Class XI Chemistry Lab Manual

Laboratory Manual
Chemistry
Class XI
FOREWORD
The National Council of Educational Research and Training (NCERT) is the apex
body concerning all aspects of refinement of School Education. It has recently
developed textual material in Chemistry for Higher Secondary stage which is
based on the National Curriculum Framework (NCF)2005. NCF recommends
that childrens experience in school education must be linked to the life outside
school so that learning experience is joyful and fills the gap between the experience
at home and in community. It recommends to diffuse the sharp boundaries
between different subjects and discourages rote learning. The recent development
of syllabi and textual material is an attempt to implement this basic idea. The
present laboratory manual will be complementary to the textbook of Chemistry
for Class XI. It is in continuation to the NCERTs efforts to improve upon
comprehension of concepts and practical skills among students. The purpose of
this manual is not only to convey the approach and philosophy of the practical
course to students and teachers but to provide them appropriate guidance for
carrying out experiments in the laboratory. The manual is supposed to encourage
children to reflect on their own learning and to pursue further activities and
questions. Of course the success of this effort also depends on the initiatives to
be taken by the principals and teachers to encourage children to carry out
experiments in the laboratory and develop their thinking and nurture creativity.
The methods adopted for performing the practicals and their evaluation will
determine how effective this practical book will prove to make the childrens life
at school a happy experience, rather than a source of stress and boredom. The
practical book attempts to provide space to opportunities for contemplation and
wondering, discussion in small groups, and activities requiring hands-on
experience. It is hoped that the material provided in this manual will help students
in carrying out laboratory work effectively and will encourage teachers to
introduce some open-ended experiments at the school level.
P ROFESSOR YASH PAL

