary standards. However, sodium carbonate, sodium
tetraborate, potassium hydrogenphthalate, oxalic acid, ferrous
ammonium sulphate etc. can be used as primary standards
because of their sufficient stabilities.
A solution of secondary standard is the one which may be
used for standardization after finding out its exact concentration
by titration against a standard solution of primary standard.
A secondary standard cannot be used for preparing standard
solution by direct weighing. Sodium hydroxide and potassium
permanganate are examples of secondary standards.
Before starting titrimetric analysis, you should be familiar with
some techniques such as, weighing by using chemical balance,
preparing standard solution, measuring volume by using burette
and pipette.
6.4 INDICATORS IN ACID BASE TITRATION

Acid base indicators are sensitive to pH change. For most acid base
titrations, it is possible to select indicators which exhibit colour
change at pH close to the equivalence point. We will discuss here
about only two indicators phenolphthalein and methyl orange.
Phenolpthalein
Phenolpthalein is a weak acid, therefore it does not dissociate in
the acidic medium and remains in the unionised form, which is
colourless.
HPh
ZZZX
YZZ
Z
H + Ph
Unionised
Ionised
Colourless
Pink
Ionised and unionised forms of phenolphthalein are given below :
(Colourless in acid)
(Pink in alkali)
Fig. 6.1 : Phenolphthalein in acidic and basic medium
67
In the acidic medium, equilibrium lies to the left. In the alkaline

medium, the ionisation of phenolphthalein increases considerably
+
due to the constant removal of H ions released from HPh by the
OH ions from the alkali. So the concentration of Ph ion increases

in the solution, which imparts pink colour to the solution.
HPh
NaOH
+
H + OH
ZZZX
YZZ
Z
H + Ph
+
Na + OH
H2O
For a weak acid vs strong alkali titration, phenolphthalein is

the most suitable indicator. This is so because the last drop of
added alkali brings the pH of the solution in the range in which
phenolphthalein shows sharp colour change.
Methyl orange
Methyl orange is a weak base and is yellow in colour in the unionised
form. Sodium salt of methyl orange is represented as follows:
The anion formed from the indicator is an active species, which

on accepting a proton (i.e acting as Bronsted Lowry base) changes
from the benzenoid form to the quinonoid form. The quinonoid
form is deeper in colour and thus is responsible for the colour
change at the end point. This is illustrated in the following manner:
Benzenoid form of the anion

(Yellow in colour)
Quinonoid form of the anion

(Pinkish red in colour)
(Bronsted-Lowry base)
Fig. 6.2 : Structures of Methyl orange
Choice of Indicator
In the titration of strong acid and a weak base, methyl orange is
chosen as indicator. When titration between strong base and weak
acid is to be performed then phenolphthalein is a good indicator.
In this case alkali is dropped from the burette and acid is taken in
the tiration flask. Colour of the solution taken in the titration flask
68
changes from colourless to pink. This change of colour is easily

perceptible to the human eye. If we take alkali in the titration flask,
the colour change will be from pink to colourless and accuracy in
noting the colour change may be less. In the titration of strong
acid versus strong base anyone of the above indicators can be
used. For the titration of weak acid vs weak base no indicator is
available.
EXPERIMENT 6.1
Aim
Determination of the concentration (strength) of a given sodium
hydroxide solution by titrating it against a standard solution of
oxalic acid.
Theory
In the titration of a strong acid with a strong base, the amount of
acid and base becomes chemically equivalent at the end point and
the chemical reaction is called neutralization reaction. Near the
end point there is a sudden change in the pH of the solution. If
after end point even a small amount of base/acid is added the
solution would become slightly alkaline or acidic respectively. In
the titration between oxalic acid (weak acid) and sodium hydroxide
(strong base), following reaction takes place:
In this titration phenolphthalein (HPh) is used as an indicator.

The concentration of unknown solution is calculated in g/L.
Molarity of the solution can be calculated by using the formula
a1 M1 V1 = a2 M2 V2
...(4)
where a1, M1, V1 are respectively basicity, molarity and volume

of acid used and a2, M2 and V2 are acidity, molarity and volume
respectively of base used in the titration.
69
Material Required
Burette (50 mL)

Pipette (10 mL)
Burette stand
Funnel
White glazed tile
:
:
:
:
:
:
:
One
One
One
One
One
One
One
Oxalic acid
: As per need
Sodium hydroxide
solution
: As per need
Phenolphthalein
indicator
: As per need
Procedure
Oxalic acid
(A) Preparation of 0.1M Standard Solution of Oxalic Acid

Follow the procedure as described in Experiment No. 2.1.
Sodium Hydroxide
(B) Titration of Sodium Hydroxide and Oxalic Acid Solution

(i) Clean the burette thoroughly, wash it with distilled water
and finally rinse it with sodium hydroxide solution. (Always
rinse the burette (Fig. 2.17) with the solution, which is to be
taken in it). Clamp the burette vertically in a burette stand.
(ii) Fill sodium hydroxide solution into the burette through a
funnel above the zero mark.
(iii) Remove the air gap, if any, from the nozzle of the burette
by running the solution forcefully from the burette nozzle.
(iv) Remove the funnel before noting initial reading of the
burette. Also while noting the reading, see that no drop of
the liquid is hanging at the nozzle of the burette.
(v) Note the initial reading by keeping the eye exactly at the
same level as the meniscus of the solution.
(vi) Pipette out 10 mL of oxalic acid solution in a washed and
dried conical flask. Always wash the pipette with water and
rinse (Fig. 2.21) with the liquid to be measured before
pipetting out the liquid.
(vii) Add 1-2 drops of phenolphthalein indicator to the conical
flask. Place the flask over the glazed tile as shown in
Fig. 6.3 Titrate the acid with sodium hydroxide solution
till a very faint permanent pink colour is obtained. Add
sodium hydroxide solution in small amounts initially and
then dropwise.
70
Note : Adjust the flow of liquid by the thumb and two
fingers held around the stop cock with a slight
inward pressure on the plug to prevent leakage.
Swirl the liquid during the titration.
Fig. 6.3 : Titrating the solution
(viii) Read the lower meniscus of the solution in the burette again
and record it as final reading.
(ix) Repeat the procedure until three concordant readings are
obtained. Record your readings as in Table 6.1.
Table 6.1 : Titration of sodium hydroxide vs oxalic acid solution
Sl. No.
Volume of oxalic
acid solution
taken in conical
flask each time
V1mL
Burette readings
Initial
reading
(x)
Final
reading
(y)
Volume of sodium
hydroxide solution
used
V2 mL = (yx) mL
Concordant
reading in
mL
71
Calculations
Molarity of NaOH solution can be calculated by using the equation:
Oxalic acid Sodium hydroxide
a1 M1V1
a2 M2V2
where, M1 and V1 are the molarity and volume of the oxalic

acid solution.
M2 and V2 are the molarity and volume of the sodium hydroxide
solution.
a1 and a2 are respectively the basicity of oxalic acid and acidity
of sodium hydroxide. In this case a1= 2 and a2 = 1.
Also, Molar mass of oxalic acid, (COOH) 2.2H2O = 126 g mol
1
and Molar mass of sodium hydroxide (NaOH) = 40 g mol
Calculate the concentration of sodium hydroxide solution in g/L

by using the equation given below.
Concentration (strength) in g/L = MolarityMolar mass
Result
Concentration of NaOH solution is g/L.
Precautions
(a)
(b)
(c)
(d)
(e)
(f)
(g)
(h)
(i)
(j)
(k)
72
Always rinse the burette with the solution, which is to be taken in it.
Remove the air gap if any, from the burette before titrating the solution. Make
sure that the nozzle of burette is also filled.
Never forget to remove the funnel from the burette before noting the readings of
the burette and ensure that no drop is hanging from the nozzle of the burette.
Always read the lower meniscus for all transparent solutions and upper meniscus
for coloured solutions.
To note the burette readings place the eye exactly at the level of the meniscus.
Never hold the pipette at the bulb.
Never use the pipette and burette with a broken nozzle.
Never suck a strong acid or an alkali with the pipette.
Always keep the lower end of the pipette dipped in the liquid while sucking the
liquid.
Do not blow out the last drop of the solution from the jet end of the pipette into
the flask.
The concentration (strength) of the solution must be calculated up to the fourth
place of decimal.
(i) Why are the burette and the pipette rinsed with the solution with which these are filled?
(ii) What is an indicator? Which indicator is used in the titration of oxalic acid vs sodium
hydroxide? Can the titration be performed by using some other indicator?
(iii) Why should one read the lower meniscus in the case of colourless and transparent solutions
and the upper meniscus for solutions of dark colour?
(iv) Explain the term end point?
(v) What do you mean by 1.0 M solution?
(vi) Why should the last drop of the solution not be blown out of a pipette?
(vii) Explain the term basicity of an acid and acidity of a base?
(viii) For titrating NaOH vs HCl, phenolphthalein and methyl orange, both are suitable indicators.
Why?
(ix) What is meant by the term , concordant readings?
(x) Can one take oxalic acid solution in the burette and sodium hydroxide solution in the
titration flask? Point out the limitations of doing so if any.
KNOW
THIS ALSO
The complete neutralisation is possible only when the amount of alkali is in equivalent
proportion to the amount of acid. Therefore, at the end point equivalent mass of acid dissolved
in volume V1 of solvent should be equal to the equivalent mass of the base dissolved in
Volume V2 of solvent. If N1 and N2 are equivalent masses of acid and base respectively dissolved
(i)
in per litre of solution then N1V1 = N2V2
Equivalent mass of acids and bases is given by the following expression:
Equivalent mass of acid =
Equivalent mass of base =
molar mass
(ii)
basicity
molar mass
acidity
... (iii)
The number of gram equivalent mass of solute dissolved in one litre of the solution is
called the normality of the solution. For acids and bases
Normality (N)=
Number of gram equivalent mass

w/ Equivalent mass
=
(iv)
Volume of solution in litre (V )
Volume of solution in litre (V )
Where w = mass of substance in grams
Relationship between Normality and Molarity

From definition of normality (N) [(equation (iv)]
Equivalent mass =
w
N V
... (v)
If acidity or basicity is a, then by definition of equivalent mass
73
Equivalent mass =
Molar mass
a
From equations (v) and (vi) we can write
w
N
Or
But
(vi)
Molar mass
V
a (w/Molar mass )
V
w/Molar mass
is the molarity (M)
Therefore, N = a M
(vii)
Equation (vii) is the expression for the relationship between normality and molarity.
.... (viii)
By using equation (vii) in equation (i) we have a1M1V1 = a2M2V2
Where a1 and a2 are basicity and acidity of acid and base respectively and M1 and M2 are
the molar masses of acid and base respectively. Thus we see that equation (i) can also be
used to calculate the strength of the solution. Equation (viii) can be used for making the
solution by dilution. For solutions of the same substance a1 = a2. Therefore for using equation
(viii) for dilution of solution
...(ix)
M1V1 = M2V2
Therefore, to obtain V2 volume of a solution of molarity M2 from a solution of molarity M1,
the volume V1 of the solution of molarity M1 which is required for dilution, can be calculated
from equation (ix). (V2V1) volume of solvent will be required to be added to V1 volume of the
solution of molarity M1.
EXPERIMENT 6.2
Aim
Preparation of 0.1 M standard solution of sodium carbonate.
Theory
Sodium carbonate has characteristics nearer to the primary
standards therefore its standard solution can be made by direct
weighing.
To prepare 0.1 M Na2CO3 solution, 10.6000g of sodium
carbonate should be dissolved per litre of the solution (Molar mass
1
of sodium carbonate is 106 g mol ).
Therefore, to prepare 100 mL of 0.1M Na2CO3 solution 1.0600 g
of sodium carbonate is dissolved in minimum quantity of water
and the solution is diluted to exactly 100 mL by adding water to it.
74
Material Required
Measuring flask (100 mL) :

Watch glass
:
Funnel
:
Wash bottle
:
One
One
One
One
Sodium carbonate
: As per need
Procedure
Follow the same procedure as in Experiment 2.1.
EXPERIMENT 6.3
Aim
Determination of the strength of a given solution of dilute
hydrochloric acid by titrating it against a standard solution of sodium
carbonate.
Theory
The strength of hydrochloric acid is determined by titrating it against
a standard solution of sodium carbonate. The following reaction
takes place:
Na2CO3 + 2HCl 2 NaCl + CO2 + H2O
In this titration, methyl orange, a weak base (yellow in the
unionised form) is used as an indicator.
In this experiment also, the titration follows the usual course,
i.e., the proton furnished by the addition of the acid first neutralises
sodium carbonate solution. When the entire sodium carbonate
solution is neutralised, the last drop of the acid added from the burette
produces the pinkish red colour change, which is the end point.
The concentration (strength) of the unknown solution is
calculated in g/L. It is calculated from the molarity of the solution.
Here, the molarity equation is written as
Base
Acid
a1M1V1 = a2M2V2
where, a1 and a2 are the acidity and basicity of the alkali and the
acid respectively. M1 and M2 are the molarities, V1 and V2 are the
volumes of the base and acid respectively used to neutralise each
other.
75
Material Required
Burette (50 mL)

:
Pipette (10 mL)
:
:
Burette stand
:
Funnel
:
Glazed tile (white)
:
Measuring flask (100 mL) :
One
One
One
One
One
One
One
Hydrochloric acid
Sodium carbonate
Methyl orange solution
: As per need
: As per need
: As per need
Procedure
(A)
Hydrochloric acid
Preparation of 0.1 M standard solution of sodium

carbonate
Follow the procedure as described in Experiment 2.1.
(B)
Titration of hydrochloric acid and standard sodium

carbonate solution.
Follow the procedure as given in the Experiment 6.1.

In this case, hydrochloric acid is taken in the burette and
sodium carbonate solution in the conical flask. Methyl orange is
used as an indicator. The colour change at the end point will be
from yellow to pinkish-red. Record your observations in Table 6.2.
Table 6.2 : Titration of Hydrochloric acid with standard sodium carbonate solution
Sl. No.
76
Volume V1 of
Na2CO3 solution
taken in the
conical flask
each time in mL
Burette readings
Initial
reading
(x)
Final
reading
(y)
Volume of HCl
solution used
V2 mL = (yx) mL
Concordant
reading
in mL
Calculations
Calculate the strength of HCl solution by using the equation
HCl solution
Na2CO3 solution
=
a2M2V2
a1M1V1
where M 1 and V1 are the molarity and volume of sodium carbonate solution
respectively and a1 is the number of moles of OH (aq) ions supplied by one

mole of the base (i.e. the acidity of the Na2CO3 solution).
a1 = 2
M2 and V2 are the molarity and volume respectively of hydrochloric acid

solution.
+
a2 is the number of moles of H (aq) ions supplied by one mole of the acid
(i.e. the basicity of HCl).
a2 = 1
1
Molar mass of Na2CO3 = 106 g mol , Molar mass of HCl = 36.5 g mol ,
Concentration (Strength) of HCl solution in g/L = Molarity Molar mass
Result
The concentration (strength) of the given HCl solution is _______g/L.
Precautions
(a)
(b)
(c)
(d)
(e)
(f)
(g)
(h)
(i)
(j)
Care should be taken while handling the acid and base.

Always rinse the burette and the pipette with the solution which is to be taken in
them.
Remove the air gap if any, from the burette before titration.
Never forget to remove the funnel from the burette before noting the initial reading
of the burette and ensure that no drop is hanging from the nozzle.
Always read the lower meniscus for all transparent solutions and upper meniscus
for the coloured solutions.
Never use burette and pipette with a broken nozzle.
Never suck a strong acid or an alkali with the pipette, use pipette bulb.
Always keep the lower end of the pipette dipped in the liquid while sucking the
liquid.
While transferring the solution to the flask, do not blow out the last drop of the
solution from the jet of the pipette.
The strength of the solution must be calculated up to the fourth decimal place.
77
KNOW
THIS ALSO
Potassium hydrogenphthalate is primary standard for standardisation of sodium hydroxide

solution. Formula of potassium hydrogen phthalate is C6H5O4K. It behaves as a monobasic
acid. Sodium hydroxide reacts with potassium hydrogenphthalate according to the following
equation.
Phenolphthalein can be used as an indicator in this titration.
(i) Which indicator is used in the titration of sodium carbonate against hydrochloric acid and
what is the colour change at the end point?
(ii) How will you prepare 250 mL of 0.05 M solution of sodium carbonate?
(iii) Though sodium carbonate is a salt yet its aqueous solution is weakly alkaline in nature.
Explain why?
(iv) How can you determine the acidity of sodium carbonate solution?
(v) Why is methyl orange not an Arrhenius base?
(vi) How can you titrate a solution of the mixture of Na2CO3 and NaHCO3 against HCl?
(vii) What is the difference between an end point and an equivalence point?
(viii) Can you directly prepare standard solution of HCl, HNO3 and H2SO4 ?
78
UNIT-7
SYSTEMATIC QUALITATIVE
ANALYSIS
always does not mean breaking of substance into its ultimate

constituents. Finding out the nature of substance and identity of
its constituents is also analysis and is known as qualitative analysis.
Qualitative analysis of inorganic salts means the identification of cations and
anions present in the salt or a mixture of salts. Inorganic salts may be obtained
by complete or partial neutralisation of acid with base or vice-versa. In the
formation of a salt, the part contributed by the acid is called anion and the part
contributed by the base is called cation. For example, in the salts CuSO4 and
2+
2
NaCl, Cu and Na+ ions are cations and SO4 and Cl ions are anions. Qualitative
analysis is carried out on various scales. Amount of substance employed in
these is different. In macro analysis, 0.1 to 0.5 g of substance and about 20 mL
of solution is used. For semimicro analysis, 0.05 g substance and 1 mL solution
is needed while for micro analysis amount required is very small. Qualitative
analysis is carried out through the reactions which are easily perceptible to our
senses such as sight and smell. Such reactions involve:
NALYSIS
(a) Formation of a precipitate

(b) Change in colour
(c) Evolution of gas etc.
Systematic analysis of an inorganic salt involves the following steps:
(i) Preliminary examination of solid salt and its solution.
(ii) Determination of anions by reactions carried out in solution (wet tests)
and confirmatory tests.
(iii) Determination of cations by reactions carried out in solution (wet tests)
and confirmatory tests.
Preliminary examination of a salt often furnishes important information, which
simplifies further course of analysis. Although these tests are not conclusive but
sometimes they give quite important clues for the presence of certain anions or
cations. These tests can be performed within 1015 minutes. These involve noting
the general appearance and physical properties, such as colour, smell, solubility
etc. of the salt. These are named as dry tests.
Heating of dry salt, blow pipe test, flame tests, borax bead test, sodium
carbonate bead test, charcoal cavity test etc. come under dry tests. Some of these
tests are given later in this unit.
Solubility of a salt in water and the pH of aqueous solutions give important

information about the nature of ions present in the salt. If a solution of the salt is
acidic or basic in nature, this means that it is being hydrolysed in water. If the
solution is basic in nature then salt may be some carbonate or sulphide etc. If
the solution shows acidic nature then it may be an acid salt or salt of weak base
and strong acid. In this case it is best to neutralise the solution with sodium
carbonate before testing it for anions.
Gases evolved in the preliminary tests with dil. H2SO4/dil. HCl and conc. H2SO4
also give good indication about the presence of acid radicals (see Tables 7.1 and
7.3). Preliminary tests should always be performed before starting the confirmatory
tests for the ions.
EXPERIMENT 7.1
Aim
To detect one cation and one anion in the given salt from the following ions:
2+
2+
3+
3+
3+
2+
2+
2+
2+
2+
2+
2+
Cations - Pb , Cu , As , Al , Fe , Mn , Ni , Zn , Co , Ca , Sr , Ba ,
+
2+
Mg , NH 4
2
Anions - CO3 , S , SO3 ,
SO 4 , NO2 , NO3 , Cl , Br , I , PO 4 , C2 O 4 ,
CH3COO .
(Insoluble salts to be excluded)
Theory
Two basic principles of great use in the analysis are:
(i) the Solubility product and
(ii) the Common ion effect
When ionic product of a salt exceeds its solubility product, precipitation takes
place. Ionic product of salt is controlled by making use of common ion effect
which you have studied in the textbook of chemistry.
Material Required
80
Boiling tube
Test tubes
Measuring cylinder
Test tube stand
Test tube holder
Delivery tube
Corks
Filter paper
:
:
:
:
:
:
:
:
As per need
As per requirement
One
One
One
One
As per need
As per need
Reagents
As per need
SYSTEMATIC QUALITATIVE ANALYSIS
SYSTEMATIC ANALYSIS OF ANIONS

Step - I : Preliminary Test with Dilute Sulphuric Acid
In this test the action of dilute sulphuric acid (procedure is given
below) on the salt is noted at room temperature and on warming.
2
Carbonate ( CO 3 ), sulphide (S2), sulphite ( SO3 ), nitrite ( NO 2 )
and acetate (CH3COO ) react with dilute sulphuric acid to evolve

different gases. Study of the characteristics of the gases evolved
gives information about the anions. Summary of characteristic
properties of gases is given in Table 7.1 below.
Procedure
(a)
Take 0.1 g of the salt in a test tube and add 12 mL of

dilute sulphuric acid. Observe the change, if any, at
room temperature. If no gas is evolved, warm the
content of the test tube. If gas is evolved test it by using
the apparatus shown in Fig.7.1 and identify the gas
evolved (See Table 7.1).
Fig. 7.1 : Testing a Gas
Table 7.1 : Preliminary test with dilute sulphuric acid

Inference
Observations
Gas evolved
A colourless, odourless gas is evolved
with brisk effervescence, which turns
lime water milky.
CO2
Colourless gas with the smell of rotten

eggs is evolved which turns lead acetate
paper black.
H2S
Colourless gas with a pungent smell, like

burning sulphur which turns acidified
potassium dichromate solution green.
SO2
Brown fumes which turn acidified

potassium iodide solution containing
starch solution blue.
NO2
Colourless vapours with smell of

vinegar. Vapours turn blue litmus red.
CH3COOH vapours
Possible Anion
Carbonate ( CO3 )
Sulphide (S )
Sulphite ( SO 3 )
Nitrite ( NO 2 )
Acetate, (CH3COO )
81

2-
2-
Confirmatory tests for CO3 S , SO3 , NO2 and CH3COO
Confirmatory (wet) tests for anions are performed by using water extract when
salt is soluble in water and by using sodium carbonate extract when salt is
2
insoluble in water. Confirmation of CO3 is done by using aqueous solution of
the salt or by using solid salt as such because sodium carbonate extract contains
carbonate ions. Water extract is made by dissolving salt in water. Preparation of
sodium carbonate extract is given below.
Preparation of sodium carbonate extract

Take 1 g of salt in a porcelain dish or boiling tube. Mix about 3 g of solid sodium
carbonate and add 15 mL of distilled water to it. Stir and boil the content for about
10 minutes. Cool, filter and collect the filtrate in a test tube and label it as sodium
carbonate extract.
Confirmatory tests for acid radicals, which react with dilute sulphuric acid
are given below in Table 7.2.
2
Table 7.2 : Confirmatory tests for CO3 , S , SO3 , NO3 , CH3COO

Confirmatory test
Anion
2
Carbonate ( CO3 )
Take 0.1 g of salt in a test tube, add dilute sulphuric acid.

CO2 gas is evolved with brisk effervescence which turns lime
water milky. On passing the gas for some more time, milkiness
disappears.
Take 1 mL of water extract and make it alkaline by adding
ammonium hydroxide or sodium carbonate extract. Add a drop of
sodium nitroprusside solution. Purple or violet colouration appears.
Sulphide (S )
*Sulphite ( SO3 )
(a)
(b)
Nitrite ( NO 2 )
(a)
(b)
Take 1 mL of water extract or sodium carbonate

extract in a test tube and add barium chloride
solution. A white precipitate is formed which dissolves
in dilute hydrochloric acid and sulphur dioxide gas
is also evolved.
Take the precipitate of step (a) in a test tube and add
a few drops of potassium permanganate solution
acidified with dil. H 2 SO 4 . Colour of potassium
permanganate solution gets discharged.
Take 1 mL of water extract in a test tube. Add a few
drops of potassium iodide solution and a few drops of
starch solution, acidify with acetic acid. Blue colour
appears.
Acidify 1 mL of water extract with acetic acid. Add
2-3 drops of sulphanilic acid solution followed by 2-3
drops of 1-naphthylamine reagent. Appearance of red
colour indicates the presence of nitrite ion.
Like CO2 sulphur dioxide also turns lime water milky. But CO2 is odourless gas and SO2 has a
characteristic smell.
82
(a)
Acetate (CH3COO )
(b)
**
Take 0.1 g of salt in a china dish. Add 1 mL of ethanol

and 0.2 mL conc. H 2SO 4 and heat. Fruity odour
confirms the presence of acetate ion.
Take 0.1 g of salt in a test tube, add 1-2 mL distilled
water, shake well filter if necessary. Add 1 to 2 mL
neutral** ferric chloride solution to the filtrate. Deep
red colour appears which disappears on boiling and
a brown-red precipitate is formed.
Prepareation of neutral Ferric Chloride : Add dilute NaOH solution to ferric chloride solution drop by drop with
shaking until a small but permanent precipitate of ferric hydroxide is obtained. Filter the precipitate and use
the filtrate for analysis.
Chemistry of Confirmatory Tests

2
1. Test for Carbonate ion [CO3 ]

If there is effervescence with the evolution of a colourless and odourless gas on
adding dil. H2SO4 to the solid salt, this indicates the presence of carbonate ion.
The gas turns lime water milky due to the formation of CaCO3 (Fig. 7.1)
Na2CO3 + H2SO4 Na2SO4 + H2O +CO2
Ca(OH)2 + CO2 CaCO3 + H2O
If CO2 gas is passed in excess through lime water, the milkiness produced
disappears due to the formation of calcium hydrogen carbonate which is soluble
in water.
CaCO3 + CO2 + H2O Ca (HCO3)2
Hydrogen
sulphide
2. Test for Sulphide ion [S ]

(a)
(b)
With warm dilute H2SO4 a sulphide gives hydrogen sulphide gas which
smells like rotten eggs. A piece of filter paper dipped in lead acetate
solution turns black on exposure to the gas due to the formation of
lead sulphide which is black in colour.
Na2S + H2SO4
Na2SO4 + H2S
(CH3COO)2Pb + H2S
PbS
+
Lead sulphide
Black precipitate
2CH3COOH
If the salt is soluble in water, take the solution of salt in water make it
alkaline with ammonium hydroxide and add sodium nitroprusside
solution. If it is insoluble in water take sodium carbonate extract and
add a few drops of sodium nitroprusside solution. Purple or violet
83
colouration due to the formation of complex compound Na4[Fe(CN)5NOS]

confirms the presence of sulphide ion in the salt.
Na2S +
Na2 [Fe(CN)5NO] Na4 [Fe(CN)5NOS]

Sodium nitroprusside Complex of Purple colour
2
3. Test for Sulphite ion [SO3 ]

(a)
On treating sulphite with warm dil. H2SO4, SO2 gas is evolved which is
suffocating with the smell of burning sulphur.
Na2SO3 + H2SO4 Na2SO4 + H2O + SO2
The gas turns potassium dichromate paper acidified with dil. H2SO4, green.
Barium
compounds
Potassium
permanganate
K2Cr2O7 + H2SO4 + 3SO2
(b)
K2SO4
Cr2 (SO4)3 + H2O

Chromium
sulphate (green)
An aqueous solution or sodium carbonate extract of the salt produces a

white precipitate of barium sulphite on addition of barium chloride solution.
Na2SO3 + BaCl2 2NaCl + BaSO3
(i)
This precipitate gives following tests.

This precipitate on treatment with dilute HCl, dissolves due to
decomposition of sulphite by dilute HCl. Evolved SO2 gas can be tested.
BaSO3 + 2HCl BaCl2 + H2O + SO2
(ii)
Precipitate of sulphite decolourises acidified potassium permanganate

solution.
BaSO3 + H2SO4 BaSO4 + H2O + SO2
2KMnO4 + 3H2SO4 K2SO4 + 2MnSO4 + 3H2O + 5 [O]
SO2 + H2O + [O] H2SO4
4. Test for Nitrite ion [NO2 ]

(a)
On treating a solid nitrite with dil. H2SO4 and warming , reddish brown
fumes of NO2 gas are evolved. Addition of potassium iodide solution to
the salt solution followed by freshly prepared starch solution and
acidification with acetic acid produces blue colour. Alternatively, a filter
paper moistened with potassium iodide and starch solution and a few
drops of acetic acid turns blue on exposure to the gas due to the
interaction of liberated iodine with starch.
(i)
2NaNO2 + H2SO4 Na2SO4 + 2HNO2

3HNO2 HNO3 + 2NO + H2O
2NO + O2 2NO2
Brown gas
84
(ii)
NO2 + CH3COOH HNO2 + CH3COO
2HNO2 + 2KI + 2CH3COOH 2CH3 COOK + 2H2O + 2NO + I2

I2 + Starch Blue complex
(b)
Sulphanilic acid 1-naphthylamine reagent test (Griss-Ilosvay test)

On adding sulphanilic acid and 1-naphthylamine reagent to the water
extract or acidified with acetic acid, sulphanilic acid is diazotised in the
reaction by nitrous acid formed. Diazotised acid couples with
1-naphthylamine to form a red azo-dye.
NO2 + CH3COOH HNO2 + CH3COO
The test solution should be very dilute. In concentrated solutions

reaction does not proceed beyond diazotisation.
5. Test for Acetate ion [CH3COO ]

(a)
If the salt smells like vinegar on treatment with dil. H2SO4, this indicates
the presence of acetate ions. Take 0.1 g of salt in a china dish and add
1 mL of ethanol. Then add about 0.2 mL of conc. H2SO4 and heat. Fruity
odour of ethyl acetate indicates the presence of CH3COO ion.

2 CH3COONa + H2SO4 Na2SO4 + 2 CH3COOH
H
CH3COOH + C2H5OH CH3COOC2H5 + H2O

Ethylacetate
(Fruity odour)
85
(b)
Acetate gives deep red colour on reaction with neutral ferric chloride
solution due to the formation of complex ion which decomposes on
heating to give Iron (III) dihydroxyacetate as brown red precipitate.
3+
6 CH3COO + 3Fe + 2H2O [Fe3(OH)2 (CH3COO)6] + 2H

+
[Fe3(OH)2 (CH3COO)6] + 4H2O 3[Fe (OH)2 (CH3COO)] + 3CH3COOH + H

Iron(III)dihydroxyacetate
(Brown-red precipitate)
Step-II : Preliminary Test with Concentrated Suphuric Acid

If no positive result is obtained from dil. H2 SO4 test, take 0.1 g of salt in a test
tube and 3-4 drops of conc. H2SO4. Observe the change in the reaction mixture
in cold and then warm it. Identify the gas evolved on heating (see Table 7.3).
Table 7.3 : Preliminary examination with concentrated sulphuric acid
Inference
Observations
Gas/vapours evolved
Possible anions
A colourless gas with pungent smell,

which gives dense white fumes when a
rod dipped in ammonium hydroxide is
brought near the mouth of the test tube.
HCl
Chloride, (Cl )
Reddish brown gas with a pungent

odour is evolved. Intensity of reddish gas
increases on heating the reaction
mixture after addition of solid MnO2 to
the reaction mixture. Solution also
acquires red colour.
Br2 vapours
Bromide, (Br )
I2 vapours
Iodide, (I )
Brown fumes evolve which become dense

upon heating the reaction mixture after
addition of copper turnings and the
solution acquires blue colour.
NO2
Nitrate, ( NO 3 )
Colourless, odourless gas is evolved

which turns lime water milky and the
gas coming out of lime water burns with
a blue flame, if ignited.
CO and CO2
Oxalate, ( C2 O 4 )
Violet vapours, which turn starch paper

blue and a layer of violet sublimate is
formed on the sides of the tube. Fumes
become dense on adding MnO2 to the
reaction mixture.
86
Confirmatory tests for the anions which react with concentrated sulphuric
acid are given in Table 7.4.
Table 7.4 : Confirmatory tests for Cl , Br , I , NO3 and C2O4

Confirmatory test
Anion
Chloride (Cl )
(a)
(b)
(c)
Bromide (Br )
(a)
(b)
(c )
Iodide ( I )
(a)
(b)
Take 0.1 g of salt in a test tube, add a pinch of

manganese dioxide and 3-4 drops of conc. sulphuric
acid. Heat the reaction mixture. Greenish yellow
chlorine gas is evolved which is detected by its pungent
odour and bleaching action.
Take 1 mL of sodium carbonate extract in a test tube,
acidfy it with dil. HNO3 or take water extract and add silver
nitrate solution. A curdy white precipitate is obtained
which is soluble in ammonium hydroxide solution.
Take 0.1 g salt and a pinch of solid potassium
dichromate in a test tube, add conc. H2SO4, heat and
pass the gas evolved through sodium hydroxide
solution. It becomes yellow. Divide the solution into
two parts. Acidify one part with acetic acid and add
lead acetate solution. A yellow precipitate is formed.
Acidify the second part with dilute sulphuric acid and
add 1 mL of amyl alcohol followed by 1 mL of 10%
hydrogen peroxide. After gentle shaking the organic
layer turns blue.
Take 0.1 g of salt and a pinch of MnO2 in a test tube.
Add 3-4 drops conc.sulphuric acid and heat. Intense
brown fumes are evolved.
Neutralise 1 mL of sodium carbonate extract with
hydrochloric acid (or take the water extract). Add 1
mL carbon tetrachloride (CCl4)/chloroform (CHCl3)/
carbon disulphide. Now add an excess of chlorine
water dropwise and shake the test tube. A brown
colouration in the organic layer confirms the presence
of bromide ion.
Acidify 1 mL of sodium carbonate extract with dil.
HNO3 (or take 1 mL water extract) and add silver
nitrate solution. A pale yellow precipitate soluble with
difficulty in ammonium hydroxide solution is obtained.
Take 1 mL of salt solution neutralised with HCl and
add 1 mL chloroform/carbon tetrachloride/carbon
disulphide. Now add an excess of chlorine water drop
wise and shake the test tube. A violet colour appears
in the organic layer.
Take 1 mL of sodium carbonate extract acidify it with
dil. HNO3 (or take water extract). Add, silver nitrate
solution. A yellow precipitate insoluble in NH 4OH
solution is obtained.
87
*Nitrate ( NO 3 )
Oxalate ( C2 O 4 )
Take 1 mL of salt solution in water in a test tube. Add 2 mL

conc. of H2SO4 and mix thoroughly. Cool the mixture under
the tap. Add freshly prepared ferrous sulphate along the
sides of the test tube without shaking. A dark brown ring is
formed at the junction of the two solutions.
(a)
(b)
Take 1 mL of water extract or sodium carbonate

extract acidified with acetic acid and add calcium
chloride solution. A white precipitate insoluble in
ammonium oxalate and oxalic acid solution but
soluble in dilute hydrochloric acid and dilute nitric
acid is formed.
Take the precipitate from test (a) and dissolve it in
dilute H2SO4. Add very dilute solution of KMnO4 and
warm. Colour of KMnO4 solution is discharged. Pass
the gas coming out through lime water. The lime water
turns milky.
1. Test for Chloride ion [Cl ]

(a)
Manganese
dioxide
Silver nitrate
(b)
(c)
If on treatment with warm conc. H2SO4 the salt gives a colourless gas
with pungent smell or and if the gas which gives dense white fumes
with ammonia solution, then the salt may contain Cl ions and the
following reaction occurs.
NaCl + H2SO4
NaHSO4
+
HCl
Sodium
Hydrogen chloride
hydrogen sulphate Colourless gas
HCl + NH3
NH4Cl
Ammonium chloride
White fumes
If a salt gives effervescence on heating with conc. H2SO4 and MnO2 and
a light greenish yellow pungent gas is evolved, this indicates the presence
of Cl ions.
MnO2 + 2NaCl + 2H2SO4 Na2SO4 + MnSO4 + 2H2O + Cl2
Salt solution acidified with dilute HNO3 on addition of silver nitrate
solution gives a curdy white precipitate soluble in ammonium hydroxide
solution. This indicates the presence of Cl ions in the salt.

NaCl + AgNO3
AgCl + 2NH4OH
NaNO3
Ag Cl
Silver chloride
(White precipitate)
[Ag(NH3)2 ]Cl
Diammine silver (I)
chloride
+ 2H2O
* This test can also be performed by adding first ferrous sulphate solution and then conc. H2SO4 .
88
(d)
Mix a little amount of salt and an equal amount of solid potassium

dichromate (K2Cr2O7) in a test tube and add conc. H2SO4 to it. Heat the
test tube and pass the evolved gas through sodium hydroxide solution.
If a yellow solution is obtained, divide the solution into two parts. Acidify
the first part with acetic acid and then add lead acetate solution.
Formation of a yellow precipitate of lead chromate confirms the presence
of chloride ions in the salt. This test is called chromyl chloride test.*
4NaCl + K2Cr2O7 + 6H2SO4 2KHSO4 + 2CrO2Cl2 + 4NaHSO4 + 3H2O
(Chromyl
chloride)
Chromyl
chloride
CrO2Cl2 + 4NaOH Na2CrO4 + 2NaCl + 2H2O

(CH3COO)2Pb + Na2CrO4
Sodium
chromate
Lead
chromate
PbCrO4
+ 2CH3COONa
Lead chromate
(Yellow precipitate)
Acidify the second part with dilute sulphuric acid and add small amounts of
amyl alcohol and then 1 mL of 10% hydrogen peroxide solution. On gentle shaking
2
organic layer turns blue. CrO4 ion formed in the reaction of chromyl chloride
with sodium hydroxide reacts with hydrogen peroxide to form chromium pentoxide
(CrO5) (See structure) which dissolves in amyl alcohol to give blue colour.
2
CrO4 + 2H + 2H2O2
Cr O5
+ 3H2O
Chromium
pentoxide
2. Test for Bromide ion (Br )

If on heating the salt with conc. H2SO4 reddish brown fumes of bromine are
evolved in excess, this indicates the presence of Br ions. The fumes get intensified
on addition of MnO2. Bromine vapours turn starch paper yellow.
2NaBr + 2H2SO4 Br2 + SO2 + Na2SO4 + 2H2O
2NaBr + MnO2 + 2H2SO4 Na2SO4 + MnSO4 + 2H2O + Br2
(a)
Bromine
very toxic by
inhalation
corrosive
Add 1 mL of carbon tetrachloride (CCl4)/chloroform (CHCl3)** and excess

of freshly prepared chlorine water dropwise to the salt solution in water
or sodium carbonate extract neutralised with dilute HCl. Shake the test
tube vigorously. The appearance of an orange brown colouration in the
organic layer due to the dissolution of bromine in it, confirms the
presence of bromide ions.
2NaBr + Cl2 2NaCl + Br2
*
**
3+
Chromyl chloride test should be performed with minimum amount of substance to avoid pollution by Cr ions.
In place of carbon tetrachloride or chloroform, carbon disulphide or dichloromethane (CH2Cl2) can also be used.
89
(b)
Acidify the sodium carbonate extract of the salt with dil. HNO3. Add
silver nitrate (AgNO3) solution and shake the test tube. A pale yellow
precipitate is obtained which dissolves in ammonium hydroxide with
difficulty.
NaBr + AgNO3
NaNO3
+ AgBr
Silver bromide
Pale yellow precipitate
3. Test for Iodide ion ( I )

(a)
Iodine,
harmful by
inhalation
and contact
with skin
If on heating the salt with conc. H2SO4 , deep violet vapours with a
pungent smell are evolved. These turns starch paper blue and a violet
sublimate is formed on the sides of the test tube, it indicates the presence
of I ions. Some HI, sulphur dioxide, hydrogen sulphide, and sulphur

are also formed due to the following reactions.
2NaI + 2H2SO4 Na2SO4 + SO2 + 2H2O + I2
I2 + Starch Blue colour
solution
NaI + H2SO4 NaHSO4 + HI
Chlorine,
toxic by
inhalation
2HI + H2SO4 2H2O + I2 + SO2

6NaI + 4H2SO4 3I2 + 4H2O +S + 3Na2SO4
Chloroform,
harmful and
toxic by
inhalation
8NaI + 5 H2SO4 4I2 + H2S + 4Na2SO4 + 4H2O

On adding MnO2 to the reaction mixture, the violet vapours become
dense.
2NaI + MnO2 + 2H2SO4 I2 + MnSO4 + Na2SO4 + 2H2O
(b)
Add 1 mL of CHCl3 or CCl4 and chlorine water in excess to the salt

solution in water or sodium carbonate extract neutralised with dil.HCl
and shake the test tube vigorously. Presence of violet colouration in the
organic layer confirms the presence of iodide ions.
2NaI + Cl2 2NaCl + I2
Iodine dissolves in the organic solvent and the solution becomes violet.
(c)
Acidify sodium carbonate extract of the salt with dil.HNO3 and add
AgNO3 solution. Appearance of a yellow precipitate insoluble in excess
of NH4OH confirms the presence of iodide ions.
NaI + AgNO3
AgI
+
silver iodide
90
NaNO3
4. Test for Nitrate ion [ NO3 ]

(a)
If on heating the salt with conc. H2SO4 light brown fumes are evolved
then heat a small quantity of the given salt with few copper turnings or
chips and conc. H2SO4. Evolution of excess of brown fumes indicates
the presence of nitrate ions. The solution turns blue due to the formation
of copper sulphate.
NaNO3 + H2SO4
NaHSO4 + HNO3
Copper
sulphate
4HNO3 4NO2 + O2 + 2H2O

2NaNO3 + 4H2SO4 + 3Cu
3 CuSO4 + Na2SO4 + 4H2O + 2NO

Copper sulphate
(Blue)
Nitric
acid
2NO + O2
2NO2
(Brown fumes)
(b)
Take 1 mL of an aqueous solution of the salt and add 2 mL conc. H2SO4

slowly. Mix the solutions thoroughly and cool the test tube under the
tap. Now, add freshly prepared ferrous sulphate solution along the sides
of the test tube dropwise so that it forms a layer on the top of the liquid
already present in the test tube. A dark brown ring is formed at the
junction of the two solutions due to the formation of nitroso ferrous
sulphate (Fig. 7.2). Alternatively first ferrous sulphate is added and
then concentrated sulphuric acid is added.
Oxalates
Fig. 7.2 : Formation of brown ring
NaNO3 + H2SO4 Na HSO4 + HNO3

6 FeSO4 + 3H2SO4 + 2HNO3 3Fe2 (SO4)3 + 4H2O + 2NO
[Fe(NO)]SO4
FeSO4 + NO
Nitroso ferrous sulphate
(Brown)
2
5. Test for Oxalate ion [C2O4 ]

If carbon dioxide gas along with carbon monoxide gas is evolved in the
preliminary examination with concentrated sulphuric acid, this gives indication
about the presence of oxalate ion.
(COONa)2 + Conc. H2SO4 Na2SO4 + H2O + CO2 + CO
91
Oxalate is confirmed by the following tests:

(a)
Acidify sodium carbonate extract with acetic acid and add calcium chloride
solution. A white precipitate of calcium oxalate, insoluble in ammonium
oxalate and oxalic acid solution indicates the presence of oxalate ion.
CaCl2 + Na2C2O4
CaC2O4
+ 2NaCl
Calcium oxalate
(White precipitate)
(b)
KMnO4 test
Filter the precipitate from test (a). Add dil. H2SO4 to it followed by dilute
KMnO4 solution and warm. Pink colour of KMnO4 is discharged:
CaC2O4 + H2SO4
CaSO4
+ H2C2O4
Calcium sulphate
Oxalic acid
2 KMnO4 + 3H2SO4 + 5H2C2O4 2MnSO4 + K2SO4 + 8H2O + 10CO2

Pass the gas evolved through lime water. A white precipitate is formed
which dissolves on passing the gas for some more time.
Step-III : Test for Sulphate and Phosphate

If no positive test is obtained in Steps-I and II, then tests for the presence of
sulphate and phosphate ions are performed. These tests are summarised in
Table 7.5.
Table 7.5 : Confirmatory tests for Sulphate and Phosphate
Confirmatory Test
Ion
2
Sulphate ( SO 4 )
(a)
(b)
Take 1 mL water extract of the salt in water or sodium

carbonate and after acidifying with dilute
hydrochloric acid add BaCl 2 solution. White
precipitate insoluble in conc. HCl or conc. HNO3 is
obtained.
Acidify the aqueous solution or sodium carbonate
extract with acetic acid and add lead acetate solution.
Appearance of white precipitate confirms the presence
2
of SO 4 ion.
3
Phosphate ( PO4 )
92
(a)
Acidify sodium carbonate extract or the solution of

the salt in water with conc. HNO3 and add ammonium
molybdate solution and heat to boiling. A canary
yellow precipitate is formed.