Chairperson
National Steering Committee
New Delhi National Council of Educational
21 May 2008 Research and Training
PREFACE
The development of the present laboratory manual is in continuation to the
NCERTs efforts to improve upon comprehension of concepts and practical skills
among the students. The present laboratory manual will be complementary to
the textbook of Chemistry for Class XI.
The expansion of scientific knowledge and consequently the change in the
system of education has led to the development of new methods of instructions.
Today the stress is laid on the enquiry approach and discussion method instead
of lecture method of teaching. Unfortunately, it is believed that study of chemistry
means abstract thinking, writing long formulas and complex structures and
handling complicated equipments. The reason behind such endeavour is that
even well-endowed schools tend to give only the cosmetic importance to the
laboratory work. Childrens natural spirit of inquiry is often not nurtured.
The new syllabus of practical work in chemistry has been designed to cater
to the needs of pupil who are desirous of pursuing science further. The
fundamental objective of this course is to develop scientific attitude and desired
laboratory skills required at this level. The practical syllabus includes content
based experiments, which help in comprehension of the concepts.
The project work is expected to provide thrill in learning chemistry. It is
expected to serve the real purpose of practical work, which means inculcating
the ability to design an experiment, to make observations methodically and to
draw conclusions out of experimental data .The real purpose of practical work
should be to enable the students to represent the outcome of experiments
logically to conclusion, with genuine appreciation of its limitation.
For each practical work, brief theory, material required, procedure,
precautions and the questions for discussion are given in the book. The questions
are aimed at testing learners understanding of the related problems. However,
teacher may provide help in case the problem is found to be beyond the capability
of the learner. Precautions must be well understood by the learners before
proceeding with the experiments and projects.
In order to provide some basic idea about the investigatory projects, a brief
description of some investigatory projects is given in the book. However, this list
is only suggested and not exhaustive. The students may select projects from
subject area of chemistry, interdisciplinary areas or from the environment. While
selecting a project, care should be taken to see that the facilities for carrying it
out are available.
Appendices related to the chemical data and logarithmic tables are
attached at the end of the book. International symbols for hazards and hazard
warnings are given at several places in the book. It is expected that this will
make the learners more careful about the environment and make them careful
while dealing with the chemicals. Some non evaluative learning material has
been given in the boxes to provide interesting information related to the
practical work.
It is a pleasure to express my thanks to all those who have been associated
at various stages of development of this laboratory manual. It is hoped that this
practical book will improve teaching learning process in chemistry to a great
extent. The learners will be able to understand the subject well and will be able
to apply the acquired knowledge in new situations. I acknowledge with thanks
the dedicated efforts and valuable contribution of Dr Alka Mehrotra, coordinator
of this programme and other team members who contributed and finalised the
manuscript. I especially thank Professor Krishna Kumar, Director, and Professor
G. Ravindra, Joint Director, NCERT for their administrative support and keen
interest in the development of this laboratory manual. I am also grateful to the
participating teachers and subject experts who participated in the review
workshop and provided their comments and suggestions which helped in the
refinement of this manual and make it learner friendly. We warmly welcome
comments and suggestions from our readers for further improvement of this
manual.
HUKUM SINGH
Professor and Head
Department of Education in
Science and Mathematics
vi
LABORATORY MANUAL DEVELOPMENT TEAM
MEMBERS
Anjni Koul, Senior Lecturer, DESM, NCERT, New Delhi
Brahm Parkash, Professor, DESM, NCERT, New Delhi
I. P. Aggarwal, Professor, Regional Institute of Education, NCERT, Bhopal
R. S. Sindhu, Professor, DESM, NCERT, New Delhi
Ruchi Verma, Lecturer, DESM, NCERT, New Delhi
MEMBER-COORDINATOR
Alka Mehrotra, Reader, DESM, NCERT, New Delhi
ACKNOWLEDGEMENTS
The National Council of Educational Research and Training (NCER T)
acknowledges the valuable contributions of the individuals and the
organisations involved in the development of Manual for Chemistry Practicals
for Class XI. The following academics contributed very effectively for the
review of the manuscript of this manual : D. S. Rawat, Reader, Department
of Chemistry, University of Delhi; Haritima Chopra, Reader, Maitreyi College,
New Delhi; K. G. Trikha, Reader (Retired), A.R.S.D. College, New Delhi;
M. S. Frank, Vice Principal, St. Stephens College, Delhi; Samta Goel, Reader,
Zakir Hussain College, New Delhi; S. G. Warkar, Lecturer, Delhi College of
Engenering, Delhi; Sunita Bhagat, Reader, A.R.S.D. College, New Delhi;
K. K. Singh, PGT, Kendriya Vidyalaya, Pushp Vihar, New Delhi; Mona Rastogi,
Senior Headmistress, ITL Public School, Dwarka, New Delhi; Nivedita Bose,
PGT, Bluebells School, New Delhi; Nishi Saraswat, PGT, Kendriya Vidyalaya
No.1, Delhi Cantt. We are thankful to them. We also acknowledge the
contribution of Sunita Kumari, JPF. Special thanks are due to Hukum Singh,
Professor and Head, DESM, NCERT for his administrative support.
The Council also acknowledges the support provided by the administrative
staff of DESM; Deepak Kapoor, Incharge, Computer Station; Ishwar Singh,
DTP Operator for refining and drawing some of the illustrations; Ritu Jha, DTP
Operator; K. T. Chitralekha, Copy Editor. The efforts of the Publication
Department are also highly appreciated.
CONTENTS
F OREWORD iii
P REFACE v
UNIT-1 : Introduction 1
Dos and donts in a chemistry laboratory 2
Analytical methods 5
Basic laboratory equipment and procedures 5
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 38

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) 46

Experiment 4.1 : Study of shift in equilibrium in the reaction
of ferric ions and thiocyanate ions 47
Experiment 4.2 : Study of shift in equilibrium in the reaction

between [Co(H2O)6] 2+ and Cl ions 50
UNIT-5 : pH and pH Change in Aqueous Solutions 53