2
1. Test of Sulphate ions [SO4 ]

(a)
Aqueous solution or sodium carbonate extract of the salt acidified with

acetic acid on addition of barium chloride gives a white precipitate of
barium sulphate insoluble in conc. HCl or conc. HNO3 .
BaSO4
+
Na2SO4 + BaCl2
Barium sulphate
(White precipitate)
(b)
2NaCl
Sulphate ions give white precipitate of lead sulphate when aqueous

solution or sodium carbonate extract neutralised with acetic acid is
treated with lead acetate solution.
Na2SO4 + (CH3COO)2Pb
PbSO4
+ 2CH3COONa
Lead sulphate
(White precipitate)
2. Test for Phosphate ion [PO4 ]

(a)
Add conc. HNO3 and ammonium molybdate solution to the test solution
containing phosphate ions and boil. A yellow colouration in solution
or a canary yellow precipitate of ammonium-phosphomolybdate,
(NH4)3[P (Mo3O10)4] is formed. Each oxygen of phosphate has been
replaced by Mo3O10 group.
Na2HPO4 + 12 (NH4)2 MoO4 + 23 HNO3 (NH4)3[P (Mo3O10)4] + 2NaNO3 + 21NH4NO3 + 12H2O

Canary yellow
precipitate
SYSTEMATIC ANALYSIS OF CATIONS

The tests for cations may be carried out according to the following scheme.
Step - I : Preliminary Examination of the Salt for Identification of Cation

1. Colour Test
Observe the colour of the salt carefully, which may provide useful information
about the cations. Table 7.6 gives the characteristic colours of the salts of some
cations.
93
Table 7.6 : Characteristic colours of some metal ions

Colour
Cations Indicated
Fe2+, Fe3+
Cu2+
Ni2+
Co2+
Mn2+
Light green, Yellow, Brown

Blue
Bright green
Blue, Red, Violet, Pink
Light pink
2. Dry Heating Test

(i)
(ii)
Take about 0.1 g of the dry salt in a clean and dry test tube.
Heat the above test tube for about one minute and observe the colour of
the residue when it is hot and also when it becomes cold. Observation of
changes gives indications about the presence of cations, which may not be
taken as conclusive evidence (see Table 7.7).
Table 7.7 : Inferences from the colour of the salt in cold and on heating
Colour when cold
Colour when hot
Inference
Blue
White
Cu2+
Green
Dirty white or yellow
Fe2+
White
Yellow
Zn2+
Pink
Blue
Co2+
3. Flame Test
The chlorides of several metals impart characteristic colour to the flame because
they are volatile in non-luminous flame. This test is performed with the help of a
platinum wire as follows :
(i) Make a tiny loop at one end of a platinum wire.
(ii) To clean the loop dip it into concentrated hydrochloric acid and hold it in a
non-luminous flame (Fig. 7.3).
(iii) Repeat step (ii) until the wire imparts no colour to the flame.
(iv) Put 2-3 drops of concentrated hydrochloric acid on a clean watch glass
and make a paste of a small quantity of the salt in it.
(v) Dip the clean loop of the platinum wire in this paste and introduce the loop
in the non-luminous (oxidising) flame (Fig. 7.3).
(vi) Observe the colour of the flame first with the naked eye and then through
a blue glass and identify the metal ion with the help of Table 7.8.
94
Fig.7.3 : Performing flame test
Table 7.8 : Inference from the flame test

Colour of the flame
observed by naked eye
Colour of the flame

observed through blue glass
Inference
Green flame with

blue centre
Same colour as observed

without glass
Cu2+
Crimson red
Purple
Sr2+
Apple green
Bluish green
Ba2+
Brick red
Green
Ca2+
4. Borax Bead Test

This test is employed only for coloured salts because borax reacts
with metal salts to form metal borates or metals, which have
characteristic colours.
(i) To perform this test make a loop at the end of the platinum
wire and heat it in a flame till it is red hot.
(b)
(a)
(ii) Dip the hot loop into borax powder and heat it again until
borax forms a colourless transparent bead on the loop. Fig. 7.4 : Borax bead test
Before dipping the borax bead in the test salt or mixture,
(a) Heating in reducing
flame (b) Heating in
confirm that the bead is transparent and colourless. If it
oxidising flame
is coloured this means that, the platinum wire is not clean.
Then make a fresh bead after cleaning the wire.
(iii) Dip the bead in a small quantity of the dry salt and again hold it in the flame.
(iv) Observe the colour imparted to the bead in the non - luminous flame as well
as in the luminous flame while it is hot and when it is cold (Fig. 7.4).
(v) To remove the bead from the platinum wire, heat it to redness and tap the
platinum wire with your finger. (Fig. 7.5).
95
On heating, borax loses its water of crystallisation and decomposes to give

sodium metaborate and boric anhydride.
Na2B4O7 .10H2O Na2B4O7 + 10H2O
Borax
Na2B4O7
2NaBO2
+
B 2 O3
Sodium metaborate Boric anhydride
On treatment with metal salt, boric anhydride forms metaborate of the metal
which gives different colours in oxidising and reducing flame. For example, in
the case of copper sulphate, following reactions occur.
CuSO4 + B2O3
Non-luminous flame
Cu(BO2)2 +
Cupric metaborate
Blue-green
SO3
Two reactions may take place in the reducing flame:

(i) The blue Cu (BO2)2 is reduced to colourless cuprous metaborate as follows:
Luminous flame
2Cu(BO2 )2 + 2NaBO2 + C
2CuBO 2 + Na 2 B4 O7 + CO
or (ii) Cupric metaborate may be reduced to metallic copper and the bead appears
red and opaque.
2Cu(BO2 )2 + 4NaBO2 + 2C
Luminous flame
2Cu + 2Na 2 B4 O7 + 2CO
The preliminary identification of metal ion can be made from Table 7.9.
Fig. 7.5 : Removing borax bead
Table 7.9 : Inference from the borax bead test

Heating in oxidising
(non-luminous) flame
Colour of the salt bead
96
Heating in reducing
(luminous) flame
Colour of the salt bead
Inference
In cold
In hot
In cold
In hot
Blue
Green
Red opaque
Colourless
Cu2+
Reddish brown
Violet
Grey
Grey
Ni2+
Light violet
Light violet
Colourless
Colourless
Mn2+
Yellow
Yellowish brown
Green
Green
Fe3+
5. Charcoal Cavity Test

Metallic carbonate when heated in a charcoal cavity decomposes to give
corresponding oxide. The oxide appears as a coloured residue in the cavity.
Sometimes oxide may be reduced to metal by the carbon of the charcoal cavity.
The test may be performed as follows:
(i) Make a small cavity in a charcoal block with the help of a charcoal borer.
Do not apply pressure otherwise it will crack [Fig.7.6 (a)].
(ii) Fill the cavity with about 0.2 g of the salt and about 0.5 g of anhydrous
sodium carbonate.
(b)
(a)
Fig. 7.6 : (a) Making charcoal cavity (b) Heating salt in the cavity
(iii)
(iv)
(v)
Moisten the salt in the cavity with one or two drops of water, otherwise
salt/mixture will blow away.
Use a blowpipe to heat the salt in a luminous (reducing) flame and
observe the colour of oxide/ metallic bead formed in the cavity both
when hot and cold [ Fig. (7.6 b)]. Obtain oxidising and reducing flame as
shown in Fig. 7.7 a and b.
Always bore a fresh cavity for testing the new salt.
(a)
Note : To obtain oxidising flame

hold the nozzle of the
blowpipe about one third
within the flame.
To obtain reducing flame
place nozzle of the
blowpipe just outside the
flame.
(b)
Fig. 7.7 : Obtaining oxidising and reducing flame (a) Oxidising flame (b) Reducing flame
97
When test is performed with CuSO4, the following change occurs.

CuSO4 + Na 2 CO3
Heat
CuCO3
CuO + C
Heat
CuCO3 + Na 2 SO4
CuO + CO2
Heat
Cu
+ CO
Red colour
In case of ZnSO4 :
ZnSO4 + Na 2 CO3
ZnCO3
Heat
Heat
ZnCO3 + Na 2 SO4
ZnO
CO2
Yellow when hot,

White when cold
The metal ion can be inferred from Table 7.10.
Table 7.10 : Inference from the charcoal cavity test
Observations
Inference
Yellow residue when hot and grey metal when cold
Pb2+
White residue with the odour of garlic
As3+
Brown residue
Cd2+
Yellow residue when hot and white when cold
Zn2+
6. Cobalt Nitrate Test

If the residue in the charcoal cavity is white, cobalt nitrate test is performed.
(i) Treat the residue with two or three drops of cobalt nitrate solution.
(ii) Heat it strongly in non-luminous flame with the help of a blow pipe and
observe the colour of the residue.
On heating, cobalt nitrate decomposes into cobalt (II) oxide, which gives a
characteristic colour with metal oxide present in the cavity.
Thus, with ZnO, Al2O3 and MgO, the following reactions occur.
2 Co(NO3 )2
Heat
2CoO + 4NO2 + O2
CoO + ZnO CoO.ZnO

Green
CoO + MgO CoO. MgO
Pink
CoO + Al2O3 CoO. Al2O3
Blue
98
Step-II : Wet Tests for Identification of Cations

The cations indicated by the preliminary tests given above are confirmed by
systematic analysis given below.
The first essential step is to prepare a clear and transparent solution of the
salt. This is called original solution. It is prepared as follows:
Preparation of Original Solution (O.S.)
To prepare the original solution, following steps are followed one after the other
in a systematic order. In case the salt does not dissolve in a particular solvent
even on heating, try the next solvent.
The following solvents are tried:
1. Take a little amount of the salt in a clean boiling tube and add a few mL of
distilled water and shake it. If the salt does not dissolved, heat the content
of the boiling tube till the salt completely dissolves.
2. If the salt is insoluble in water as detailed above, take fresh salt in a clean
boiling tube and add a few mL of dil.HCl to it. If the salt is insoluble in
cold, heat the boiling tube till the salt is completely dissolved.
3. If the salt does not dissolve either in water or in dilute HCl even on heating,
try to dissolve it in a few mL of conc. HCl by heating.
4. If salt does not dissolve in conc. HCl, then dissolve it in dilute nitric acid.
5. If salt does not dissolve even in nitric acid then a mixture of conc. HCl and
conc. HNO3 in the ratio 3:1 is tried. This mixture is called aqua regia. A salt
not soluble in aqua regia is considered to be an insoluble salt.
Group Analysis
(I) Analysis of Zero group cation (NH4+ ion)
(a)
(b)
Take 0.1 g of salt in a test tube and add 1-2 mL of NaOH solution to
it and heat. If there is a smell of ammonia, this indicates the presence
of ammonium ions. Bring a glass rod dipped in hydrochloric acid
near the mouth of the test tube. White fumes are observed.
Pass the gas through Nesslers reagent. Brown precipitate is obtained.
+
Chemistry of Confirmatory Tests for NH4 ion

(a)
Ammonia gas evolved by the action of sodium hydroxide on ammonium

salts reacts with hydrochloric acid to give ammonium chloride, which is
visible as dense white fume.
(NH4)2 SO4 + 2NaOH Na2SO4 + 2NH3 + 2H2O
NH3 + HCl NH4Cl
99
On passing the gas through Nesslers reagent, a brown colouration or a

precipitate of basic mercury(II) amido-iodine is formed.
2K2HgI4 + NH3 + 3KOH
Mercury
Salts
HgO.Hg(NH2)I
+
Basic mercury (II)
amido-iodine
(Brown precipitate)
7KI + 2H2O
For the analysis of cations belonging to groups I-VI, the cations are precipitated
from the original solution by using the group reagents (see Table 7.11) according to
the scheme shown in the flow chart given below:
The separation of all the six groups is represented as below:
Flow Chart*
Original Solution
Dil.HCl
If no precipitate is formed
Precipitate, Group I
Pass H2S gas
2+
(Pb ) as chloride
Precipitate, Group II
(Pb2+, Cu2+, As3+)
as sulphides
If no precipitate, take original solution

Heat (O.S.) with conc. HNO3,
cool and add solid NH4Cl + NH4OH
solution in excess
If no precipitate
Precipitate, Group III

(Fe3+, Al3+) as hydroxides
Precipitate, Group IV
Pass H2S
If no precipitate, take original solution
(Co2+, Ni2+, Mn2+, Zn2+)

as sulphides
Precipitate, Group V
(Ba2+, Sr2+, Ca2+)
as carbonates
Add NH4OH and

solid (NH4)2 CO3
If no precipitate, take original

solution to test Group VI,
* This flow chart is for the detection of one cation only.

For detection of more than one cation modification will be required.
100
Mg 2+
Table 7.11 : Group reagents for precipitating ions

Group
Cations*
Group zero
NH4
Group Reagent
None
2+
Group-I
Dilute HCl
Pb
2+
2+
3+
Pb , Cu , As
Group-II
3+
H2S gas in presence of dil. HCl
3+
Group-III
Al , Fe
Group-IV
2+
2+
2+
NH4OH in presence of NH4Cl
2+
2+
2+
2+
Co , Ni , Mn , Zn
Group-V
Ba , Sr , Ca
Group-VI
Mg
H2S in presence of NH4OH

(NH4)2CO3 in presence of NH4OH
2+
None
(II) Analysis of Group-I cations

Take a small amount of original solution ( if prepared in hot conc. HCl) in a test
tube and add cold water to it and cool the test tube under tap water. If a white
precipitate appears, this indicates the presence of Pb2+ ions in group I. On the
other hand, if the original solution is prepared in water and on addition of dil.
HCl, a white precipitate appears, this may also be Pb2+. Confirmatory tests are
described below in Table 7.12.
2+
Table 7.12 : Confirmatory tests for Group-I cation (Pb )

Experiment
Observation
Dissolve the precipitate in hot water and divide

the hot solution into three parts.
1.
Add potassium iodide solution to the first
part.
A yellow precipitate is obtained.
2.
To the second part add potassium chromate

solution.
A yellow precipitate is obtained which

is soluble in NaOH and insoluble in
ammonium acetate solution.
3.
To the third part of the hot solution add few

drops of alcohol and dilute sulphuric acid.
A white precipitate is obtained

which is soluble in ammonium
acetate solution.
2+
Chemistry of the Confirmatory Tests of Pb
ions
Lead is precipitated as lead chloride in the first group. The precipitate is soluble
in hot water.
1. On adding potassium iodide (KI) solution, a yellow precipitate of lead
2+
iodide is obtained which confirms the presence of Pb ions.
PbCl2
+
(Hot solution)
2KI
PbI2
+ 2KCl
Yellow precipitate
* Here only those cations are given which are in the syllabus.
101
2.
This yellow precipitate (PbI2) is soluble in boiling water and reappears

on cooling as shining crystals.
On addition of potassium chromate (K2CrO4) solution a yellow precipitate
of lead chromate is obtained. This confirms the presence of Pb2+ ions.
+ K2CrO4
PbCrO4
+ 2KCl
PbCl2
(Hot solution)
Lead chromate
The yellow precipitate (PbCrO4) is soluble in hot NaOH solution.
PbCrO4 + 4NaOH U
Na2[Pb(OH)4]
Na2CrO4
Sodium tetra
hydroxoplumbate (II)
3.
Hydrogen
sulphide
A white precipitate of lead sulphate (PbSO4) is formed on addition of

alcohol followed by dil. H2SO4.
PbSO4
+ 2 HCl
PbCl2 + H2SO4
Lead sulphate
(White precipitate)
Lead sulphate is soluble in ammonium acetate solution due to the formation
of tetraacetoplumbate(II) ions. This reaction may be promoted by addition of few
drops of acetic acid.
PbSO4 + 4 CH3COONH4 (NH4)2 [Pb(CH3COO)4] + (NH4)2SO4
Ammonium
tetraacetoplumbate(II)
(III) Analysis of GroupII cations
If group-I is absent, add excess of water to the same test tube. Warm the solution
and pass H2S gas for 1-2 minutes (Fig. 7.6). Shake the test tube. If a precipitate
appears, this indicates the presence of group-II cations. Pass more H2S gas
through the solution to ensure complete
precipitation and separate the precipitate.
If the colour of the precipitate is black, it
2+
2+
indicates the presence of Cu or Pb ions.
If it is yellow in colour, then presence of
3+
As ions is indicated.
Take the precipitate of group-II in a
test tube and add excess of yellow
ammonium sulphide solution to it. Shake
the test tube. If the precipitate is insoluble,
group II-A (copper group) is present. If
the precipitate is soluble, this indicates the
presence of group-II B (arsenic group).
Confirmatory tests for the groups II A
and II B are given in Table 7.13.
Fig. 7.8 : Kipps apparatus for preparation of H2S gas
102
Table 7.13 : Confirmatory tests for Group-II A and II B cations

Black precipitate of Group II A ions (Pb , Cu )
insoluble in yellow ammonium sulphide is formed.
2+
2+
If a yellow precipitate soluble in

yellow ammonium sulphide is
3+
formed then As ion is present.
Boil the precipitate of Group II A with dilute nitric

acid and add a few drops of alcohol and dil. H2SO4.
Acidify this solution with dilute

HCl. A yellow precipitate is formed.
Heat
the
precipitate
with
concentrated nitric acid and add
ammonium molybdate solution. A
canary yellow precipitate is formed.
White precipitate confirms

2+
the presence of Pb ions.
Dissolve the precipitate in
ammonium
acetate
solution. Acidify with
acetic acid and divide the
solution into two parts.
(i) To the first part add
potassium chromate
solution, a yellow
precipitate is formed.
(ii) To the second part,
add potassium iodide
solution, a yellow
If no precipitate is
formed, add excess of
ammonium hydroxide
solution. A blue solution
is obtained, acidify it
with acetic acid and add
potassium ferrocyanide
solution. A chocolate
brown precipitate is
formed.
Group-II A (Copper Group)

Alcohol
Chemistry of confirmatory tests of Group-II A cations

2+
1. Test for Lead ion (Pb )

Lead sulphide precipitate dissolves in dilute HNO3. On adding dil. H2SO4 and a
few drops of alcohol to this solution a white precipitate of lead sulphate appears.
This indicates the presence of lead ions.
3PbS + 8HNO3 3Pb (NO3)2 + 2NO + 4H2O + 3S
Pb(NO3)2 + H2SO4 PbSO4 + 2HNO3
The white precipitate dissolves in ammonium acetate solution on boiling.
When this solution is acidified with acetic acid and potassium chromate solution
is added, a yellow precipitate of PbCrO4 is formed. On adding potassium iodide
solution, a yellow precipitate of lead iodide is formed.
PbSO4 + 4CH3COONH4 (NH4)2[Pb (CH3COO)4] + (NH4)2SO4
(NH4)2 [Pb(CH3COO)4] + K2CrO4 PbCrO4 + 2CH3COOK + 2(NH4)2SO4
Ammonium
Yellow
tetraacetoplumbate(II)
precipitate
103
2. Test for Copper ion (Cu2+)

(a)
Copper sulphide dissolves in nitric acid due to the formation of copper

nitrate.
3CuS + 8HNO3 3Cu(NO3)2 + 2NO + 3S + 4H2O
On heating the reaction mixture for long time, sulphur is oxidised to
sulphate and copper sulphate is formed and the solution turns blue. A
small amount of NH4OH precipitates basic copper sulphate which is soluble
in excess of ammonium hydroxide due to the formation of
tetraamminecopper (II) complex.
S + 2HNO3 H2SO4 + 2NO
2Cu2++ SO 4 +2NH3+2H2O Cu(OH)2. CuSO4+ 2NH4
2
Cu(OH)2.CuSO4 + 8NH3 2 [Cu(NH3)4]SO4
+ 2OH + SO 4
Tetraamminecopper (II)
sulphate (Deep blue)
(b)
The blue solution on acidification with acetic acid and then adding
potassium ferrocyanide [K4Fe(CN)6 ] solution gives a chocolate colouration
due to the formation of copper ferrocyanide i.e.Cu2[Fe(CN)6].
[Cu(NH3)4] SO4 + 4CH3COOH CuSO4 + 4CH3COONH4
2CuSO4 + K4[Fe(CN)6]
Potassium
hexacyanoferrate (II)
Cu2[Fe(CN)6]
+ 2K2SO4
Copper
hexacyanoferrate (II)
(Chocolate brown precipitate)
Group-II B (Arsenic Group)

If group- II precipitate dissolves in yellow ammonium sulphide and the colour of
3+
the solution is yellow, this indicates the presence of As ions. Ammonium
thioarsenide formed on dissolution of As2S3 decomposes with dil. HCl, and a
yellow precipitate of arsenic (V) sulphide is formed which dissolves in concentrated
nitric acid on heating due to the formation of arsenic acid. On adding ammonium
molybdate solution to the reaction mixture and heating, a canary yellow
3+
precipitate is formed. This confirms the presence of As ions.
As2S3
+ 3 (NH4)2S2
2 (NH4)3As S4 + S
Yellow ammonium
sulphide
2(NH4)3AsS4+ 6HCl As2S5 + 3H2S + 6NH4Cl

3As2S5 + 10HNO3 + 4H2O 6H3AsO4 + 10NO + 15S
Arsenic acid
104
H3AsO4
Arsenic acid
+ 12(NH4)2 MoO4
Ammonium
molybdate
+ 21HNO3 (NH4)3[As (Mo3 O10)4] + 21NH4NO3 +12H2O

Ammonium
arsinomolybdate
(yellow precipitate)
(IV) Analysis of GroupIII cations

If group-II is absent, take original solution and add 2-3 drops of conc. HNO3 to
oxidise Fe2+ ions to Fe3+ ions. Heat the solution for a few minutes. After cooling
add a small amount of solid ammonium chloride (NH4Cl) and an excess of ammonium
hydroxide (NH4OH) solution till it smells of ammonia. Shake the test tube. If a brown
or white precipitate is formed, this indicates the presence of group-III cations.
Confirmatory tests of group-III cations are summarised in Table 7.14.
Observe the colour and the nature of the precipitate. A gelatinous white
3+
precipitate indicates the presence of aluminium ion (A1 ). If the precipitate is
3+
brown in colour, this indicates the presence of ferric ions (Fe ).
Table 7.14 : Confirmatory test for Group-III cations
White precipitate
3+
Al
Brown precipitate
3+
Fe
Dissolve the precipitate in dilute HCl
and divide the solution into two parts.
(a) To the first part add potassium
ferrocyanide solution [Potasium
hexacyanoferrate (II)]. A blue
precipitate/colouration appears.
(b) To the second part add potassium
thiocyanate solution. A blood red
colouration appears.
Dissolve the white precipitate in dilute

HCl and divide into two parts.
(a) To the first part add sodium hydroxide
solution and warm. A white
gelatinous precipitate soluble in
excess of sodium hydroxide solution.
(b) To the second part first add blue
litmus solution and then ammonium
hydroxide solution drop by drop along
the sides of the test tube. A blue
floating mass in the colourless
solution is obtained.
Chemistry of confirmatory tests of Group-III cations

When original solution is heated with concentrated nitric acid, ferrous ions are
oxidised to ferric ions.
2FeCl2 + 2HCl + [O] 2FeCl3 + H2O
Third group cations are precipitated as their hydroxides, which dissolve in
dilute hydrochloric acid due to the formation of corresponding chlorides.
3+
1. Test for Aluminium ions (A1 )

(a)
When the solution containing aluminium chloride is treated with sodium

hydroxide, a white gelatinous precipitate of aluminium hydroxide is formed
105
which is soluble in excess of sodium hydroxide solution due to the formation

of sodium aluminate.
AlCl3
+ 3NaOH Al(OH)3 + 3NaCl
+ NaOH NaAlO2 + 2H2O

Al(OH)3
White gelatinous
Sodium
precipitate
aluminate
(b)
In the second test when blue litmus is added to the solution, a red
colouration is obtained due to the acidic nature of the solution. On addition
of NH4OH solution drop by drop the solution becomes alkaline and
aluminium hydroxide is precipitated. Aluminium hydroxide adsorbs blue
colour from the solution and forms insoluble adsorption complex named
lake. Thus a blue mass floating in the colourless solution is obtained. The
test is therefore called lake test.
3+
2. Test for ferric ions (Fe )

Reddish brown precipitate of ferric hydroxide dissolves in hydrochloric acid and
ferric chloride is formed.
Fe(OH)3 + 3HCl FeCl3 + 3H2O
(a)
When the solution containing ferric chloride is treated with potassium

ferrocyanide solution a blue precipitate/colouration is obtained. The colour
of the precipitate is Prussian blue. It is ferric ferro-cyanide. The reaction
takes place as follows:
4FeCl3 + 3K4[Fe(CN)6] Fe4[Fe(CN)6]3 + 12KCl
Potassium
Prussian blue
ferrocyanide
precipitate
If potassium hexacyanoferrate (II) (i.e. potassium ferrocyanide) is added in
excess then a product of composition KFe[Fe(CN)6] is formed. This tends to
form a colloidal solution (soluble Prussian blue) and cannot be filtered.
FeCl3 + K4[Fe(CN)6]
(b)
KFe[Fe(CN)6]
+ 3KCl
(Soluble prussian blue)
To the second part of the solution, add potassium thiocyanate (potassium

sulphocyanide) solution. The appearance of a blood red colouration
3+
confirms the presence of Fe ions.
3+
2+
Fe + SCN [Fe(SCN)]
Blood red colour
(V) Analysis of group-IV cations
If group-III is absent, pass H2S gas in the solution of group-III for a few
minutes. If a precipitate appears (white, black or flesh coloured), this indicates
106
the presence of group-IV cations. Table 7.15 gives a summary of confirmatory

tests of group-IV cations.
Table 7.15 : Confirmatory test for Group-IV cations

White precipitate
2+
(Zn )
Dissolve the precipitate
in dilute HCl by boiling.
Divide the solution into
two parts.
(a) To the first part add
sodium hydroxide
solution. A white
precipitate soluble
in excess of sodium
hydroxide solution
confirms
the
2+
presence of Zn
ions.
Flesh coloured precipitate

2+
(Mn )
dilute HCl by boiling, then add
sodium hydroxide solution in
excess. A white precipitate is
formed which turns brown on
keeping.
(b) Neutralise
the
second part with
a m m o n i u m
hydroxide solution
and add potassium
ferrocyanide
solution. A bluish
white precipitate
appears.
Black precipitate
2+
2+
(Ni , Co )
aqua regia. Heat the
solution to dryness and
cool. Dissolve the residue
in water and divide the
solution into two parts.
(a) To the first part of the
solution add ammonium
hydroxide solution till it
becomes alkaline. Add
a few drops of dimethyl
glyoxime and shake the
test tube. Formation of
a bright red precipitate
confirms the presence
2+
of Ni ions.
(b) Neutralise the second
part with ammonium
hydroxide solution.
Acidify it with dilute
acetic acid and add
solid potassium nitrite.
A yellow precipitate
confirms the presence
2+
of Co ions.
Chemistry of confirmatory tests of GroupIV cations

Fourth group cations are precipitated as their sulphides. Observe the colour of
the precipitate. A white colour of the precipitate indicates the presence of zinc
ions, a flesh colour indicates the presence of manganese ions and a black colour
2+
2+
indicates the presence of Ni or Co ions.
2+
1. Test for Zinc ion (Zn )

Zinc sulphide dissolves in hydrochloric acid to form zinc chloride.
ZnS + 2HCl ZnCl2 + H2S
107
(a)
On addition of sodium hydroxide solution it gives a white precipitate of

zinc hydroxide, which is soluble in excess of NaOH solution on heating.
2+
This confirms the presence of Zn ions.
ZnCl2 + 2NaOH Zn(OH)2 + 2NaCl
Zn(OH)2 + 2NaOH
(b)
Na2ZnO2 +
Sodium zincate
2H2O
When potassium ferrocyanide K4Fe(CN)6 solution is added to the solution

after neutralisation by NH4OH solution, a white or a bluish white precipitate
of zinc ferrocyanide appears.
2 ZnCl2 + K4 [Fe(CN)6] Zn2 [Fe(CN)6] + 4 KCl
Zinc
ferrocyanide
2. Test for Manganese ion (Mn2+)

Manganese sulphide precipitate dissolves in dil. HCl on boiling. On addition of
NaOH solution in excess, a white precipitate of manganese hydroxide is formed
which turns brown due to atmospheric oxidation into hydrated manganese dioxide.
MnS + 2HCl Mn Cl2 + H2S
+ 2NaCl
MnCl2 + 2NaOH Mn(OH)2
(White precipitate)
Mn (OH)2 + [O]
MnO(OH)2
Hydrated manganese dioxide
(Brown colour)
2+
3. Test for Nickel ion (Ni )

The black precipitate of nickel sulphide dissolves in aqua regia and the reaction
takes place as follows:
3NiS + 2HNO3 + 6HCI 3NiCl2 + 2NO + 3S + 4H2O
After treatment with aqua regia nickel-chloride is obtained which is soluble
in water. When dimethyl glyoxime is added to the aqueous solution of nickel
chloride, made alkaline, by adding NH4OH solution, a brilliant red precipitate is
obtained.
Complex of red colour

(Stable form of complex)
108

2+
4. Test for Cobalt ion (Co )

Cobalt sulphide dissolves in aqua regia in the same manner as nickel sulphide.
When the aqueous solution of the residue obtained after treatment with aqua
regia is treated with a strong solution of potassium nitrite after neutralisation with
ammonium hydroxide and the solution is acidified with dil. acetic acid, a yellow
precipitate of the complex of cobalt named potassium hexanitritocobaltate (III)
is formed.
CoS + HNO3 + 3HCl CoCl2 + NOCl + S + 2H2O
CoCl2 + 7KNO2 + 2CH3COOH K3 [Co(NO2)6] + 2KCl + 2CH3COOK + NO + H2O
Potassium
hexanitritocobaltate(III)
(VI) Analysis of GroupV cations
If group-IV is absent then take original solution and add a small amount of solid
NH4Cl and an excess of NH4OH solution followed by solid ammonium carbonate
(NH4)2CO3. If a white precipitate appears, this indicates the presence of groupV
cations.
Dissolve the white precipitate by boiling with dilute acetic acid and divide
2+
2+
2+
the solution into three parts one each for Ba , Sr and Ca ions. Preserve a
small amount of the precipitate for flame test. Summary of confirmatory
tests is given in Table 7.16.
Table 7.16 : Confirmatory test for GroupV cations
Dissolve the precipitate by boiling with dilute acetic acid and divide the
2+
2+
2+
solution into three parts one each for Ba , Sr and Ca ions
2+
2+
2+
Ca ions
Ba ions
Sr ions
(a) To the first part add
potassium chromate
solution. A yellow
precipitate appears.
(b) Perform the flame
test
with
the
preserved precipitate.
A grassy green flame
is obtained.
(a) If barium is absent, take

second part of the solution
and
add
ammonium
sulphate solution. Heat
and scratch the sides of the
test tube with a glass rod
and
cool.
A
white
(b) Perform the flame test with
the preserved precipitate.
A crimson-red flame
confirms the presence of
Sr2+ ions.
(a) If both barium and

strontium are absent,
take the third part of
the solution. Add
ammonium oxalate
solution and shake
well.
A
white
precipitate of calcium
oxalate is obtained.
(b) Perform the flame test
with the preserved
precipitate. A brick red
flame, which looks
greenish-yellow through
blue glass, confirms the
2+
presence of Ca ions.
109
Chemistry of Confirmatory Tests of GroupV cations

The GroupV cations are precipitated as their carbonates which dissolve in acetic
acid due to the formation of corresponding acetates.
2+
1. Test for Barium ion (Ba )

(a)
Potassium chromate (K2CrO4) solution gives a yellow precipitate of barium

chromate when the solution of fifth group precipitate in acetic acid is treated
with it.
BaCO3 + 2CH3COOH (CH3COO)2 Ba + H2O + CO2
(CH3COO)2Ba + K2CrO4
(b)
BaCrO4
+ 2CH3COOK
Barium chromate
(yellow precipitate )
Flame test Take a platinum wire and dip it in conc. HCl. Heat it strongly
until the wire does not impart any colour to the non-luminous flame.
Now dip the wire in the paste of the (GroupV) precipitate in conc. HCl.
Heat it in the flame. A grassy green colour of the flame confirms the
presence of Ba2+ ions.
2+
2. Test for Strontium ion (Sr )

(a)
Solution of V group precipitate in acetic acid gives a white precipitate of

strontium sulphate with ammonium sulphate, (NH4)2SO4, solution on
heating and scratching the sides of the test tube with a glass rod.
SrCO3 + 2CH3COOH (CH3COO)2 Sr + H2O + CO2
(CH3COO)2 Sr + (NH4)2SO4
SrSO4
+ 2CH3COONH4
Strontium
sulphate
(White precipitate)
(b)
2+
Flame test Perform the flame test as given in the case of Ba . A crimson
2+
red flame confirms the presence of Sr ions.
2+
3. Test for Calcium ion (Ca )

(a)
Solution of the fifth group precipitate in acetic acid gives a white precipitate
with ammonium oxalate solution.
CaCO3 + 2CH3COOH (CH3COO)2 Ca + H2O + CO2
(CH3COO)2Ca + (NH4)2C2O4 (COO)2Ca
+ 2CH3COONH4
Ammonium
Calcium oxalate
oxalate
(White precipitate)
(b)
110
Flame test Perform the flame test as mentioned above. Calcium imparts
brick red colour to the flame which looks greenish-yellow through blue glass.
(VII) Analysis of GroupVI cations

2+
If groupV is absent then perform the test for Mg ions as given below.
Chemistry of Confirmatory Tests of GroupVI cations
2+
Test for Magnesium ion ( Mg )

(a)
If groupV is absent the solution may contain magnesium carbonate, which

is soluble in water in the presence of ammonium salts because the
equilibrium is shifted towards the right hand side.
+
2-
ZZZX
NH4 + CO 3 YZZ
Z NH3 + HCO 3
The concentration of carbonate ions required to produce a precipitate is
not attained. When disodium hydrogenphosphate solution is added and
the inner walls of the test tube are scratched with a glass rod, a white
crystalline precipitate of magnesium ammonium phosphate is formed which
2+
indicates the presence of Mg ions.
2+
Mg + Na2HPO4 Mg (NH4)PO4 + NH4OH + 2Na+ + H2O

Magnesium ammonium
phosphate (White precipitate)
Note down the observations and the inferences of the qualitative analysis
in tabular form as given in the specimen record given in pages 114-115.
Note :
Some times
precipitate of
magnesium
ammonium
phosphate
appears
after some
time.
So
warm the
solution and
scrach the
sides of test
tube after
a d d i n g
s o d i u m
hydrogen
phosphate
solution.
Precautions
(a)
(b)
(c)
(d)
(e)
(f)
(g)
Always use an apron, an eye protector and hand

gloves while working in the chemistry laboratory.
Before using any reagent or a chemical, read the
label on the bottle carefully. Never use
unlabelled reagent.
Do not mix chemicals and reagents
unnecessarily. Never taste any chemical.
Be careful in smelling chemicals or vapours.
Always fan the vapours gently towards your
nose (Fig. 7.9).
Never add sodium metal to water or throw it in
the sink or dustbin.
Always pour acid into water for dilution. Never
add water to acid.
Be careful while heating the test tube. The test
tube should never point towards yourself or
towards your neighbours while heating or
adding a reagent.
Fig. 7.9 : How to smell a gas
111
(h)
(i)
(j)
(k)
Be careful while dealing with the explosive compounds, inflammable substances,

poisonous gases, electric appliances, glass wares, flame and the hot substances.
Keep your working surroundings clean. Never throw papers and glass in the
sink. Always use dustbin for this purpose.
Always wash your hands after the completion of the laboratory work.
Always use the reagents in minimum quantity. Use of reagents in excess, not
only leads to wastage of chemicals but also causes damage to the environment.
(i) What is the difference between a qualitative and a quantitative analysis?
(ii) Can we use glass rod instead of platinum wire for performing the flame test? Explain
your answer.
(iii) Why is platinum metal preferred to other metals for the flame test?
(iv) Name the anions detected with the help of dilute H2SO4?
(v) Why is dilute H2SO4 preferred over dilute HCl while testing anions?
(vi) Name the anions detected by conc. H2SO4.
(vii) How is sodium carbonate extract prepared ?
(viii) What is lime water and what happens on passing carbon dioxide gas through it?
(ix) Carbon dioxide gas and sulphur dioxide gas both turn lime water milky. How will you
distinguish between the two?
(x) How will you test the presence of carbonate ion?
(xi) What is the composition of dark brown ring which is formed at the junction of two layers
in the ring test for nitrates?
(xii) Name the radical confirmed by sodium nitroprusside test.
(xiii) What is chromyl chloride test ? How do you justify that CrO2Cl2 is acidic in nature?
(xiv) Why do bromides and iodides not give tests similar to chromyl chloride test?
(xv) Describe the layer test for bromide and iodide ions.
112
(xvi) Why is silver nitrate solution stored in dark coloured bottles?

(xvii) How do you test the presence of sulphide ion?
(xviii) Why does iodine give a blue colour with starch solution?
(xix) What is Nesslers reagent?
(xx) Why is original solution for cations not prepared in conc. HNO3 or H2SO4?
(xxi) Why cannot conc. HCl be used as a group reagent in place of dil. HCl for the precipitation
of Ist group cations?
(xxii)
How can one prevent the precipitation of GroupIV radicals, with the second group
radicals?
(xxiii)
Why is it essential to boil off H2S gas before precipitation of radicals of groupIII?
(xxiv)
Why is heating with conc. nitric acid done before precipitation of groupIII?
(xxv)
Can we use ammonium sulphate instead of ammonium chloride in groupIII?
(xxvi)
Why is NH4OH added before (NH4)2CO3 solution while precipitating groupV cations?
(xxvii)
Why do we sometimes get a white precipitate in groupVI even if the salt does not
2+
contain Mg radical?
(xxviii)
What is aqua regia?
(xxix)
Name a cation, which is not obtained from a metal.
(xxx)
How can you test the presence of ammonium ion?
(xxxi)
Why are the groupV radicals tested in the order Ba2+, Sr2+ and Ca2+ ?
(xxxii)
Why does conc. HNO3 kept in a bottle turn yellow in colour?
(xxxiii)
Why should the solution be concentrated before proceeding to groupV?
(xxxiv)
Why is the reagent bottle containing sodium hydroxide solution never stoppered?
(xxxv)
What do you understand by the term common ion effect?
(xxxvi)
Why is zinc sulphide not precipitated in groupII?
113
SPECIMEN RECORD
OF
SALT ANALYSIS
Aim
To analyse the given salt for one anion and one cation present in it.
Material required
Boiling tubes, test tubes, test tube holder, test tube stand, delivery tube, corks,
filter papers, reagents
Sl. No.
Experiment
Observation
Inference
2+
2+
2+
2+
1.
Noted the colour of the given

salt.
White
Cu , Fe , Ni ,Co ,
2+
Mn are absent.
2.
Noted the smell of the salt.
No specific smell.
S , SO3 , CH3COO
may be absent.
3.
Heated 0.5 g of the salt in a

dry test tube and noted the
colour of the gas evolved and
change in the colour of the
residue on heating and
cooling.
(i) No gas was evolved.
(i) CO 3
may
be
present, NO3 , NO2 ,
Br
may
be
absent.
2+
(ii) Zn
may
be
absent.
4.
Prepared a paste of the salt

with conc. HCl and performed
the flame test.
No distinct colour of the

flame seen.
5.
Borax bead test was not

performed as the salt was
white in colour.
6.
Treated 0.1 g of salt with 1 mL

dil.H2SO4 and warmed.
No effervescence and
evolution of vapours.
CO 3 , SO 3 , S , NO 2 ,
7.
Heated 0.1 g of salt with 1 mL

conc. H2SO4.
No gas evolved.
Cl , Br , I , NO3 , C2O4
are absent.
8.
Acidified 1mL of aqueous salt

solution with conc. HNO 3 .
Warmed the contents and then
added 4-5 drops of ammonium
molybdate solution.
No yellow precipitate
PO4 absent.
114
(ii) No
particular
change in colour of
the residue is
observed
when
heated and when
cooled.
2+
2+
2+
Ca , Sr , Ba
may be absent.
Cu
2+
CH3COO absent.

2
9.
Acidified water extract of the

salt with dil. HCl and then
added 2mL of BaCl2 solution.
A white ppt. is obtained

which is
insoluble in conc. HNO3
and conc. HCl.
SO4
10.
Heated 0.1 g of salt with 2 mL

NaOH solution.
Ammonia gas is not

evolved.
NH4 absent.
11.
Attempted to prepare original

solution of the salt by
dissolving 1g of it in 20 mL
water.
Clear solution formed
Water soluble salt is

present.
12.
To a small part of the above

salt solution added 2 mL of
dil. HCl.
No white precipitate
formed.
GroupI absent.
13.
Passed H2S gas through one

portion of the solution of step 12.
No precipitate formed.
GroupII absent.
14.
Since salt is white, heating

with conc. HNO 3 is not
required. Added about 0.2 g
of solid ammonium chloride
and then added excess of
ammonium hydroxide to the
solution of step 12.
GroupIII absent.
15.
Passed H2S gas through the

above solution.
GroupIV absent.
16.
Added excess of ammonium

hydroxide solution to the
original solution and then
added 0.5 g of ammonium
carbonate.
GroupV absent.
17.
To the original solution of salt

added ammonium hydroxide
solution, followed by disodium
hydrogen phosphate solution.
Heated and scratched the
sides of the test tube.
White precipitate.
Mg
present.
2+
confirmed.
Result
The given salt contains:
Anion
: SO4
Cation : Mg
2+
115
APPENDICES
APPENDIX I
ARRANGEMENT OF REAGENTS IN THE LABORATORY
Laboratory assistants must see that the reagent bottles on each shelf are properly arranged, labelled and
contain sufficient quantity of the freshly prepared reagents.
1. Reagents to be placed on the shelf of each seat
Reagents kept in narrow-mouthed stoppered bottles
1. Ammonium carbonate
2. Ammonium hydroxide
3. Hydrochloric acid (dil.)
4. Hydrochloric acid (conc.)
5.
6.
7.
8.
Lime water
Nitric acid (dil.)
Sulphuric acid (dil.)
Sulphuric acid (conc.)
2. Reagents to be placed on common shelf

(A) Solutions kept in narrow-mouthed stoppered bottles
1.
2.
3.
4.
5.
6.
7.
8.
9.
10.
11.
12.
13.
14.
15.
16.
17.
18.
Acetic acid (glacial)

Acetic acid (dilute)
Alkaline--naphthol
Ammonium molybdate
Ammonium oxalate
Ammonium sulphate
Ammonium sulphide (yellow)
Barium chloride
Bromine water
Calcium chloride
Calcium sulphate
Carbon disulphide
Chlorine water
Cobalt nitrate
Copper sulphate
Dimethyl glyoxime
Ferric chloride
Ferrous sulphate
19.
20.
21.
22.
23.
24.
25.
26.
27.
28.
29.
30.
31.
32.
33.
34.
35.
36.
37.
Lead acetate
Magnesium sulphate
Mercuric chloride
Methyl orange
Nesslers reagent
Phenolphthalein
Potassium chromate
Potassium dichromate
Potassium ferricyanide
Potassium ferrocyanide
Potassium iodide
Potassium permanganate
Rectified spirit
Silver nitrate
Sodium hydrogenphosphate
Sodium nitroprusside
Stannous chloride
Starch solution
Universal indicator
(B) Reagents kept in wide-mouthed bottles on common shelf

(a)
Solids
1.
2.
3.
4.
5.
6.
7.
Ammonium chloride
Borax
Ferrous sulphate
Fusion mixture
Manganese dioxide
Oxalic acid
Potassium chromate
8.
9.
10.
11.
12.
13.
14.
Sodium carbonate
Sodium hydrogencarbonate
Sodium hydroxide
Sodium nitrate
Sodium peroxide
(b) Metals
1.
2.
Copper
Tin
3. Zinc granules
4. Zinc powder
(c) Papers
1.
2.
3.
4.
Lead acetate paper

Litmus paper (blue)
Litmus paper (red)
Potassium dichromate paper
5.
6.
7.
8.
Starch iodide paper