Experiment 5.1 : To determine the pH of some fruit
juices 54
Experiment 5.2 : 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 65

Detection of end point 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
UNIT-7 : 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 81
Confirmatory tests for anions of dilute sulphuric acid group 82
Preliminary tests with concentrated sulphuric acid 86
x
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
L
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 DO S AND DON TS 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.
2
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 INTERNATIONAL
are advised to do so.
HAZARD SYMBOLS
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 Note : Look for these symbols
running so that nothing stinks and sticks and the waste on the labels of bottles
of chemicals.
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.
3
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.
4
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 A NALYTICAL 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 :
5
Fig. 1.2 : Common laboratory equipments
6
INTRODUCTION
Fig. 1.3 : Common laboratory glass apparatus
7
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.
8
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 Fig. 1.5 : Separating funnels

of various shapes
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) (b)
Fig. 1.6 : (a) Air condenser
(b) Water condensers
9
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
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
Fig. 1.8 : Method for taking out pouring liquid from the bottle is shown in Fig. 1.9. When
solid from the reagent adding liquids directly from bottles into the beaker, a glass
bottle rod is held against the mouth of the bottle so as to permit
the flow of liquid along the rod without splashing.
10
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-a-
days, 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 thr ough 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
T
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 oxygen-
natural 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 G LASS ROD
Material Required
Soda-glass tube : 15 cm long

Soda-glass rod : 15 cm long
Triangular file : 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) 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).
(iii) 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.
(iv) If the glass tube does not break, make a deeper scratch at
the point marked earlier and make a fresh attempt.
(v) Trim any jagged edge by striking with a wire gauge (Fig. 2.2 a).
(vi) 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 Properly Overheated

The cut
the cut end in a Bunsen rounded edge end
flame, rotate back and forth end
after fire
until the edges are rounded polishing
(a) (b) (c)
Fig. 2.2 : (a) Trimming the jagged edges
(b) Rounding the edges
(c) Properly and improperly rounded edges
17
Precautions
(a) Make a single deep scratch at the desired length with one stroke of the file.
(b) 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 : 20-25 cm long

Procedure
(i) Cut a tube of desired length with the help of a triangular file
as described in section 2.1.
(ii) 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).
(iii) 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).
(a) (b) (c)
Fig. 2.3 : (a) Heating the tube

(b) The tube softens and starts bending under its own weight
(c) Making the bend coplanar
18
(iv) 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).
(v) Cool it by placing on a glazed tile (Fig. 2.3 c).
(vi) Bend the tubes at different angles as shown in Fig. 2.5.
Fig. 2.4 : A glance of proper Fig. 2.5 : Bend drawn at

and improper bends various angles
Precautions
(a) Avoid heating the glass tube only on one side, rather rotate it while heating.
(b) Select a glass tube of appropriate length (nearly 30 cm long) to keep your hands
safe from heat.
(c) 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 D RAWING OUT A JET
Material Required
Glass tube : 20-25 cm long

Sand paper : As per need
19
Procedure
(i) Select a glass tube of appropriate diameter for drawing a jet.
(ii) Cut the glass tube of desired length with the help of a
triangular file.
(iii) Heat the tube in the hottest portion of the Bunsen burner
flame by holding it at both the ends.
(iv) Rotate the tube slowly until the portion, which is kept in the
flame, becomes red hot and soft.
(v) 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.
(vi) 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 : As per need Glycerine solution