Starch paper
Turmeric paper
Universal indicator paper
129
APPENDIX II
LIST OF CHEMICALS AND APPARATUS FOR CHEMISTRY LABORATORY
Sl. No. Inorganic Chemicals
Grade*
1.
2.
3.
4.
5.
6.
7.
8.
9.
10.
11.
12.
13.
14.
15.
16.
17.
18.
19.
20.
21.
22.
23.
24.
25.
26.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
27.
28.
29.
30.
31.
32.
33.
34.
35.
36.
37.
38.
39.
40.
41.
42.
43.
44.
45.
46.
47.
48.
49.
50.
51.
52.
53.
54.
55.
56.
57.
58.
Alum (potash)
Aluminium chloride
Aluminium sulphate
Ammonium acetate
Ammonium carbonate
Ammonium ceric nitrate
Ammonium chloride
Ammonium molybdate
Ammonium nitrate
Ammonium oxalate
Ammonium phosphate
Ammonium sulphate
Ammonium thiocyanate
Arsenious oxide
Barium chloride
Barium nitrate
Bismuth nitrate
Boric acid
Bromine (liquid)
Cadmium carbonate
Cadmium chloride
Cadmium nitrate
Calcium carbonate
Calcium chloride
Calcium hydoxide
Calcium hydrogenphosphate
anhydrous
Calcium nitrate
Calcium oxide
Chlorine water
Cobalt nitrate
Copper carbonate
Copper sulphate
Copper turnings
Cupric acetate
Cupric nitrate
Disodium tetraborate
Ferric alum
Ferric chloride
Ferrous ammonium sulphate
Ferrous sulphate
Ferrous sulphide
Hydrochloric acid (conc.)
Hydrogen peroxide
Iodine
Iron filings
Lead acetate
Lead chloride
Lead nitrate
Liquor ammonia
Litmus solution
Magnesium bromide
Magnesium carbonate
Magnesium chloride
Magnesium ribbon
Magnesium sulphate
Manganese dioxide
Manganese sulphate
Marble chips
* L. R. = Laboratory reagent
A. R. = Analytical reagent
130
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
Sl. No. Inorganic Chemicals

59.
60.
61.
62.
63.
64.
65.
66.
67.
68.
69.
70.
71.
72.
73.
74.
75.
76.
77.
78.
79.
80.
81.
82.
83.
84.
85.
86.
87.
88.
89.
90.
91.
92.
93.
94.
95.
96.
97.
98.
99.
100.
101.
102.
103.
104.
105.
106.
107.
108.
109.
110.
111.
112.
113.
Mercuric chloride
Methyl orange
Methyl red
Nickel (II) nitrate
Nitric acid (conc.)
pH paper and chart
Potash alumns
Potassium bromide
Potassium chromate
Potassium ferricyanide
Potassium ferrocyanide
Potassium hydroxide
Potassium iodate
Potassium iodide
Potassium nitrate
Potassium nitrite
Potassium sulphate
Potassium thiocyanate
Schiffs reagent (or Fuchsin)
Silver nitrate
Sodium acctate
Sodium bromide
Sodium carbonate
Sodium chloride
Sodium dihydrogenorthophosphate
Sodium dihydrogenphosphate
Sodium hydrogencarbonate
Sodium hydroxide (flakes)
Sodium metabisulphite
Sodium metal
Sodium nitrate
Sodium nitrite
Sodium oxalate
Sodium peroxide
Sodium potassium tartarate
(Rochelles salt)
Sodium sulphate
Sodium tartarate
Sodium thiosulphate
Stannous chloride
Starch (soluble)
Sulphanilic acid
Sulphur
Sulphuric acid, (commercial)
Tin metal
Universal indicator solution/paper
Uranyl zinc acetate
Zinc acetate
Zinc carbonate
Zinc chloride
Zinc metal (granulated)
Zinc oxide
Zinc sulphate
Grade
L.R.
A.R.
A.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
APPENDIX II
Sl. No. Organic Chemicals
1.
2.
3.
4.
5.
6.
7.
8.
9.
10.
11.
12.
13.
14.
15.
16.
17.
18.
19.
20.
21.
22.
23.
24.
25.
26.
27.
28.
29.
30.
31.
32.
33.
Acetaldehyde
Acetanilide
Acetic acid (ethanoic acid)
Acetic anhydride
Acetone
Acetyl chloride
Amyl alcohol
Aniline
Benedicts reagent
Benzene
Benzoic acid
Benzyl alcohol
Benzyaldehyde
Butanol
Carbon disulphide
Carbon tetrachloride
Castor oil
Chloroform
Citric acid
Congo red (direct azo dye)
Diazoaminobenzene
p-dichlorobenzene
Diethyl ether
Dimethyl glyoxime
2, 4-Dinitro phenyl hydrazine
Diphenylamine
Eriochram Black-T
Ethyl acetate
Ethyl alcohol
Ethylamine
Ethylene diamine tetraacetic
acid disodium salt
Fehlings solutions (A & B)
Formaldehyde
Grade
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
AR.
L.R.
L.R.
L.R.
A.R.
L.R.
L.R.
Sl. No. Glassware (Borosilicate glass)
Sl. No. Organic Chemicals

34.
35.
36.
37.
38.
39.
40.
41.
42.
43.
44.
45.
46.
47.
48.
49.
50.
51.
52.
53.
54.
55.
56.
57.
58.
59.
60.
61.
62.
63.
64.
65.
66.
67.
Formic acid
Fructose
Glucose
Glycerol
Lactose
Linseed oil
Liquid paraffin
Malachite green (basic dye)
Maltose
Machine oil
Methyl alcohol
Methyl orange (acidic dye)
Mustard oil
Naphthalene
1-Naphthylamine
1-Naphthol
2-Naphthol
Ninhydrin
Oxalic acid
Petroleum ether (6080)
Phenol
Phenolphthalein
Phenyl hydrazine hydrochloride
Phthalic acid
Phthalic anhydride
Pyridine
Pyrogallol
Resorcinol
Salicylic acid
Succinic acid
Sucrose
Thiourea
p-Toluidine
Urea
Beaker (50 mL)
18.
Measuring cylinder (10 mL)
2.
Beaker (100 mL)
19.
3.
Beaker (150 mL)
20.
4.
Beaker (250 mL)
21.
6.
Beaker (500 mL)
22.
7.
Boiling tubes
23.
Petri dish (8 cm diameter)
8.
Burette (50 mL)
24.
Pipette (10 mL)
9.
25.
Pipette (25 mL)
10.
26.
Round bottom flask (500 mL)
11.
12.
Flat bottomed flask (1 litre)
27.
Round bottom flask (1 litre)
13.
Funnel (8 cm diameter)
28.
Separating funnel (250 mL)
14.
Glass droppers
15.
Kipps apparatus (diameter 1000 mm)

Kjeldals flask
17.
Liebigs condenser
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
L.R.
Sl. No. Glassware (Borosilicate glass)
1.
16.
Grade
29.
Test tube (15 mL)
30.
Thieles tube
31.
Watch glass (9 cm diameter)
32.
Water aspirator weighing bottle
131
Miscellaneous Articles
Sl. No. Item Description
132
Sl. No. Item Description
1.
Agar agar
34.
Polythene wash bottle (500 mL)
2.
Ammeter (0-1 amp)
35.
Porcelain dish
3.
Beehive shelf
36.
Reagent bottle (150 mL)
4.
Blow pipe
37.
5.
Blue glass
38.
6.
Bunsen burner
39.
7.
Burette brush
40.
Ring clamp
8.
Burette stand (wooden)
41.
Rubber cork-all sizes
9.
Calorimeter
42.
Rubber tubing
43.
Sand paper
44.
Sand bath
45.
Spatula (plastic)
46.
Spirit
47.
Spirit lamp
48.
Stop watch
49.
Test tube brush
50.
Test tube holder
51.
Test tube stand (plastic)
52.
Thermometer - ordinary (100C and 360C)
53.
Thermometer (0110C and 1/10th division)
54.
Thistle funnel
55.
Triangular file
10.
Capillary tube
11.
Charcoal black
12.
Chemical balance
13.
Clamp
14.
Connecting wires
15.
Copper plate
16.
Cork
17.
Cork borer sets
18.
Cork opener
19.
Dry cell (1.5 volts)
20.
Filter paper sheets (Whatman and ordinary)
21.
Fractional weights
22.
Funnel stand
23.
Gas jar with lid
24.
Glass rod
56.
Tripod stand (iron)
25.
Glass tube
57.
Trough
26.
Glass wool
58.
Wash bottle
27.
Glazed tile (white)
59.
Water bath
28.
Ignition tube
60.
Water distillation plant
29.
Iron stand
61.
Wax (paraffin)
30.
Key (one way)
62.
Weight box (for chemical balance)
31.
Mortar and pestle
63.
Wire gauze (asbestos centre)
32.
Pair of tongs
64.
Woulf bottle
33.
Platinum wire
65.
Zinc plate
APPENDIX III
PREPARATION OF COMMON LABORATORY REAGENTS
I. Concentration acids
Name
Approximate
Specific
Approximate
Percentage
concentration
gravity
amount
by weight
1.
Acetic acid (glacial)
17.6 M (17.6 N)
1.06
1.06 g/mL
99.5%
2.
Conc. Hydrochloric acid
11.7 M (11.7 N)
1.19
0.426 g/mL
36.0%
3.
Conc. Nitric acid
15.6 M (15.6 N)
1.42
0.998 g/mL
69.5%
4.
Conc. Sulphuric acid
18 M (36.0 N)
1.84
1.76 g/mL
98.0%
Note : Concentrated acids are used as supplied.
II. Dilute acids

Name
Concentration
Method of preparation
1.
Dil. Acetic acid
5 M (5 N)
Dilute 285 mL of glacial acetic acid with distilled water

water and make up the volume to 1 litre.
2.
Dil. Hydrochloric acid
5 M (5 N)
Add 430 mL of conc. HCl in the distilled water and make

up the volume to 1 litre.
3.
Dil. Nitric acid
5 M (5 N)
Add 320 mL of conc. nitric acid to distilled water and

make up the volume to litre.
4.
Dil. Sulphuric acid
2.5 M (5 N)
Pour 140 mL of conc. sulphuric acid slowly and with

constant stirring in 500 mL of distilled water. Cool and
make up the volume to 1 litre.
III. Bases
Name
Concentration
1.
Ammonia solution (Liquor ammonia)
15 M (15 N)
As supplied
2.
Dil. Ammonia solution

(ammonium hydroxide)
2 M (2 N)
Pour 266.6 mL of the conc. ammonia solution in distilled

water and make up the volume to 1 litre.
Sodium hydroxide
5 M (5 N)
Dissolve 200 g sodium hydroxide pellets in 1 L of distilled

water.
3.
IV. Other reagents

Name
Concentration
Molar mass
1.
Ammonium acetate
2 M (2 N)
77
Dissolve 154 g of the salt in distilled water

anddilute to 1 litre.
2.
Ammonium chloride
5 M (5 N)
53.5
Dissolve 267.5 g of the salt in distilled water and

dilute to one litre.
3.
Ammonium carbonate
1.7 M (3.5 N)
96
Dissolve 160 g of ammonium carbonate in 140 mL

liquor ammonia and make up the solution to 1
litre with distilled water.
133

4.
Ammonium molybdate
Dissolve 100 g of the salt in a mixture of 100 mL

of liquor ammonia solution and add 250 g of
ammonium nitrate and dilute it to 1 litre with
distilled water.
5.
Ammonium oxalate
0.5 M (1 N)
142
Dissolve 71 g of the salt in distilled water and

dilute to 1 litre.
6.
Ammonia sulphate
1 M (2 N)
132

dilute to 1 litre.
7.
Barium chloride
BaCl2.2H2O
0.5 M (0.5 N)
244

dilute to 1 litre.
8.
Bromine water
approx. saturated
160
Add 2 mL of bromine in 100 mL of distilled water

shake the mixture well. Keep it in a dark bottle.
9.
Calcium chloride
0.5 M (0.5 N)
219

71
Prepare chlorine gas by treating solid KMnO4

with conc. HCl. Saturate one litre of distilled
water with chlorine gas and keep the solution in
a dark coloured bottle.
249.5

make up the volume to 100 mL.
291

10. Chlorine water
11. Copper sulphate
14%
12. Cobalt nitrate
0.15 M (0.075 N)
13. Dimethyl glyoxime
1%
Dissolve 1.0 g of the solid in 100 mL ethyl

alcohol.
14. Diphenylamine
0.5%
Dissolve 0.5 g of the solid in 85 mL of conc.

sulphuric acid and dilute it with care with distilled
water to 100 mL.
15. Disodium hydrogen

phosphate
Na2HPO4.12H2O
0.3 M (N)
358

make up the volume to litre.
16. Ferric chloride

FeCl3.6H2O
0.33 M (1 N)
270
Dissolve 90 g of the salt in distilled water

containing 10 mL of conc. hydrochloric acid and
254
Dissolve 1.0 g of iodine crystals in a solution of

2 g potassium iodide in minimum amount of water
and dilute the solution to 100 mL.
17. Iodine solution
18. Lead acetate

(CH3COO)2 Pb
0.5 M (N)
19. Lime water

Ca(OH)2
0.02 M (0.04 N)
20. Litmus solution (blue)
21. Litmus solution (red)
Dissolve 200 g of solid salt in 500 mL of distilled

water containing 15 mL acetic acid and make up
the volume to 1 litre with distilled water.
74
Dissolve 10 g of litmus in distilled water and

make the volume to 1 litre.
To the blue litmus solution add about 10 drops
of dilute hydrochloric acid.
Dissolve 1 g of the solid in 1 litre of distilled
water.
22. Methyl orange

23. Mercuric chloride
134
0.25 M (0.5 N)
Shake 23 g of calcium hydroxide with 1 L distilled

water, filter the solution after some time and keep
it in a reagent bottle. Bottle should be securely
stoppered in order to protect the reagent from
CO2 of atmosphere.
272
Dissolve 70 g of the salt in small amount of

distilled water and make up the volume to 1 litre
with distilled water.
APPENDIX III
24. Nesslers reagent
Dissolve 23 g of mercuric iodide and 16 g of

potassium iodide in distilled water and make up
the volume to 100 mL. Add 150 mL of 4 M NaOH
solution. Allow it to stand for 24 hours and decant
the solution. Solution should be stored in a dark
coloured bottle.
25. Potassium chromate

K2CrO4
0.25 M (0.5 N)
194

26. Potassium dichromate
0.15 M (1 N)
294

27. Potassium ferrocyanide
0.15 M (0.5 N)
368

dilute to 1 litre.
28. Potassium ferricyanide
0.2 M (0.5 N)
329

dilute to 1 litre.
29. Potassium iodide
0.5 M (0.5 N)
166

30. Potassium permanganate
0.06 M (0.3 N)
158
Dissolve 10.0 g of the salt in 1 litre distilled

water. Heat the solution and filter it through glass
wool.
31. Potassium thiocyanate
0.5 M (0.5 N)
97

32. Phenolphthalein
1%
33. Silver nitrate
0.1 M
34. Sodium acetate
5 M (5 N)
Dissolve 1.0 g of the solid in 100 mL of ethyl

alcohol.
170
Dissolve 17 g of the salt in 250 mL of distilled

water and store it in a brown coloured bottle.
82
Dissolve 410 g of salt in distilled water and dilute

to 1 litre.
35. Sodium nitroprusside
Dissolve 4 g of the solid in 100 mL of distilled

water.
36. Starch
Prepare a paste of about 1.0 g of soluble starch

in cold water and pour it gradually in 100 mL of
boiling water with constant stirring. Boil it for 10
minutes and cool.
37. Stannous chloride

SnCl2.2H2O
0.25 M (0.5 N)
38. Yellow ammonium sulphide

(NH4)2Sx
6 N
39. Buffer solution in non-aqueous media

(For EDTA titration)
40. Eriochrome Black T in non aqueous media

(Indicator for EDTA titration)
226
Dissolve 55.0 g of the salt in 200 mL of conc.

hydrochloric acid by heating (if necessary). Dilute
with distilled water to make up the volume to 1
litre. Add several pieces of metallic tin into the
solution.
Take about 200 mL of conc. ammonia solution in
a bottle and saturate it with H2S gas. Add 10 g
of flower of sulphur and 200 mL of conc. NH4OH.
Warm gently and shake well until sulphur is
completely dissolved. Dilute the solution to 1 litre
with distilled water.
Dissolved 67.5 g of ammonium chloride in 570 mL
conc. ammonia solution and make up the volume
to 1 L.
Dissolve 0.5 gram of solid Eriochrome
Black-T in methanol and make up the volume to
100 mL.
135
Special Reagents Used in Organic Analysis

1.
Alcohol (1:1)
Mix equal volumes of rectified spirit and distilled water.
2.
Alcoholic potassium hydroxide solution
Dissolve 11.2 g of potassium hydroxide in 100 mL ethand (or rectified

spirit) by boiling for 30 minutes.
3.
Alkaline -naphthol
Dissolve 10 g of -naphthol in 100 mL of 10% sodium hydroxide solution.
4.
Barfoed reagent
Dissolve 13 g of copper acetate in 200 mL of 1% acetic acid.
5.
Benedicts solution
Dissolve 17.3 g of crystalline copper sulphate in 100 mL of water.

Separately dissolve 173 g of sodium citrate and 100 g of anhydrous
sodium carbonate in 800 mL of water. Mix both solutions and make up
the volume to 1 L.
6.
Ceric ammonium nitrate solution
Dissolve 40 g of the reagent in 100 mL of 2 N nitric acid.
7.
Copper sulphate solution
Dissolve 14 g of copper sulphate in 100 mL water (14% solution)
8.
2,4dinitrophenylhydrazine reagent
(i)
(ii)
For water soluble compounds
Add 0.5 g solid in a mixture of 42 mL conc. HCl and 54 mL water and

dissolve by warming on water bath. Add water to make up the volume to
250 mL.
For compounds not soluble in water :
Dissolve 1 g of reagent in 7.5 mL conc. sulphuric acid. Add this solution

gradually to 7.5 mL rectified spirit. Make up the volume to 250 mL by
adding water.
9.
*Fehlings solution A
Dissolve 69.28 g of copper sulphate crystals in 1 L of water.
10.
*Fehlings solution B
Dissolve 350 g of Rochelles salt and 100 g sodium hydroxide in 1 L

water.
11.
Hydroxylamine hydrochloride
Dissolve 69.5 g of dry solid in 1 L of methyl alcohol.
12.
Molischs reagent
Dissolve 10 g of 1naphthol in 90 mL of rectified spirit.
13.
Ninhydrin reagent
Prepare 0.25% aqueous solution.
14.
Prepare 1 % aqueous solution.
15.
Schiffs reagent
Dissolve 1 g of rosaniline in 50 mL water with gentle warming, cool,

saturate with sulphur dioxide gas. Dilute the solution upto 1 L with water.
If pink colour reappears on standing add few drops of saturated aqueous
solution of SO2 with stirring until the colour just disappears.
16.
Seliwanoffs reagent
Dissolve 1 g of resorcinol in 100 mL of 20% hydrochloric acid.
17.
Sodium hypochlorite (2M)
Dissolve 100 g of NaOH in 200 mL of water in a large beaker. Cool the

solution and add about 500 g of crushed ice. Weigh the beaker on a rough
balance and pass chlorine gas until the weight increases by 72 g. Dilute
the solution to 1 L with water. The solution must be kept in a cool dark
place. Even then it slowly decomposes.
18.
Tollens reagent
To 1 mL
hydroxide
hydroxide
hydroxide
reagent.
of 2% solution of silver nitrate add 1 mL of 10% sodium

till the precipitate just appears. Add solution of ammonium
with stirring till the solution becomes clear. Ammonium
should not be added in excess. Always use fresh Tollens
*Before use, mix equal volumes of Fehlings solution A and Fehlings solution B.
136
APPENDIX IV
SOME USEFUL TABLES
Table 1 : Fundamental physical constants

Physical constant
Symbol
Value
Acceleration due to gravity
9.81 ms2
Atomic mass unit
amu
1.66053 1027 Kg
Avogadro constant
NA
6.02217 1023 mol1
Boltzmann constant
1.38062 1023 J K1
Electronic charge
1.602192 1019 C
Faraday cosntant
9.64867 104 C mol1
Gas constant
8.314 J K1 mol1
Ice-point temperature
Tice
273.150 K
Molar volum of ideal gas at stp.
Vm
2.24136 102 m3 mol1
Permittivity of a vaccuum
E0
8.854185 1012
Kg1 m3s4 A2
Plank constant
6.62620 1034 J s
Rydberg constant
Rw
1.973731 107 m1
Standard pressure (atmosphere)
101325 N m2
2.997925 108 m s1
Triple point of water
273016 K
Velocity of light of vacuum
Table 2 : General properties of some organic compounds

Compound
mp.C
bp.C
Density/
Kg m
(298 K)
Refractive
104
103
index (nD)
Viscosity/
Surface
(293 K)
N s m2)
Tension/
(298 K)
N m1
(293 K)
Acetic acid
16.7
117.9
1044.0
1.3716
11.55
27.8
94.7
56.1
785.0
1.3588
3.16
23.7
6.3
184.1
1022.0 (293)
1.5863
3.71
42.9
122.4
249.0
1266.0 (288)
1.504 (405)
Carbon tetra-chloride 22.9
76.5
1584.0
1.4601
8.8
26.95
Acetone
Aniline
Benzoic acid
Chlorobenzene
45.2
132.0
1106.0
1.5241
7.97
33.56
Chloroform
63.5
61.7
1480.0
1.4459
5.42
27.14
Cyclohexane
Di-ethyl ether
Ethyl acetate
6.6
80.7
774.0
1.42662
9.8
25.5
116.2
34.51
714.0
1.3526
2.22
17.01
82.4
77.1
900.0 (293)
1.3723
4.41
23.9
114.1
78.3
785.0
1.3611
10.6
22.75
Glycerol
18.07
290.0
1264.4
1.4746
942.0
63.4
Hexane
95.3
68.7
655.0
1.37506
2.94
18.43
Methanol
Ethanol
97.7
64.5
787.0
1.3288
5.47
22.61
Napthalene
80.3
218.0
1180.0
1.4003 (297)
Phenol
40.9
181.8
1132.0
1.5509
Toluene
95.1
110.6
862.0
1.4961
5.50
28.5
137

Table 3 : Solubility of common inorganic compounds in water
These ions form soluble compounds
(solubility greater than 0.1 M)
with these cations
Form slightly
soluble compounds
(solubility less than 0.1 M)
Name
of
Anion
Symbol
nitrate
NO3
Most cations
None
acetate
CH3COO
Most cations
Ag+
chloride
Cl
Most cations
Ag+, Pb2+, Hg2
bromide
Br
Most cations
Ag+, Pb2+, Hg2
iodide
I,
Most cations
Ag+, Pb2+, Hg2
sulphate
SO4 ,
Most cations
Br2+, Sr2+, Pb2+, Ag+
chromate
CrO4
Most cations
Br2+, Sr2+, Pb2+, Ag+
sulphide
S2,
NH4 , alkali metal cations,
2+
2+
2+
Most other cations
and alkaline earth metal cations

hydroxide
OH ,
NH4 , alkali metal and alkaline earth
Most other cations
metal and Ba2+ and Sr2+

2
carbonate
CO3
phosphate
PO4
138
NH4 and alkali metal cations

except Li+
Most other cations
APPENDIX V
ELEMENTS, THEIR ATOMIC NUMBER AND MOLAR MASS
Element
Actinium
Aluminium
Americium
Antimony
Argon
Arsenic
Astatine
Barium
Berkelium
Beryllium
Bismuth
Bohrium
Boron
Bromine
Cadmium
Caesium
Calcium
Californium
Carbon
Cerium
Chlorine
Chromium
Cobalt
Copper
Curium
Dubnium
Dysprosium
Einsteinium
Erbium
Europium
Fermium
Fluorine
Francium
Gadolinium
Gallium
Germanium
Gold
Hafnium
Hassium
Helium
Holmium
Hydrogen
Indium
Iodine
Iridium
Iron
Krypton
Lanthanum
Lawrencium
Lead
Lithium
Lutetium
Magnesium
Manganese
Meitneium
Mendelevium
Symbol
Atomic
Number
Molar
mass/
(g mol1)
Element
Ac
Al
Am
Sb
Ar
As
At
Ba
Bk
Be
Bi
Bh
B
Br
Cd
Cs
Ca
Cf
C
Ce
Cl
Cr
Co
Cu
Cm
Db
Dy
Es
Er
Eu
Fm
F
Fr
Gd
Ga
Ge
Au
Hf
Hs
He
Ho
H
In
I
Ir
Fe
Kr
La
Lr
Pb
Li
Lu
Mg
Mn
Mt
Md
89
13
95
51
18
33
85
56
97
4
83
107
5
35
48
55
20
98
6
58
17
24
27
29
96
105
66
99
68
63
100
9
87
64
31
32
79
72
108
2
67
1
49
53
77
26
36
57
103
82
3
71
12
25
109
101
227.03
26.98
(243)
121.75
39.95
74.92
210
137.34
(247)
9.01
208.98
(264)
10.81
79.91
112.40
132.91
40.08
251.08
12.01
140.12
35.45
52.00
58.93
63.54
247.07
(263)
162.50
(252)
167.26
151.96
(257.10)
19.00
(223)
157.25
69.72
72.61
196.97
178.49
(269)
4.00
164.93
1.0079
114.82
126.90
192.2
55.85
83.80
138.91
(262.1)
207.19
6.94
174.96
24.31
54.94
(268)
258.10
Mercury
Molybdenum
Neodymium
Neon
Neptunium
Nickel
Niobium
Nitrogen
Nobelium
Osmium
Oxygen
Palladium
Phosphorus
Platinum
Plutonium
Polonium
Potassium
Praseodymium
Promethium
Protactinium
Radium
Radon
Rhenium
Rhodium
Rubidium
Ruthenium
Rutherfordium
Samarium
Scandium
Seaborgium
Selenium
Silicon
Silver
Sodium
Strontium
Sulphur
Tantalum
Technetium
Tellurium
Terbium
Thallium
Thorium
Thulium
Tin
Titanium
Tungsten
Ununbium
Ununnilium
Unununium
Uranium
Vanadium
Xenon
Ytterbium
Yttrium
Zinc
Zirconium
Symbol
Atomic
Number
Hg
Mo
Nd
Ne
Np
Ni
Nb
N
No
Os
O
Pd
P
Pt
Pu
Po
K
Pr
Pm
Pa
Ra
Rn
Re
Rh
Rb
Ru
Rf
Sm
Sc
Sg
Se
Si
Ag
Na
Sr
S
Ta
Tc
Te
Tb
Tl
Th
Tm
Sn
Ti
W
Uub
Uun
Uuu
U
V
Xe
Yb
Y
Zn
Zr
80
42
60
10
93
28
41
7
102
76
8
46
15
78
94
84
19
59
61
91
88
86
75
45
37
44
104
62
21
106
34
14
47
11
38
16
73
43
52
65
81
90
69
50
22
74
112
110
111
92
23
54
70
39
30
40
Molar
mass/
(g mol1)
200.59
95.94
144.24
20.18
(237.05)
58.71
92.91
14.0067
(259)
190.2
16.00
106.4
30.97
195.09
(244)
210
39.10
140.91
(145)
231.04
(226)
(222)
186.2
102.91
85.47
101.07
(261)
150.35
44.96
(266)
78.96
28.08
107.87
22.99
87.62
32.06
180.95
(98.91)
127.60
158.92
204.37
232.04
168.93
118.69
47.88
183.85
(277)
(269)
(272)
238.03
50.94
131.30
173.04
88.91
65.37
91.22
The value given in parenthesis is the molar mass of the isotope of largest known half-life.
139
APPENDIX VI
SOME USEFUL CONVERSION FACTORS
Common Unit of Mass and Weight

1 pound = 453.59 grams
1 pound = 453.59 grams = 0.45359 kilogram
1 kilogram = 1000 grams = 2.205 pounds
1 gram = 10 decigrams = 100 centigrams
= 1000 milligrams
1 gram = 6.022 1023 atomic mass units or u
1 atomic mass unit = 1.6606 1024 gram
1 metric tonne = 1000 kilograms
= 2205 pounds
Common Unit of Volume
1 quart = 0.9463 litre
1 litre = 1.056 quarts
1 litre = 1 cubic decimetre = 1000 cubic
centimetres = 0.001 cubic metre
1 millilitre = 1 cubic centimetre = 0.001 litre
= 1.056 10-3 quart
1 cubic foot = 28.316 litres = 29.902 quarts
= 7.475 gallons
Common Units of Energy
1 joule = 1 107 ergs
1 thermochemical calorie** = 4.184 joules
= 4.184 107 ergs
= 4.129 102 litre-atmospheres
= 2.612 1019 electron volts
7
1 ergs = 1 10 joule = 2.3901 108 calorie
1 electron volt = 1.6022 1019 joule
= 1.6022 1012 erg
= 96.487 kJ/mol
1 litre-atmosphere = 24.217 calories
= 101.32 joules
= 1.0132 109 ergs
1 British thermal unit = 1055.06 joules
= 1.05506 1010 ergs
= 252.2 calories
Common Units of Length

1 inch = 2.54 centimetres (exactly)
1 mile = 5280 feet = 1.609 kilometres
1 yard = 36 inches = 0.9144 metre
1 metre = 100 centimetres
= 39.37 inches
= 3.281 feet
= 1.094 yards
1 kilometre = 1000 metres
= 1094 yards
= 0.6215 mile
1 Angstrom = 1.0 108 centimetre
= 0.10 nanometre
= 1.0 1010 metre
= 3.937 109 inch
Common Units of Force* and Pressure
1 atmosphere= 760 millimetres of mercury
= 1.013 105 pascals
= 14.70 pounds per square inch
1 bar = 105 pascals
1 torr = 1 millimetre of mercury
1 pascal = 1 kg/ms2 = 1 N/m2
Temperature
SI Base Unit: Kelvin (K)
K = -273.15C
K = C + 273.15
F
= 1.8(C) + 32
C =
F 32
1.8
Force: 1 newton (N) = 1 kg m/s 2 , i.e.,the force that, when applied for 1 second, gives a
1-kilogram mass a velocity of 1 metre per second.
** The amount of heat required to raise the temperature of one gram of water from 14.50C to 15.50C.
Note that the other units are per particle and must be multiplied by 6.022 1023 to be strictly
comparable.
*
140
APPENDIX VII
STANDARD POTENTIALS AT 298 K IN ELECTROCHEMICAL
Reduction half-reaction
E J /V
Reduction half-reaction
H4XeO6 + 2H+ + 2e XeO3 + 3H2O
+3.0
Pu4+ + e Pu3+
+0.97
F2 + 2e 2F
+2.87
NO3 + 4H+ + 3e NO + 2H2O
+0.96
O3 + 2H+ + 2e O2 + H2O
+2.07
2Hg2+ + 2e Hg 2+
2
+0.92
S2O8 + 2e 2SO4
+2.05
ClO + H2O + 2e Cl + 2OH
+0.89
Ag+ + e Ag+
+1.98
Hg2+ + 2e Hg
+0.86
Co3+ + e Co2+
+1.81
NO3 + 2H+ + e NO2 + H2O
+0.80
H2O2 + 2H+ + 2e 2H2O
+1.78
Ag+ + e Ag
+0.80
Au+ + e Au
+1.69
Hg 2+
2 +2e 2Hg
+0.79
Pb4+ + 2e Pb2+
+1.67
Fe3+ + e Fe2+
+0.77
2HClO + 2H+ + 2e Cl2 + 2H2O
+1.63
BrO + H2O + 2e Br + 2OH
+0.76
Ce4+ + e Ce3+
+1.61
Hg2SO4 +2e 2Hg + SO42
+0.62
2HBrO + 2H+ + 2e Br2 + 2H2O
+1.60
MnO42 + 2H2O + 2e MnO2 + 4OH +0.60
MnO4 + 8H+ + 5e Mn2+ + 4H2O
+1.51
MnO4 + e MnO42
+0.56
Mn3+ + e Mn2+
+1.51
I2 + 2e 2I
+0.54
Au3+ + 3e Au
+1.40
I3 + 2e 3I
+0.53
Cl2 + 2e 2Cl
+1.36
Cu+ + e Cu
+0.52
Cr2O 7 + 14H+ + 6e 2Cr3+ + 7H2O
+1.33
NiOOH + H2O + e Ni(OH)2 + OH +0.49
O3 + H2O + 2e O2 + 2OH
+1.24
Ag2CrO4 + 2e 2Ag + CrO42
+0.45
O2 + 4H+ + 4e 2H2O
+1.23
O2 + 2H2O + 4e 4OH
+0.40
ClO4 + 2H+ +2e ClO3 + 2H2O
+1.23
ClO4 + H2O + 2e ClO3 + 2OH
+0.36
MnO2 + 4H+ + 2e Mn2+ + 2H2O
+1.23
[Fe(CN)6]3 + e [Fe(CN)6]4
+0.36
Pt2+ + 2e Pt
+1.20
Cu2+ + 2e Cu
+0.34
Br2 + 2e 2Br
+1.09
Hg2Cl2 + 2e 2Hg + 2Cl
+0.27
E J /V
141

AgCl + e Ag + Cl
+0.27
S + 2e S2
0.48
Bi3+ + 3e Bi
+0.20
In3+ + e In2+
0.49
SO42 + 4H+ + 2e H2SO3 + H2O
+0.17
U4+ + e U3+
0.61
Cu2+ + e Cu+
+0.16
Cr3+ + 3e Cr
0.74
Sn4+ + 2e Sn2+
+0.15
Zn2+ + 2e Zn
0.76
AgBr + e Ag + Br
+0.07
Cd(OH)2 + 2e Cd + 2OH
0.81
Ti4+ + e Ti3+
0.00
2H2O + 2e H2 + 2OH
0.83
2H+ + 2e H2
(by definition) 0.0
Cr2+ + 2e Cr
0.91
Fe3+ + 3e Fe
0.04
Mn2+ + 2e Mn
1.18
O2 + H2O + 2e HO2 + OH
0.08
V2+ + 2e V
1.19
Pb2+ + 2e Pb
0.13
Ti2+ + 2e Ti
1.63
In+ + e In
0.14
Al3+ + 3e Al
1.66
Sn2+ + 2e Sn
0.14
U3+ + 3e U
1.79
AgI + e Ag + I
0.15
Sc3+ + 3e Sc
2.09
Ni2+ + 2e Ni
0.23
Mg2+ + 2e Mg
2.36
V3+ + e V2+
0.26
Ce3+ + 3e Ce
2.48
Co2+ + 2e Co
0.28
La3+ + 3e La
2.52
In3+ + 3e In
0.34
Na+ + e Na
2.71
Tl+ + e Tl
0.34
Ca2+ + 2e Ca
2.87
PbSO4 + 2e Pb + SO2
4
0.36
Sr2+ + 2e Sr
2.89
Ti3+ + e Ti2+
0.37
Ba2+ + 2e Ba
2.91
Cd2+ + 2e Cd
0.40
Ra2+ + 2e Ra
2.92
In2+ + e In+
0.40
Cs+ + e Cs
2.92
Cr3+ + e Cr2+
0.41
Rb+ + e Rb
2.93
Fe2+ + 2e Fe
0.44
K+ +e K
2.93
In3+ + 2e In+
0.44
Li+ + e Li
3.05
142
APPENDIX VIII
LOGARITHMS
Sometimes, a numerical expression may involve multiplication, division or rational powers of large
numbers. For such calculations, logarithms are very useful. They help us in making difficult calculations
easy. In Chemistry, logarithm values are required in solving problems of chemical kinetics, thermodynamics,
electrochemistry, etc. We shall first introduce this concept, and discuss the laws, which will have to be
followed in working with logarithms, and then apply this technique to a number of problems to show
how it makes difficult calculations simple.
We know that
23 = 8, 32 = 9, 53 = 125, 70 = 1
In general, for a positive real number a, and a rational number m, let am = b,
where b is a real number. In other words
the mth power of base a is b.
Another way of stating the same fact is
logarithm of b to base a is m.
If for a positive real number a, a 1
am = b,
we say that m is the logarithm of b to the base a.
b
We write this as lo g a = m ,
log being the abbreviation of the word logarithm.
Thus, we have
log 2 8 = 3,
Since 2
log 3 9 = 2,
Since 3
log
125
= 3,
=8
=9
= 125
=1
Since 5
5
log 7 1 = 0,
Since 7
Laws of Logarithms
In the following discussion, we shall take logarithms to any base a, (a > 0 and a 1)
First Law: loga (mn) = logam + logan
Proof: Suppose that logam = x and logan = y
Then ax= m, ay = n
Hence mn = ax.ay = ax+y
It now follows from the definition of logarithms that
loga (mn) = x + y = loga m loga n
m
= loga m logan
n
Second Law: loga
Proof: Let logam = x, logan = y
143

Then ax = m, ay = n
Hence
a
a
=a
xy
Therefore
log a
m

n
= x y = log a m log a n
Third Law :
loga(mn) = n logam
Proof : As before, if logam = x, then ax = m
Then
( )
= a
x n
=a
nx
giving loga(mn) = nx = n loga m

Thus according to First Law: the log of the product of two numbers is equal to the sum of their logs.
Similarly, the Second Law says: the log of the ratio of two numbers is the difference of their logs. Thus,
the use of these laws converts a problem of multiplication / division into a problem of addition/
subtraction, which are far easier to perform than multiplication/division. That is why logarithms are so
useful in all numerical computations.
Logarithms to Base 10
Because number 10 is the base of writing numbers, it is very convenient to use logarithms to the base
10. Some examples are:
log10 10 = 1,
since 101 = 10
log10 100 = 2,
since 102 = 100
log10 10000 = 4,
since 104 = 10000
log10 0.01 = 2,
since 102 = 0.01
log10 0.001 = 3,
since 103 =
and log101 = 0
0.001
since 10 = 1
The above results indicate that if n is an integral power of 10, i.e., 1 followed by several zeros or
1 preceded by several zeros immediately to the right of the decimal point, then log n can be easily found.
If n is not an integral power of 10, then it is not easy to calculate log n. But mathematicians have
made tables from which we can read off approximate value of the logarithm of any positive number
between 1 and 10. And these are sufficient for us to calculate the logarithm of any number expressed
in decimal form. For this purpose, we always express the given decimal as the product of an integral
power of 10 and a number between 1 and 10.
Standard Form of Decimal

We can express any number in decimal form, as the product of (i) an integral power of 10, and (ii) a
number between 1 and 10. Here are some examples:
(i) 25.2 lies between 10 and 100
144
APPENDIX VIII
25.2
25.2 =
10 = 2.52 10
10
(ii) 1038.4 lies between 1000 and 10000.
1038.4
1038.4
10
1.0384
10
1000
(iii) 0.005 lies between 0.001 and 0.01

0.005 = (0.005 1000) 103 = 5.0 103
(iv) 0.00025 lies between 0.0001 and 0.001
0.00025 = (0.00025 10000) 104 = 2.5 104
In each case, we divide or multiply the decimal by a power of 10, to bring one non-zero digit to the left
of the decimal point, and do the reverse operation by the same power of 10, indicated separately.
Thus, any positive decimal can be written in the form
p
n = m 10
where p is an integer (positive, zero or negative) and 1< m < 10. This is called the standard form of n.
Working Rule
1. Move the decimal point to the left, or to the right, as may be necessary, to bring one non-zero digit
to the left of decimal point.
2.
(i) If you move p places to the left, multiply by 10p.

(ii) If you move p places to the right, multiply by 10p.
(iii) If you do not move the decimal point at all, multiply by 100.
(iv) Write the new decimal obtained by the power of 10 (of step 2) to obtain the standard form of
the given decimal.
Characteristic and Mantissa

Consider the standard form of n
p
n = m 10 , where 1 < m < 10
Taking logarithms to the base 10 and using the laws of logarithms

log n = log m + log 10
= log m + p log 10
= p + log m
Here p is an integer and as 1 < m < 10, so 0 < log m < 1, i.e., m lies between 0 and 1. When log
n has been expressed as p + log m, where p is an integer and 0 log m < 1, we say that p is the
characteristic of log n and that log m is the mantissa of log n. Note that characteristic is always an
integer positive, negative or zero, and mantissa is never negative and is always less than 1. If we can
find the characteristics and the mantissa of log n, we have to just add them to get log n.
Thus to find log n, all we have to do is as follows:
1. Put n in the standard form, say
p
n = m 10 , 1 < m <10
145

2. Read off the characteristic p of log n from this expression (exponent of 10).
3. Look up log m from tables, which is being explained below.
4. Write log n = p + log m
If the characteristic p of a number n is say, 2 and the mantissa is .4133, then we have log n
= 2+ .4133 which we can write as 2.4133. If, however, the characteristic p of a number m is say 2 and
the mantissa is .4123, then we have log m = 2 + .4123. We cannot write this as 2.4123. (Why?) In order
to avoid this confusion we write 2 for 2 and thus we write log m = 2.41 23 .
Now let us explain how to use the table of logarithms to find mantissas. A table is appended at the
end of this Appendix.
Observe that in the table, every row starts with a two digit number, 10, 11, 12,... 97, 98, 99. Every
column is headed by a one-digit number, 0, 1, 2, ...9. On the right, we have the section called Mean
differences which has 9 columns headed by 1, 2...9.
0
..
61
62
63
..
..
7853
7924
7993
..
..
..
7860 7868
7931 7935
8000 8007
..
..
..
7875
7945
8014
..
..
..
7882 7889
7954 7959
8021 8028
..
..
..
7896
7966
8035
..
..
..
7803 7810
7973 7980
8041 8048
..
..
..
7817
7987
8055
..
..
1
1
1
..
..
1
1
1
..
..
2
2
2
..
..
3
3
3
..
..
4
3
3
..
..
4
4
4
..
..
5
5
5
..
..
6
6
6
..
..
6
6
6
..
Now suppose we wish to find log (6.234). Then look into the row starting with 62. In this row, look
at the number in the column headed by 3. The number is 7945. This means that
log (6.230) = 0.7945*
But we want log (6.234). So our answer will be a little more than 0.7945. How much more? We look
this up in the section on Mean differences. Since our fourth digit is 4, look under the column headed
by 4 in the Mean difference section (in the row 62). We see the number 3 there. So add 3 to 7945. We
get 7948. So we finally have
log (6.234) = 0.7948.
Take another example. To find log (8.127), we look in the row 81 under column 2, and we find 9096.
We continue in the same row and see that the mean difference under 7 is 4. Adding this to 9096, and
we get 9100. So, log (8.127) = 0.9100.
Finding N when log N is given

We have so far discussed the procedure for finding log n when a positive number n given. We now turn
to its converse i.e., to find n when log n is given and give a method for this purpose. If log n = t, we
sometimes say n = antilog t. Therefore our task is given t, find its antilog. For this, we use the readymade antilog tables.
Suppose log n = 2.5372.
To find n, first take just the mantissa of log n. In this case it is .5372. (Make sure it is positive.)
Now take up antilog of this number in the antilog table which is to be used exactly like the log table.
* It should, however, be noted that the values given in the table are not exact. They are only approximate values,
although we use the sign of equality which may give the impression that they are exact values. The same
convention will be followed in respect of antilogarithm of a number.
146
APPENDIX VIII
In the antilog table, the entry under column 7 in the row .53 is 3443 and the mean difference for the
last digit 2 in that row is 2, so the table gives 3445. Hence,
antilog (.5372) = 3.445
Now since log n = 2.5372, the characteristic of log n is 2. So the standard form of n is given by
n = 3.445 10
or n = 344.5
Illustration 1
If log x = 1.0712, find x.
Solution: We find that the number corresponding to 0712 is 1179. Since characteristic of log x is 1, we
have
x = 1.179 101
= 11.79
Illustration 2
If log x = 2.1352, find x.
Solution: From antilog tables, we find that the number corresponding to 1352 is 1366. Since the
characteristic is 2 i.e., 2, so
2
x = 1.366 10 = 0.01366
Use of Logarithms in Numerical Calculations

Illustration 1
Find 6.3 1.29
Solution: Let x = 6.3 1.29
Then log x = log (6.3 1.29) = log 6.3 + log 1.29
Now,
log 6.3 = 0.7993
log 1.29 = 0.1106
log x = 0.9099,
Taking antilog
x = 8.127
Illustration 2
1.5
Find
(1.23)
11.2 23.5
3
Solution: Let x =
(1.23) 2
11.2 23.5
147

3
Then log x = log
3
2
3
2
(1.23) 2
11.2 23.5
log 1.23 log (11.2 23.5)
log 1.23 log 11.2 23.5
Now,
log 1.23 = 0.0899
3
2
log 1.23 = 0.13485
log 11.2 = 1.0492

log 23.5 = 1.3711
log x = 0.13485 1.0492 1.3711
= 3.71455
x = 0.005183
Illustration 3
5
Find
(71.24) 56
7
(2.3) 21
5
(71.24) 56
Solution: Let x =
(2.3) 21
(71.24)5 56
Then log x =
log
7
2
(2.3) 21
1
[log (71.24)5 + log
2
5
2
log 71.24 +
1
4
log 56
56 log (2.3) log 21]