Cork borer set : One (Shelf reagent) : As per need
20
Procedure
(i) Mark the rubber cork on both its sides at the place where a
hole is to be drilled (Fig. 2.7 a).
(ii) 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).
(iii) Place the rubber cork on the table with its smaller end in the
upward direction as shown in Fig. 2.7 c.
(iv) 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.
(v) 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.
(v) 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) Make a mark on both sides of the cork and select borer of proper size.
(b) 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 T EST 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 S OLUTION 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) Never heat the apparatus with thick walls because it may
break. Borosilicate glass apparatus is usually used for
heating substances.
Fig. 2.9 : Heating solution in (ii) The apparatus, which is used for measuring volume, should
a beaker 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 : One
Beaker : Two
Funnel stand : One
Glass rod : One
Filter paper : As per need
Procedure
(i) 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.
(ii) 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) 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.
(b) 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 M EASURING 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
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
Fig. 2.16 : Burette burette (Fig. 2.17).
26
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) 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
(b) the pipette. Hold the pipette in one hand tightly, dip
the jet of the pipette into the solution to be pipetted out,
Fig. 2.19 : (a) Mounting anti parallax and squeeze the pipette bulb with the other hand
card on burette
(b) Using anti parallax card
(Fig. 2.20 b). Now loosen your grip on the bulb so that
for noting correct
the liquid is sucked into the pipette. When the liquid is
reading 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).
28
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) (d) (e)
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 Fig. 2.21 : Rinsing the pipette
should not be broken.
29
(d) Using 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
Fig. 2.22 : The measuring of the flask is made narrow to reduce error in adjustment of the
flask 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 two-
pan 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 knife-
edge, 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) 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.
(iv) 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.
(v) 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 Fig. 2.26 : Rider resting
from the centre of the beam multiplied by the weight of the rider. on grove of
Length of the beam from the centre to one side of the beam is balance beam
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
division corresponds to 0.01g = 0.001 g or 1 mg weight. Each
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).
Precautions
(a) Pans must be properly cleaned before and after weighing. Chemicals should never
be placed directly on the pans for weighing.
(b) Always release the beam gently.
(c) Avoid overloading the balance.
(d) Always transfer the weights from one place to another with the help of forceps.
(e) Do not allow the weights to get spoiled by corrosion.
(f) Never weigh a hot/cold object on the balance.
(g) 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) Always make necessary adjustments in the balance before weighing.

(i) To insert or remove weights and to keep the object on the pans always use the
side doors. Never use the front shutter.
(j) 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
require = 12.6g of hydrated oxalic acid. Therefore, for preparing
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 :
Mass of solute is grams 1000

Molarity (M) =
Molar mass of solute (volume of solution to
be prepared in mL)
Material Required
Measuring flask (250 mL) : One

Funnel : One
Weighing tube/Watch glass : One Oxalic acid : As per need
Wash bottle : One
Iron stand with ring clamp : One
Procedure
(i) Weigh an empty, clean and dry watch glass/weighing tube
accurately (Weight 1). Oxalic acid
(ii) 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.
(iii) 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.
35
(iv) 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.
(a) (b) (c) (d)

Fig. 2.27 : Making standard a solution
(a) T ransfering oxalic acid (b) Diluting the solution
(c) Adding last few mL dropwise (d) Standard solution
Precautions
(a) The pan of the balance should be cleaned before and after weighing.
(b) Never touch the weights with hand. Use forceps to transfer weights from the weight-
box to the pan of the balance.
(c) Always use spatula to transfer the reagent from the bottle on to the watch glass.
(d) Stopper the reagent bottle immediately after withdrawing the substance.
(e) Always use distilled water to prepare the standard solution.
(f) Always check the adjustment of the balance before weighing the substance.
(g) Care should be taken while weighing the chemicals. These should not be spilled
on the pan of the balance.
(h) Watch glass/weighing bottle and funnel should be washed several times by using
small amounts of distilled water each time.
(i) 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.
(j) To ensure uniform composition of the solution, stopper the flask and shake it
carefully and thoroughly.
36
(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
F
OR 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.
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) : One