7
2
log 2.3
1
4
log 21
Now, using log tables

log 71.24 = 1.8527
log 56 = 1.7482
log 2.3 = 0.3617
log 21 = 1.3222
log x =
5
2
log (1.8527) +
= 3.4723
x = 2967
148
1
4
(1.7482)
7
2
(0.3617)
1
4
(1.3222)
LOGARITHMS
Table 1
N
10
0000 0043
0086
0128
0170
11
0414 0453
0492
0531
0569
12
13
14
15
16
17
18
19
0792 0828
1139 1173
1461 1492
1761 1790
2041 2068
2304 2330
2553 2577
2788 2810
0864
1206
1523
1818
2095
2355
2601
2833
0899
1239
1553
1847
2122
2380
2625
2856
9
8
13
12
17
16
21 26
2O 24
30
28
34 38
32 36
0212
0253 0294 0334
0374
5
4
0607
0645 0682 0719
0755
4
4
8
7
12
11
16
15
20
18
23
22
27
26
31 35
29 33
0969
1004 1038 1072 1106
3
3
7
7
11
10
14
14
18
17
21
20
25
24
28 32
27 31
1303
1335 1367 1399
1430
3
3
6
7
10
10
13
13
16
16
19
19
23
22
26 29
25 29
1614
1644 1673 1703 1732
3
3
6
6
9
9
12
12
15
14
19
17
22
20
25 28
23 26
1903
1931 1959 1987 2014
3
3
6
6
9
8
11
11
14
14
17
17
20
19
23 26
22 25
2175
2201 2227 2253
2279
3
3
6
5
8
8
11
10
14 16
13 16
19
18
22 24
21 23
2430
2455 2480 2504 2529
3
3
5
5
8
8
10
10
13
12
15
15
18
17
20 23
20 22
2672
2695 2718 2742
2765
2
2
5
4
7
7
9
9
12 14
11 14
17
16
19 21
18 21
2900
2923 2945 2967 2989
2
2
4
4
7
6
9
8
11
11
13
13
16
15
18 20
17 19
0934
1271
1584
1875
2148
2405
2648
2878
20
21
22
23
24
25
26
27
28
29
3010
3222
3424
3617
3802
3979
4150
4314
4472
4624
3032
3243
3444
3636
3820
3997
4166
4330
4487
4639
3054
3263
3464
3655
3838
4014
4183
4346
4502
4654
3075
3284
3483
3674
3856
4031
4200
4362
4518
4669
3096
3304
3502
3692
3874
4048
4216
4378
4533
4683
3118
3324
3522
3711
3892
4065
4232
4393
4548
4698
3139
3345
3541
3729
3909
4082
4249
4409
4564
4713
3160
3365
3560
3747
3927
4099
4265
4425
4579
4728
3181
3385
3579
3766
3945
4116
4281
4440
4594
4742
3201
3404
3598
3784
3962
4133
4298
4456
4609
4757
2
2
2
2
2
2
2
2
2
1
4
4
4
4
4
3
3
3
3
3
6
6
6
6
5
5
5
5
5
4
8
8
8
7
7
7
7
6
6
6
11
10
10
9
9
9
8
8
8
7
13
12
12
11
11
10
10
9
9
9
15
14
14
13
12
12
11
11
11
10
17
16
15
15
14
14
13
13
12
12
19
18
17
17
16
15
15
14
14
13
30
31
32
33
34
4771
4914
5051
5185
5315
4786
4928
5065
5198
5328
4800
4942
5079
5211
5340
4814
4955
5092
5224
5353
4829
4969
5105
5237
5366
4843
4983
5119
5250
5378
4857
4997
5132
5263
5391
4871
5011
5145
5276
5403
4886
5024
5159
5289
5416
4900
5038
5172
5302
5428
1
1
1
1
1
3
3
3
3
3
4
4
4
4
4
6
6
5
5
5
7
7
7
6
6
9
8
8
8
8
10
10
9
9
9
11
11
11
10
10
13
12
12
12
11
35
36
37
38
39
5441
5563
5682
5798
5911
5453
5575
5694
5809
5922
5465
5587
5705
5821
5933
5478
5599
5717
5832
5944
5490
5611
5729
5843
5955
5502
5623
5740
5855
5966
5514
5635
5752
5866
5977
5527
5647
5763
5877
5988
5539 5551
5658 5670
5775 5786
5888 5899
5999 6010
1
1
1
1
1
2
2
2
2
2
4
4
3
3
3
5
5
5
5
4
6
6
6
6
5
7
7
7
7
7
9
8
8
8
8
10
10
9
9
9
11
11
10
10
10
40
41
42
43
44
6021
6128
6232
6335
6435
6031
6138
6243
6345
6444
6042
6149
6253
6355
6454
6053
6160
6263
6365
6464
6064
6170
6274
6375
6474
6075
6180
6284
6385
6484
6085
6191
6294
6395
6493
6096
6201
6304
6405
6503
6107
6212
6314
6415
6513
6117
6222
6325
6425
6522
1
1
1
1
1
2
2
2
2
2
3
3
3
3
3
4
4
4
4
4
5
5
5
5
5
6
6
6
6
6
8
7
7
7
7
9 10
8
9
8
9
8
9
8
9
45
46
47
48
49
6532
6628
6721
6812
6902
6542
6637
6730
6821
6911
6551
6646
6739
6830
6920
6561
6656
6749
6839
6928
6471
6665
6758
6848
6937
6580
6675
6767
6857
6946
6590
6684
6776
6866
6955
6599
6693
6785
6875
6964
6609
6702
6794
6884
6972
6618
6712
6803
6893
6981
1
1
1
1
1
2
2
2
2
2
3
3
3
3
3
4
4
4
4
4
5
5
5
4
4
6
6
5
5
5
7
7
6
6
6
8
7
7
7
7
9
8
8
8
8
149
LOGARITHMS
Table 1 continued
150
50
51
52
53
54
6990
7076
7160
7243
7324
6998
7084
7168
7251
7332
7007
7093
7177
7259
7340
7016
7101
7185
7267
7348
7024
7110
7193
7275
7356
7033
7118
7202
7284
7364
7042
7126
7210
7292
7372
7050
7135
7218
7300
7380
7059
7143
7226
7308
7388
7067
7152
7235
7316
7396
1
1
1
1
1
2
2
2
2
2
3
3
2
2
2
3
3
3
3
3
4
4
4
4
4
5
5
5
5
5
6
6
6
6
6
7
7
7
6
6
8
8
7
7
7
55
56
57
58
59
7404
7482
7559
7634
7709
7412
7490
7566
7642
7716
7419
7497
7574
7649
7723
7427
7505
7582
7657
7731
7435
7513
7589
7664
7738
7443
7520
7597
7672
7745
7451
7528
7604
7679
7752
7459
7536
7612
7686
7760
7466
7543
7619
7694
7767
7474
7551
7627
7701
7774
1
1
1
1
1
2
2
2
1
1
2
2
2
2
2
3
3
3
3
3
4
4
4
4
4
5
5
5
4
4
5
5
5
5
5
6
6
6
6
6
7
7
7
7
7
60
61
62
63
64
7782
7853
7924
7993
8062
7789
7860
7931
8000
8069
7796
7768
7938
8007
8075
7803
7875
7945
8014
8082
7810
7882
7952
8021
8089
7818
7889
7959
8028
8096
7825
7896
7966
8035
8102
7832
7903
7973
8041
8109
7839
7910
7980
8048
8116
7846
7917
7987
8055
8122
1
1
1
1
1
1
1
1
1
1
2
2
2
2
2
3
3
3
3
3
4
4
3
3
3
4
4
4
4
4
5
5
5
5
5
6
6
6
5
5
6
6
6
6
6
65
66
67
68
69
8129
8195
8261
8325
8388
8136
8202
8267
8331
8395
8142
8209
8274
8338
8401
8149
8215
8280
8344
8407
8156
8222
8287
8351
8414
8162
8228
8293
8357
8420
8169
8235
8299
8363
8426
8176
8241
8306
8370
8432
8182
8248
8312
8376
8439
8189
8254
8319
8382
8445
1
1
1
1
1
1
1
1
1
1
2
2
2
2
2
3
3
3
3
2
3
3
3
3
3
4
4
4
4
4
5
5
5
4
4
5
5
5
5
5
6
6
6
6
6
70
71
72
73
74
8451
8513
8573
8633
8692
8457
8519
8579
8639
8698
8463
8525
8585
8645
8704
8470
8531
8591
8651
8710
8476
8537
8597
8657
8716
8482
8543
8603
8663
8722
8488
8549
8609
8669
8727
8494
8555
8615
8675
8733
8500
8561
8621
8681
8739
8506
8567
8627
8686
8745
1
1
1
1
1
1
1
1
1
1
2
2
2
2
2
2
2
2
2
2
3
3
3
3
3
4
4
4
4
4
4
4
4
4
4
5
5
5
5
5
6
5
5
5
5
75
76
77
78
79
8751
8808
8865
8921
8976
8756
8814
8871
8927
8982
8762
8820
8876
8932
8987
8768
8825
8882
8938
8993
8774
8831
8887
8943
8998
8779
8837
8893
8949
9004
8785
8842
8899
8954
9009
8791
8848
8904
8960
9015
8797
8854
8910
8965
9020
8802
8859
8915
8971
9025
1
1
1
1
1
1
1
1
1
1
2
2
2
2
2
2
2
2
2
2
3
3
3
3
3
3
3
3
3
3
4
4
4
4
4
5
5
4
4
4
5
5
5
5
5
80
81
82
83
84
9031
9085
9138
9191
9243
9036
9090
9143
9196
9248
9042
9096
9149
9201
9253
9047
9101
9154
9206
9258
9053
9106
9159
9212
9263
9058
9112
9165
9217
9269
9063
9117
9170
9222
9274
9069
9122
9175
9227
9279
9074
9128
9180
9232
9284
9079
9133
9186
9238
9289
1
1
1
1
1
1
1
1
1
1
2
2
2
2
2
2
2
2
2
2
3
3
3
3
3
3
3
3
3
3
4
4
4
4
4
4
4
4
4
4
5
5
5
5
5
85
86
87
88
89
9294
9345
9395
9445
9494
9299
9350
9400
9450
9499
9304
9355
9405
9455
9504
9309
9360
9410
9460
9509
9315
9365
9415
9465
9513
9320
9370
9420
9469
9518
9325
9375
9425
9474
9523
9330
9380
9430
9479
9528
9335
9385
9435
9484
9533
9340
9390
9440
9489
9538
1
1
0
0
0
1
1
1
1
1
2
2
1
1
1
2
2
2
2
2
3
3
2
2
2
3
3
3
3
3
4
4
3
3
3
4
4
4
4
4
5
5
4
4
4
90
91
92
93
94
9542
9590
9638
9685
9731
9547
9595
9643
9689
9736
9552
9600
9647
9694
9741
9557
9605
9652
9699
9745
9562
9609
9657
9703
9750
9566
9614
9661
9708
9754
9571
9619
9666
9713
9759
9576
9624
9671
9717
9763
9581
9628
9675
9722
9768
9586
9633
9680
9727
9773
0
0
0
0
0
1
1
1
1
1
1
1
1
1
1
2
2
2
2
2
2
2
2
2
2
3
3
3
3
3
3
3
3
3
3
4
4
4
4
4
4
4
4
4
4
95
96
97
98
99
9777
9823
9868
9912
9956
9782
9827
9872
9917
9961
9786
9832
9877
9921
9965
9791
9836
9881
9926
9969
9795
9841
9886
9930
9974
9800
9845
9890
9934
9978
9805
9850
9894
9939
9983
9809
9854
9899
9943
9987
9814
9859
9903
9948
9997
9818
9863
9908
9952
9996
0
0
0
0
0
1
1
1
1
1
1
1
1
1
1
2
2
2
2
2
2
2
2
2
2
3
3
3
3
3
3
3
3
3
3
4
4
4
4
3
4
4
4
4
4
ANTILOGARITHMS
Table 2
N
00
.01
.02
.03
.04
.05
.06
.07
.08
.09
1000
1023
1047
1072
1096
1122
1148
1175
1202
1230
1002
1026
1050
1074
1099
1125
1151
1178
1205
1233
1005
1028
1052
1076
1102
1127
1153
1180
1208
1236
1007
1030
1054
1079
1104
1130
1156
1183
1211
1239
1009
1033
1057
1081
1107
1132
1159
1186
1213
1242
1012
1035
1059
1084
1109
1135
1161
1189
1216
1245
1014
1038
1062
1086
1112
1138
1164
1191
1219
1247
1016
1040
1064
1089
1114
1140
1167
1194
1222
1250
1019
1042
1067
1091
1117
1143
1169
1197
1225
1253
1021
1045
1069
1094
1119
1146
1172
1199
1227
1256
0
0
0
0
0
0
0
0
0
0
0
0
0
0
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
3
3
.10
.11
.12
.13
.14
.15
.16
.17
.18
.19
1259
1288
1318
1349
1380
1413
1445
1479
1514
1549
1262
1291
1321
1352
1384
1416
1449
1483
1517
1552
1265
1294
1324
1355
1387
1419
1452
1486
1521
1556
1268
1297
1327
1358
1390
1422
1455
1489
1524
1560
1271
1300
1330
1361
1393
1426
1459
1493
1528
1563
1274
1303
1334
1365
1396
1429
1462
1496
1531
1567
1276
1306
1337
1368
1400
1432
1466
1500
1535
1570
1279
1309
1340
1371
1403
1435
1469
1503
1538
1574
1282
1312
1343
1374
1406
1439
1472
1507
1542
1578
1285
1315
1346
1377
1409
1442
1476
1510
1545
1581
0
0
0
0
0
0
0
0
0
0
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
3
2
2
2
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
.20
.21
.22
.23
.24
1585
1622
1660
1698
1738
1589
1626
1663
1702
1742
1592
1629
1667
1706
1746
1596
1633
1671
1710
1750
1600
1637
1675
1714
1754
1603
1641
1679
1718
1758
1607
1644
1683
1722
1762
1611
1648
1687
1726
1766
1614
1652
1690
1730
1770
1618
1656
1694
1734
1774
0
0
0
0
0
1
1
1
1
1
1
1
1
1
1
1
2
2
2
2
2
2
2
2
2
2
2
2
2
2
3
3
3
3
3
3
3
3
3
3
3
3
3
4
4
.25
.26
.27
.28
.29
1778
1820
1862
1905
1950
1782
1824
1866
1910
1954
1786
1828
1871
1914
1959
1791
1832
1875
1919
1963
1795
1837
1879
1923
1968
1799
1841
1884
1928
1972
1803
1845
1888
1932
1977
1807
1849
1892
1936
1982
1811
1854
1897
1941
1986
1816
1858
1901
1945
1991
0
0
0
0
0
1
1
1
1
1
1
1
1
1
1
2
2
2
2
2
2
2
2
2
2
2
3
3
3
3
3
3
3
3
3
3
3
3
4
4
4
4
4
4
4
.30
.31
.32
.33
.34
.35
.36
.37
.38
.39
1995
2042
2089
2138
2188
2239
2291
2344
2399
2455
2000
2046
2094
2143
2193
2244
2296
2350
2404
2460
2004
2051
2099
2148
2198
2249
2301
2355
2410
2466
2009
2056
2104
2153
2203
2254
2307
2360
2415
2472
2014
2061
2109
2158
2208
2259
2312
2366
2421
2477
2018
2065
2113
2163
2213
2265
2317
2371
2427
2483
2023
2070
2118
2168
2218
2270
2323
2377
2432
2489
2028
2075
2123
2173
2223
2275
2328
2382
2438
2495
2032
2080
2128
2178
2228
2280
2333
2388
2443
2500
2037
2084
2133
2183
2234
2286
2339
2393
2449
2506
0
0
0
0
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
4
4
4
4
4
4
4
4
4
4
4
4
4
4
4
5
4
4
4
4
5
5
5
5
5
5
.40
.41
.42
.43
.44
.45
.46
.47
.48
2512
2570
2630
2692
2754
2818
2884
2951
3020
2518
2576
2636
2698
2761
2825
2891
2958
3027
2523
2582
2642
2704
2767
2831
2897
2965
3034
2529
2588
2649
2710
2773
2838
2904
2972
3041
2535
2594
2655
2716
2780
2844
2911
2979
3048
2541
2600
2661
2723
2786
2851
2917
2985
3055
2547
2606
2667
2729
2793
2858
2924
2992
3062
2553
2612
2673
2735
2799
2864
2931
2999
3069
2559
2618
2679
2742
2805
2871
2938
3006
3076
2564
2624
2685
2748
2812
2877
2944
3013
3083
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
2
2
2
2
2
2
2
2
2
2
2
2
3
3
3
3
3
3
3
3
3
3
3
3
3
3
3
4
4
4
4
4
4
4
4
4
4
4
4
4
4
5
5
5
5
5
5
5
5
5
5
5
5
6
5
5
6
6
6
6
6
6
6
.49
3090 3097
3105
3112
3119
3126
3133 3141 3148 3155
151
ANTILOGARITHMS
Table 2 continued
152
.50
.51
.52
.53
.54
.55
.56
3162
3236
3311
3388
3467
3548
3631
3170
3243
3319
3396
3475
3556
3639
3177
3251
3327
3404
3483
3565
3648
3184
3258
3334
3412
3491
3573
3656
3192
3266
3342
3420
3499
3581
3664
3199
3273
3350
3428
3508
3589
3673
3206
3281
3357
3436
3516
3597
3681
3214
3289
3365
3443
3524
3606
3690
3221
3296
3373
3451
3532
3614
3698
3228
3304
3381
3459
3540
3622
3707
1
1
1
1
1
1
1
1
2
2
2
2
2
2
2
2
2
2
2
2
3
3
3
3
3
3
3
3
4
4
4
4
4
4
4
4
5
5
5
5
5
5
5
5
5
6
6
6
6
6
6
6
6
6
7
7
7
7
7
7
7
7
8
.57
.58
.59
3715 3724
3802 3811
3890 3899
3733
3819
3908
3741
3828
3917
3750
3837
3926
3758
3846
3936
3767 3776 3784 3793

3855 3864 3873 3882
3945 3954 3963 3972
1
1
1
2
2
2
3
3
3
3
4
4
4
4
5
5
5
5
6
6
6
7
7
7
8
8
8
.60
.61
.62
.63
.64
.65
.66
.67
.68
.69
3981
4074
4169
4266
4365
4467
4571
4677
4786
4898
3990
4083
4178
4276
4375
4477
4581
4688
4797
4909
3999
4093
4188
4285
4385
4487
4592
4699
4808
4920
4009
4102
4198
4295
4395
4498
4603
4710
4819
4932
4018
4111
4207
4305
4406
4508
4613
4721
4831
4943
4027
4121
4217
4315
4416
4519
4624
4732
4842
4955
4036
4130
4227
4325
4426
4529
4634
4742
4853
4966
4046
4140
4236
4335
4436
4539
4645
4753
4864
4977
4055
4150
4246
4345
4446
4550
4656
4764
4875
4989
4064
4159
42S6
4355
4457
4560
4667
4775
4887
5000
1
1
1
1
1
1
1
1
1
1
2
2
2
2
2
2
2
2
2
2
3
3
3
3
3
3
3
3
3
3
4
4
4
4
4
4
4
4
4
5
5
5
5
5
5
5
5
5
6
6
6
6
6
6
6
6
6
7
7
7
6
7
7
7
7
7
7
8
8
8
7
8
8
8
8
8
9
9
9
9
8
9
9
9
9
9
10
10
10
10
.70 5012 5023

.71 5129 5140
.72 5248 5260
.73 5370 5383
.74 5495 5508
.75 5623 5636
.76 5754 5768
.77 5888 5902
.78 6026 6039
.79 6166 6180
5035
5152
5272
5395
5521
5649
5781
5916
6053
6194
5047
5164
5284
5408
5534
5662
5794
5929
6067
6209
5058
5176
5297
5420
5546
5675
5808
5943
6081
6223
5070
5188
5309
5433
5559
5689
5821
5957
6095
6237
5082
5200
5321
5445
5572
5702
5834
5970
6109
6252
5093
5212
5333
5458
5585
5715
5848
5984
6124
6266
5105
5224
5346
5470
5598
5728
5861
5998
6138
6281
5117
5236
5358
5483
5610
5741
5875
6012
6152
6295
1
1
1
1
1
1
1
1
1
1
2
2
2
3
3
3
3
3
3
3
4
4
4
4
4
4
4
4
4
4
5
5
5
5
5
5
5
5
6
6
6
6
6
6
6
7
7
7
7
7
7
7
7
8
8
8
8
8
8
9
8
8
9
9
9
9
9
10
10
10
9
10
10
10
10
10
11
11
11
11
11
11
11
11
12
12
12
12
13
13
.80
.81
.82
.83
.84
6310
6457
6607
6761
6918
6324
6471
6622
6776
6934
6339
6486
6637
6792
6950
6353
6501
6653
6808
6966
6368
6516
6668
6823
6982
6383
6531
6683
6839
6998
6397
6546
6699
6855
7015
6412
6561
6714
6871
7031
6427
6577
6730
6887
7047
6442
6592
6745
6902
7063
1
2
2
2
2
3
3
3
3
3
4
5
5
5
5
6
6
6
6
6
7
8
8
8
8
9
9
9
9
10
10
11
11
11
11
12 13
12 14
12 14
1314
13 15
.85
.86
.87
.88
.89
7079
7244
7413
7586
7762
7096
7261
7430
7603
7780
7112
7278
7447
7621
7798
7129
7295
7464
7638
7816
7145
7311
7482
7656
7834
7161
7328
7499
7674
7852
7178
7345
7516
7691
7870
7194
7362
7534
7709
7889
7211
7379
7551
7727
7907
7228
7396
7568
7745
7925
2
2
2
2
2
3
3
3
4
4
5
5
5
5
5
7
7
7
7
7
8
8
9
9
9
10
10
10
11
11
12
12
12
12
13
13
13
14
14
14
15
15
16
16
16
.90
.91
.92
.93
.94
7943
8128
8318
8511
8710
7962
8147
8337
8531
8730
7980
8166
8356
8551
8750
7998
8185
8375
8570
8770
8017
8204
8395
8590
8790
8035
8222
8414
8610
8810
8054
8241
8433
8630
8831
8072
8260
8453
8650
8851
8091 8110
8279 8299
8472 8492
8670 8690
8872 8892
2
2
2
2
2
4
4
4
4
4
6
6
6
6
6
7
8
8
8
8
9
9
10
10
10
11
11
12
12
12
13
13
14
14
14
15
15
15
16
16
17
17
17
18
18
.95
.96
.97
.98
.99
8913
9120
9333
9550
9772
8933
9141
9354
9572
9795
8954
9162
9376
9594
9817
8974
9183
9397
9616
9840
8995
9204
9419
9638
9863
9016
9226
9441
9661
9886
9036
9247
9462
9683
9908
9057
9268
9484
9705
9931
9078
9290
9506
9727
9954
2
2
2
2
2
4
4
4
4
5
6
6
7
7
7
8
8
9
9
9
10
11
11
11
11
12
13
13
13
14
15
15
15
16
16
17
17
17
18
18
19
19
20
20
20
9099
9311
9528
9750
9977
PROJECTS
BACKGAROUND INFORMATION
ABOUT INVESTIGATORY PROJECTS
INTRODUCTION
The expansion of scientific knowledge and consequently the change in the system
of education has led to a modification in the methods of instruction. Today the
stress is laid on inquiry approach and discussion method instead of the age-old
lecture method of teaching. A new dimension in the teaching of science has been
added by including the project-work at the higher secondary level. Teaching
through project work is an individualized instructional technique. It provides an
opportunity to the student to define a problem, to plan his/her work, to search
appropriate resources, to carry out his/her plans, and to draw conclusions. This
way, students are exposed to the fundamental scientific principles, methods and
processes and get a first hand knowledge about the various phases involved in a
scientific investigation. Thus the project work helps to: (a) stimulate interest in
science; (b) arouse scientific curiosity; (c) develop independent critical thinking;
(d) provide experience of using various tools and techniques in the field of science
and (e) develop self-confidence. The modern trend in the teaching of science
therefore encourages more project work.
Any kind of investigation; formulated, designed and carried out in the library,
laboratory, in the field, or at home constitutes an investigatory project. A project
may be as simple as collection of samples of minerals and it may be as difficult as
developing an original indigenous process for the production of a chemical. Some
of the projects can be completely theoretical and involve only the library work.
Others may involve the experimental work to be carried out in the laboratory.
The experimental work in science exposes the students to a number of scientific
instruments, tools, techniques and intellectual skills.
SELECTION OF PROJECTS
Projects should usually be selected by the students. The idea of a project originates
from studying a subject in the classroom, reading the reports of various projects,
science news, popular science articles from science journals etc. Sometimes the
idea of a science project may strike during classroom discussion on topics, which
may require testing, quantifying and interpreting. Some of the science journals
for getting the ideas for a project are : (a) Journal of Chemical Education;
(b) Chemistry Education; (c) Education in Chemistry; (d) New Scientist; (e) School
BACKGROUND INFORMATION ABOUT INVESTIGATORY PROJECTS
Science; (f) School Science Review; (g) Science; (h) Scientific

American; (i) School Science Resource Letter, etc. Once the project
work begins, it might provide new titles and ideas.
In spite of the availability of the above listed scientific literature,
it should not be assumed that students can begin the work on
projects spontaneously. Since majority of the science journals listed
above are not available in Indian Schools. Students need the help
and guidance from the teacher. If some student does not get an
idea for the project, the teacher may provide a list of suggested
projected or take the students to science fairs and exhibitions to
show what other students are doing. A format for working on the
projects is given below:
1. Title of Project
2. Objectives and importance of Project
3. A brief outline of work on Project
The title of the project should be written in such a manner that
the objectives and importance of the project is clearly defined. In
other words a project title and its objectives should create an
interest and curiosity. A brief outline of working on a project helps
the student to initiate the work.
It may be debatable that this approach of suggesting ideas for
the projects defeats one of the basic objectives of project work,
namely originality, but providing guidelines to the students is
completely scientific and desirable to encourage every student to
begin and aim at something in the first attempt.
MANAGING TIME
Central Board of Secondary Education has allocated ten periods
for the project work. A student can start the project right in the
beginning of the academic year and can carry it out in phases and
submit the report of the project at the end of the year.
TECHNICAL
AND
ACADEMIC GUIDANCE
This is an important factor in the smooth running of the project

work. The student should plan for the project well in advance and
discuss its design with the teacher. If improvisation of the apparatus
or some instrument is needed or a chemical is not available in the
laboratory. The help of teacher may be taken. If some technical or
academic guidance is required help may be taken not only from
the concerned teacher of chemistry but also from physics from
and other science teachers as well.
117
LABORATORY FACILITIES
The selection of the project should be such that as far as possible,
the material (apparatus, instruments, chemicals, etc.) needed for
the project-work is easily available. Student may purchase the
affordable chemical or an apparatus (improvised or original) if it is
not available in the laboratory, and the student is very curious to
take up the project and wants to do it. The students should be
discouraged from taking highly expensive projects. An effective
project-work requires an integrated approach rather than a subject
specific approach.
The project work in the laboratory requires a bigger and separate
space. Arrangements should be made in such a way that at a given
time all the students are not involved in doing the laboratory work.
Some students should carry out the work of collecting references in
the library while others should design experiments.
Problems may arise in carrying out the long term experiments
like corrosion, fermentation etc. in the laboratory. It is suggested
to have a separate bench in the laboratory, where long term
experiments can be set up. For storing the samples of certain
chemicals and apparatuses relevant to the project-work, cardboard boxes, with students name written on them can be used.
Empty bottles, if available, can also serve the purpose of storing
the chemicals.
RECORDING THE PROJECT WORK

Recording the actual observation in the project work is very
essential. Students should be encouraged to record the negative
results also. A general format for writing the project report is
suggested below. It should involve the following points :
1. Title of project reflecting objectives
2. Principles used for Investigation
3. Apparatus and Chemicals required
4. Improvisation, if any
5. Procedure
6. Observations and Calculations
7. Conclusions and the logic upon which the conclusions are
based
8. Precautions
9. Suggestions for further investigations, if any
To illustrate the format outlined above, a sample project
report is presented in the end. It may further be noted that
sample project report serves merely as a guideline to the
118
students while writing their projects. It is by no means

exhaustive and is open to further improvements. Brief
outline of some projects is given below.
PROJECT 1
Title
To test the contamination of water by bacteria by checking the
sulphide ion concentration and find out the cause of contamination.
Objective
To check the bacterial contamination in samples of water collected
from different sources by determining sulphide ion concentration.
Background Information
Sulphide ions are present in water when anaerobic bacteria
decompose organic matter or reduce sulphates. These are found
in stagnent water. Generally pollutants from paper mills, gas works,
tanneries, sewage works and other chemical plants are responsible
for the growth of such bacteria.
Brief Procedure
Collection of Samples
Sulphides are readily oxidised, therefore care should be taken at
the time of sampling to exclude air by flushing it with nitrogen or
carbon dioxide. But the best way is to fix the sample immediately
after collection. This can be done by adding small volume of
cadmium-zinc acetate solution. For this take 80 mL of water and
add cadmium-zinc acetate solution 20 mL to obtain a total volume
of about 100 mL. To make Cd-Zn acetate solution dissolve 50 g
cadmium acetate and 50 g zinc acetate in 1.0 L of water. If collected
sample is acidic in nature, then first neutralize it with little excess
of alkali.
Titration of Fixed Solution
Take 100 mL fixed solution in a titration flask, add 20 mL 0.025 M
iodine solution and immediately add 15 mL, (1:1) HCl and mix. Titrate
the excess iodine against 0.05 M Na2S2O3, adding starch solution
as indicateor towards the end point. Calculate the amount of
sulphide ions in the original samples from the amount of iodine
used in the reaction with H2S. Subtract the values of blank titration
if available from the calculated values.
119
PROJECT 2
Title
To study the methods of purification of water.
Objectives
To study level of purity achieved by using different methods
of purification.
To study advantages and disadvantages of using different
method for purification.
To know about specific uses of pure water.
Purity of water obtained from different natural sources is different.
The type of contamination and impurity present depends upon
the source from which water is obtained. Besides drinking
purposes, we require pure water for various other purposes e.g.
in chemical analysis. There are various methods for the purification
of water. these remove impurities and contamination to different
extent. There are some advantages and disadvantages in using
these methods. Comparison of various methods of purification will
provide an idea about obtaining water of specific purity for a
specific purpose.
Brief Procedure
Students may find out level of puriety achieved by various
techniques in use, for the purification of drinking water. They can
survey the literature and visit industries etc. to find out uses of
water of specific purity. Students may work in groups for the study
of various aspects of the project.
Note : Another aspect of the project may be to study different methods of
purification of water taken from different sources such as river, well,
bore-well, municipality etc.
PROJECT 3
Title
Testing the hardness, presence of iron, fluoride, chloride etc. in
drinking water obtained from different regions and a study of the
cause of presence of these ions above permissible limits.
120
Objectives
To test the total hardness, iron, fluoride and chloride etc. in
different samples of water.
To collect information about local sources of above ions in
water.
To study the effect of these ions on health if present beyond
permissible limits.
To find out whether any such problem exists in the locality
and around.
Quality of drinking water has direct relationship with the
human health and life. If iron, fluoride, chloride etc. are
present in water above permissible limits, they may cause
several health problems. For example, if fluoride is present
above permissible limit, people of the region may suffer from
fluorosis. Hardness of water is due to the presence of calcium
and magnesium ions. It is well known fact that hard water is
not fit for laundary purposes. Thus, it is very important to
know the ions and their amount present in water.
Brief Procedure
Students may collect samples of water from different sources. They
can detect the presence of different ions by usual methods of
analysis. Total hardness of water can be estimated by standard
procedure of complexometric titration. Estimation of Cl , F and

2+
Fe is difficult at this level. Therefore existing data from approved
labs can be taken for the purpose of investigation.
PROJECT 4
Title
Investigation of the foaming capacity of different washing soaps
and the effect of addition of sodium carbonate on their foaming
capacity.
Objective
To study the foaming capacity of soaps and the effect of addition
of sodium carbonate on their foaming capacity.
121
Brief Procedure
Weigh 1 gram of a sample of soap and dissolve it completely in
100 mL of distilled water. Take 10 mL of the soap solution in a
boiling tube close the mouth of the boiling tube with the help of a
cork and shake the solution making 20 regular strokes so that
foam increases uniformly. Measure the length of the boiling tube
up to which the foam rises. Similarly, perform the experiment with
other soap solutions.
Dissolve 0.5g of sodium carbonate in 50 mL of each of the
above soap solutions separately. Now take 10 mL of a solution in
a boiling tube and shake it equal number of times (e.g. 20 regular
strokes). Measure the length up to which foam appears. Similarly,
perform the experiment with other soap solutions. Record the
observations in a tabular form.
Compare the height upto which foam produced rises in different
soap solutions with and without the presence of Na2CO3 and draw
conclusions.
PROJECT 5
Title
Study of the acidity of different samples of tea leaves and reasons
for the variation in colour of tea prepared from these leaves.
Objective
To estimate the concentration of acids present in different tea
samples and the effect of addition of acids or bases on the colour
of tea extract.
Brief Procedure
(a) Estimation of Concentration of Acids Present in Tea
Weigh 10 grams of the sample of tea leaves and prepare the extract
of each sample separately in 200 mL of distilled water. For this,
boil different samples of tea leaves with distilled water 8 for a fixed
time period.
Take 5mL of tea extract in a conical flask and dilute it with 20
mL of distilled water. Shake the solution well for homogenous
mixing and then titrate it against M/50 NaOH solution using
phenolphathalein as an indicator. Similarly, titrate other tea
122
extracts with M/50 NaOH solution. Calculate the concentration of

acids present in different samples of tea leaves in terms of molarity.
If colour of the extract causes problem, then tea extract can be taken
in the burette and sodium hydroxide solution in the conical flask.
Phenolphthalein may be used as an indicator if sodium hydroxide
solution is taken is conical flask. The colour change will be from
pink to colourless.
(b) Effect of Acids and Bases on the Colour of Tea Extract
Take five filter paper strips and mark them as A, B, C, D and E. Dip
all the strips in any one sample of tea extract and then take them
out. Now put two drops of dilute HC1, acetic acid solution, NaOH
solution and NH4OH solution on strips A, B, C and D respectively.
Compare the change in colour of these strips with reference to the
colour of the strip E. Repeat this experiment with other samples of
tea extract.
PROJECT 6
Title
Study the rates of evaporation of different liquids
Objective
To study the relationship between the rates of evaporation of different
liquids and their chemical constitution.
Brief Procedure
Take five clean and dry weighing tubes and mark them as A, B, C, D
and E. Weigh each weighing tube with its stopper. Now pour 10 mL
of different liquids (ethanol, ether, tetrachloromethane, acetone etc.)
in different weighing tubes. Weigh each weighing tube again and
find the mass of the liquid taken in each weighing tube.
Remove the stoppers of the weighing tubes and keep them at
room temperature for one hour. After exactly one hour, close the
mouth of all the weighing tubes with their stoppers and weigh them
again one by one.
Calculate the loss in mass of each liquid. The temperature and
the surface area should be the same for the evaporation of each
liquid. Determine the rate of evaporation of each liquid in grams of
liquid evaporated per second. Relate the difference in rates of
evaporation of liquids with their chemical constitution and variation
in intermolecular/intra-molecular interactions.
123
PROJECT 7
Title
Study the effect of acids and alkalies on the tensile strength of
fibres
Objective
To study the effect of acids on the tensile strength of different types
of fibers.
Brief Procedure
The tensile strength of a fibre is measured by noting the minimum
weight required just to break the thread. It may be done as follows:
Take a thread of about 20 cm length and tie its one end with a
ring fixed on the iron stand and the other end with a hanger which
carries the weights. Increase the weight on the hanger and find
out the minimum weight required to just break the thread. Repeat
the experiment with threads of equal length and thickness but of
different materials (eg. cotton, wool, silk, terylene etc.). These
weights are the measure of tensile strength of the fibre.
The effect of acids and alkalies on the tensile strength of fibres
can be determined by dipping them separately in dilute HC1 or
dilute NaOH solution of equal strengths for equal intervals of time.
After a small but fixed interval of time, the fibres are removed from
the solution, washed with water and dried. Then minimum weight
required to just break these threads are determined. These weights
are the measures of the tensile strengths of fibres after treatment
with acid or alkali. Interpret your observations in terms of chemical
constitution of the material of fibre.
PROJECT 8
Title
Study of the acids and mineral contents of vegetables and fruits.
Objective
(a)
(b)
124
To determine the amount of acids present in various

vegetables and fruits.
To detect the presence of iron, carbohydrate, protein and
sugar etc. in vegetables and fruits.
Brief Procedure
(a) Acid Content
Take out the juice of a few fruits and vegetables (apple, orange, amla,
lemon, raddish, cane sugar etc.) by crushing them. Keep the juice
samples in different containers. Determine the pH of different samples
of juices. Determine their acid content by titrating a known quantity
of juice with M/100 potassium hydroxide solution using
phenolphthalein as an indicator. In case of dark coloured juices,
dilute them with enough distilled water to get sharp end point during
titration.
Compare the acid contents of juices by comparing their acid
values. Acid value of vegetables and fruits is the number of milligrams
of potassium hydroxide required for neutralizing the acids present
in one gram of vegetable/fruit.
(b) Tests for Iron, Carbohydrate (starch and sugar), Protein
and Fats
Test the vegetables and fruit juices for the presence of iron. Heat the
vegetable juice with concentrated HNO3 for some time and perform
the test for iron. Carbohydrate (starch, sugar), protein and fats can
be tested by the usual tests.
SAMPLE PROJECT REPORT

Title
A study of the variation of viscosity of organic compounds of same
homologous series with variation in the (a) molecular masses and
(b) structures of carbon chains.
Some liquids like honey or Mobil oil flow very slowly while others
like water or kerosene flow rapidly. Liquids that flow slowly are
known as viscous liquids while others that flow rapidly are known
as non-viscous liquids. The resistance offered by a liquid to flow is
known as viscosity. It is related to intermolecular forces existing in a
liquid. Different liquids have different values of viscosity due to the
existence of different magnitudes of intermolecular forces. The
comparison of viscosities of various homologues and isomers in a
particular homologous series would give an idea about the
magnitude of intermolecular forces existing in them.
125
Objectives
The objectives of this project are to establish a relationship between
(a) viscosity and molecular masses; and (b) viscosity and nature of
carbon chain in organic compounds.
Principle Involved
Hazard Warning
Acetone and alcohols are

inflamable, do not let the
bottles open when not in
use.
Keep the bottles away
from flames.
Wash your hands after
use.
Wear safety spectacles.
The resistance to flow offered by a liquid is measured in terms of

coefficient of viscosity which is defined as follows:
Coefficient of viscosity of a liquid at a specified temperature is
the steady force required to maintain a velocity difference of unity
between two parallel layers of a liquid, a unit distance apart and
having a unit area of contact. Coefficient of viscosity is measured
by Ostwald viscometer method. For two liquids whose coefficient
of viscosity are d1 and d2, 1 , 2 the time of flow in seconds are t1
and densities are d1 and respectively d2 then the following relation
holds:
d1 t1
d2 t2
Hence if the viscosity of one liquid is known, the viscosity of

other can be determined.
Material required
Ostwald viscometer, stop-watch, beaker (250 mL), pipette, graduated cylinder, kerosene,
petrol, diesel, methyl alcohol, ethyl alcohol, propyl alcohol, isopropyl alcohol, butyl
alcohol, isobutyl alcohol, tert butyl alcohol and amyl alcohol.
Brief Procedure
The viscometer was washed, rinsed with alcohol and dried.
10 mL of the liquid under investigation was filled in it and the time
required for the flow of liquid between two marks of viscometer was
noted with the help of a stop watch. These observation were recorded
in Tables I and II. The viscosities of various liquids were calculated
by the formula discussed under the heading principles involved.
Observations and Calculations

Room Temperature = 23C.
A viscometer of different capacity was used for alcohols.
126
Table 1 : Data for the time of flow of various compounds

Sl. No.
Time of flow
(seconds)
Name of the compound
Density
(g/mL)
Viscosity
(millipoise)
1.
Water
13.5
10.08
2.
Petrol
8.5
0.8
6.4
3.
Kerosene Oil
22.0
16.4
4.
Dilesel Oil
48.0
18.0
Table 2 : Data for the viscosity vs molecular mass relationship of various compounds
Sl. No.
Name of the compound
Molecular Time of flow Density in Viscosity

mass
(Seconds)
(g/mL)
(millipoise)
1.
Water
18
180
10.08
2.
Methanol
32
136
0.79
7.6
3.
Ethanol
46
258
0.78
14.4
4.
Propan-1-ol
60
391
0.8
21.9
5.
Propan-2-ol
60
546
0.79
30.6
6.
Butan-1-ol
74
612
0.81
34.3
7.
Butan-2-ol
74
686
0.80
38.4
8.
2-Methlprapan-1-ol
74
1406
0.79
78.8
9.
Pentan-1-ol
88
784
0.817
43.9
Note : * If the homologues/isomers of alcohols are not available, other suitable compounds, which
are available or are easily manageable can be used for this study.
** Time of flow recorded in the tables are specific for a viscometer and should not be taken as
standard values.
Conclusion
As seen from the Table 1, the viscosities of various hydrocarbon
fractions, i.e. petrol, kerosene and diesel oil are on an average 6.4,
16.4 and 18.0 respectively. Since the molecular mass of these
fractions increases from petrol to diesel oil, this indicates that
viscosity increases with increase in molecular mass. The
intermolcular attractions tend to increase with increase in molecular
mass.
127
In the case of alcohols, the viscosity of nine alcohols were

determined and their values are given in Table-II. The viscosity of
alchohols increases with an increase in the molecular mass as
can be seen from the viscosities of methanol, ethanol, propan-1-ol,
butan-1 ol, the viscosities are 34.3, 38.4 and 78.8 millipoise
respectively. This shows that viscosity increases with the increase
in molecular mass.
Precaution
The viscometer should be thoroughly cleaned and dried before use.
Suggestions for further investigation

A study of the variation of viscosity with intermolecular forces may
be carried out using appropriate compounds.
References
KEENAN, C.W.; WOOD, J.H. General Chemistry IVth Edition., Harper
and Row Publishers Inc. New York.
128

Introduction to Laboratory Techniques and Safety

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CONTENTS

Dos and donts in a chemistry laboratory

Basic laboratory equipment and procedures

Handling reagent bottles

UNIT-2 : Basic Laboratory Techniques

Cutting of glass tube and glass rod

Bending of a glass tube

Drawing out a jet

Heating solution in a test tube

Heating solution in a beaker or a flask

Measuring volume of liquids

Experiment 2.1 : Preparation of standard solution of

UNIT-3 : Purification and Criteria of Purity

Experiment 3.1 : Purification of sample of a compound

Experiment 3.2 : Determination of melting point of an organic

Experiment 3.3 : Determination of boiling point of an organic

UNIT-4 : Chemical Equilibrium (Ionic Equilibrium in Solution)

Experiment 4.1 : Study of shift in equilibrium in the reaction

Experiment 4.2 : Study of shift in equilibrium in the reaction

between [Co(H2O)6] 2+ and Cl ions

pH and pH Change in Aqueous Solutions

Experiment 5.1 : To determine the pH of some fruit

To observe the variation in pH of acid/

Experiment 5.3 : To study the variation in pH by common

Experiment 5.4 : To study the change in pH during the

Experiment 5.5 : To study the pH of solutions of sodium

Detection of end point

Requirement for a reaction in the titrimetric analysis

Acidimetry and alkalimetry

Indicators in acid base titration

Experiment 6.1 : Determination of the concentration

Experiment 6.2 : Preparation of a standard solution of

Experiment 6.3 : Determination of the strength of a

Systematic Qualitative Analysis

Experiment 7.1 : Detection of one cation and one anion

Systematic analysis of anions

Preliminary tests with dilute sulphuric acid

Confirmatory tests for anions of dilute sulphuric acid group

Preliminary tests with concentrated sulphuric acid

Confirmatory tests for anions of concentrated sulphuric

Tests for sulphate and phosphate

Systematic analysis of cations

Preliminary examination of salt for identification of cation

Wet tests for identification of cations

Analysis of Group-zero cation

Analysis of Group-I cations

Analysis of Group-II cations

Analysis of Group-III cations

Analysis of Group-IV cations

Analysis of Group-V cations

Analysis of Group-VI cations

Specimen record of salt analysis

ABORATORY work has special importance in the learning of science as scientific

LABORATORY MANUAL CHEMISTRY

In order to become proficient in basic principles underlying

1.1 DOS AND DONTS IN A CHEMISTRY LABORATORY

If a reagent bottle on your seat is empty, ask the laboratory

Note : Look for these symbols

LABORATORY MANUAL CHEMISTRY

Fig. 1.1 : Correct method of heating

The indication for cleanliness of glass apparatus is that

In the following pages you will be introduced to basic