Glass funnel : One
Potash alum,
Tripod stand : One
Copper sulphate
Porcelain dish : One
and Benzoic acid : As per need
Glass rod : One
Sand bath : One
Procedure
(i) Take 30-50 mL distilled water in a beaker and prepare a Copper sulphate
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.
Precautions
(a) Do not evaporate the entire solvent while concentrating the solution.
(b) Do not disturb the solution while it is being cooled.
(c) 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+ 2
(a) K (H2O)6 Al (H2O)6( SO4 )2
(b) K 2SO4.Al2(SO 4) 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
Liquid paraffin
Thieles tube
/Conc. H2SO4 : As per need
/Kjeldhals flask/beaker : One
Organic Compound
Thermometer : One
(Naphthalene/
Capillary tubes : As per need
p-Dichlorobenzene/
Iron stand with clamps : One
p-Toluidine) : As per need
Procedure
(i) Take a capillary tube of approximately 8 cm in length. Seal
its one open end by heating it in a Bunsen flame. Rotate the p-Dichlorobenzene
capillary while sealing to ensure complete closure of the
opening.
p-Toluidine
(ii) 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 Naphthalene
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 Hazard Warning
is prevented from breaking.
Avoid contact with skin
(iii) Moisten the capillary tube with liquid paraffin and stick it to and eyes and dont inhale
the thermometer. It will stick to the thermometer by cohesive vapours of these
forces. See that the lower ends of the capillary tube and the chemicals.
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.
(iv) 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.
(v) 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.
(vi) 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.
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) Keep the lower end of the capillary tube and the thermometer at the same level.
(b) Capillary tube should not be very thick.
(c) Packing of the powder should be uniform without any big air gaps in between
the solid particles.
(d) Thieles tube should be heated at the side arm by using a low flame.
(e) 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.
(f) Never fill the bulb of Kjeldahl flasks more than half.
Note : 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 : One

Thermometer 110C or 360C : One Organic liquid : 1 mL
Iron stand with clamp : One Liquid paraffin/
Ignition tube : One Conc. H2SO4 : As per need
Capillary tube : One
Concentrated 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
Fig. 3.2: Determination of boiling point the liquid.
Note : For determination of boiling point of high

boiling liquids, paraffin cannot be used
as heating medium.
44
Precautions
(a) 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.
(b) Keep the lower end of the ignition tube and the thermometer bulb at the same
level.
(c) Heat the side arm of the Thieles tube gently.
(d) 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
UNIT 4
CHEMICAL EQUILIBRIUM
(IONIC EQUILIBRIUM IN SOLUTION)
C
HEMICAL 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.
A+B C+D
According to the law of mass action, rate of forward reaction, r 1, will be directly
proportional to the product of concentrations of A and B and the rate of backward
reaction, r 2, 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, r 1 will be equal to r2
k1 [A][B] = k 2 [C][D]
k1 [C][D]
=
k2 [A][B]
k1
Putting k = Kc we have
2
[C][D]
Kc =
[A][B]
K c 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 (I ONIC 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.
Fe3+ (aq) + SCN (aq) [Fe(SCN)]2+ (aq)
(Blood red colour)
The equilibrium constant for the above reaction may be

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

Beaker (250 mL) : One
Boiling tubes : Six
Burettes : Four Ferric chloride : 0.100g
Glass droppers : Two Potassium thiocyanate : 0.100g
Test tube stand : One
Glass rod : One
* 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 (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.
Hazard Warning (ii) Mix 20 mL of ferric chloride solution with 20 mL of potassium
Avoid contact with skin thiocyanate solution. Blood red colour will be obtained. Fill
and eyes. 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
Change in colour
Volume of ferric
intensity as matched Direction of shift in
Boiling Tube chloride solution taken
with reference solution in equilibrium
in the system in mL
boiling tube a
a Reference solution for matching colour containing Equilibrium
2.5 mL blood red solution + 17.5 mL water position
(20 mL equilibrium mixture)
b 1.0
c 2.0
d 3.0
e 4.0
Table 4.2 : Equilibrium shift on increasing the concentration of thiocyanate ions
Change in colour
Volume of thiocyanate
intensity as matched Direction of shift in
Boiling Tube solution taken in the
with reference solution in equilibrium
system in mL
boiling tube a
a Reference solution for matching colour containing Equilibrium
2.5 mL blood red solution + 17.5 mL water position
(20 mL equilibrium mixture)
b 1.0
c 2.0
d 3.0
e 4.0
49
Precautions
(a) Use very dilute solutions of ferric chloride and potassium thiocyanate.
(b) Compare the colour of the solutions by keeping the boiling tube and the reference
test tube side by side.
(c) To judge the change in colour of the solution in an effective manner, note the
colour change in diffused sunlight.
(d) 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)] + H 2O.
(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
[Co(H2O)6]2+ and Cl ions, by changing the concentration of any
one of these ions.
Theory
2+
In the reaction between [Co (H2O)6] and Cl ions, the following
displacement reaction takes place.
2+ 2
[Co(H2O)6] + 4Cl [CoCl4] + 6H2O
Pink Blue
50
This reaction is known as ligand displacement reaction and

the equilibrium constant, K, for this is written as follows: Hydrochloric acid
2
[[CoCl4 ] ]
K = 2+ 4 Acetone
[[Co(H2O)6 ] ] [Cl ]
Alcohol
Since the reaction occurs in the aqueous medium, it is believed
that concentration of H 2O is almost constant and is included in
the value of K itself and is not shown separately in the expression
for equilibrium constant. Hazard Warning
2+
Now if at equilibrium the concentration of either [Co (H 2O)6] Acetone and alcohol are
ion or Cl ions is increased, then this would result in an increase inflamable, do not let the
2
in [CoCl4] ion concentration thus, maintaining the value of K as bottles open when not in
constant. In other words we can say that equilibrium will shift in use.
the forward direction and will result in a corresponding change Keep the bottles away
from flames.
in colour. Wash your hands after
use.
Wear safety spectacles.
Material Required
Conical flask (100 mL) : One

Beakers (100 mL) : Three Acetone/alcohol : 60 mL
Burettes : Three Concentrated
Test tubes : Six hydrochloric acid : 30 mL
Test tube stand : One Cobalt chloride : 0.6000 g
Glass rod : One
Procedure
(i) Take 60 mL of acetone in a 100 mL conical flask and dissolve
0.6000 g CoCl2 in it to get a blue solution.
(ii) 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 Note : In the first set
these test tubes. Add 0.2 mL, 0.4 mL, 0.6 mL and 0.8 mL of of experiments
concentration of
water to test tubes B, C, D and E respectively, so that the total
chlorocomplex is
volume of solution in each of the test tubes is 4.0 mL. constant and
(iii) Note the gradual change in colour of the mixture from blue concentration of
to pink with an increase in the amount of water. water is changing.
In the second set
(iv) Take 10 mL cobalt chloride solution in acetone prepared
concentration of
above and add 5 mL distilled water to it. A solution of pink aqua complex is
colour will be obtained. constant and
(v) Take 1.5 mL of pink solution from step (iv) in five different concentration of
test tubes labeled as A B, C, D and E. Add 2.0 mL, chloride ions is
increasing.
1.5 mL, 1.0 mL and 0.5 mL of water to the test tubes labelled
51
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.
(vi) 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. Test Volume of acetone Volume of CoCl2 Volume of water Colour
No. tube added in mL solution added in mL added in mL of mixture
1. A 1.0 3.0 0.0
2. B 0.8 3.0 0.2
3. C 0.6 3.0 0.4
4. D 0.4 3.0 0.6
5. E 0.2 3.0 0.8

Table 4.4 : Shift in equilibrium on adding Cl ions
Sl. Test Volume of conc. Volume of aquo complex Volume of water Colour
No. tube HCl added in mL solution added in mL added in mL of mixture
1. A 0.5 1.5 2.0
2. B 1.0 1.5 1.5
3. C 1.5 1.5 1.0
4. D 2.0 1.5 0.5
5. E 2.5 1.5 0.0
Precautions
(a) Take all the precautions of experiment 4.1.
(b) Use distilled water for the experiment.
(c) 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
Y
OU 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
+
H 2O(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:
+
[H3 O ] [OH ]
K= 2
[H 2O]
Since water is in large excess, its concentration can be assumed to be constant
and combining it with K provides a new constant K w, which can be written as follows:
+
Kw = [H3O ] [OH ]
K w is self ionisation constant of water or simply ionization constant of water.
It remains constant at constant temperature. At 25C value of Kw is 1.01014.
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 [H 3O ]
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 Fruit juice : Lemon,orange,

Glass droppers : Four apple,pineapple
Test tubes : Four pH papers/universal
pH chart : One 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 Colour with universal

pH Inference
Juice indicator
Lemon
Orange
Apple
Pineapple
Result
Increasing order of pH value of juices is ____________.
55
Precautions
(a) Add equal number of drops of universal indicator to equal volumes of solutions
in each of the test tubes.
(b) Match the colour of the solution with pH chart carefully.
(c) Store pH papers at a safe place to avoid contact with acidic and basic reagents
kept in the laboratory.
(d) 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
0.1 M HCl solution : 20mL

Boiling tubes : Eight 0.1 M NaOH solution : 20mL
Glass droppers : Four 0.05 M H2SO 4 solution : 20mL
Test tubes : As per need pH paper/universal
indicator : As per need
Procedure
(i) Take four boiling tubes and mark them as A, B, C and D.
(Fig. 5.1).
(ii) Take 2mL of 0.1 M HCl in boiling tube A.
56
(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
H 2SO4
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 H2SO4 NaOH
Boiling tube
Colour pH Colour pH Colour pH
A
Result
(i) Concentration of solutions of test tube B, C and D are ____________.
(ii) Write your conclusion about the variation of pH with dilution.
Precautions
(a) Add equal number of drops of the universal indicator to equal amounts of solution
in each of the boiling tubes.
(b) 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 H2SO 4, 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
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 (weak acid)
+
(2) BOH B + OH (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
Sodium ethanoate : 2g
Beakers (100 mL) : Four
Ammonium chloride : 2g
Pipettes (25 mL) : Two Ethanoic acid (1.0 M) : 50 mL
Test tubes : Four Ammonia solution (1.0 M) : 50 mL
pH chart : One pH paper and
universal indicator : As per need
Procedure
(i) Take four 100 mL beakers and mark them as A, B, C and D. Ammonia solution
(ii) Transfer 25 mL of 1M ethanoic acid in beaker A and 25 mL
of (1M) ammonia solution in beaker B. Ethanoic acid
(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
Ammonium chloride
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.
59
Table 5.3 : Comparison of pH of acid/base and its buffer
Sl. No. of Composition of the Colour

pH
Test Tube system of pH paper
1 CH3 COOH in water
2 NH4 OH (NH3 in water)
3 CH3 COOH + CH3 COONa
4 NH4 OH+NH4Cl
Result
(a) pH of acetic acid is _______

(b) pH of buffer of acetic acid and sodium acetate is ________ than acetic acid.
(c) pH of ammonia solution is _______
(d) pH of buffer of ammonia solution and ammonium chloride is _________ than the
ammonia solution.
(e) Common ion effect ________ ionization of acid/base.
Precautions
(a) Try only weak acid/weak base and its salt for the study of the common ion effect.
(b) Handle the bottle of ammonium hydroxide with care.
(c) Add equal number of drops of the universal indicator in each of the test tubes.
(e) 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
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 : One Hydrochloric acid

Beakers (250 mL) : Two (0.1 M) : 25 mL
Conical flask (100 mL): One Sodium Hydroxide
Dropper : One solution (0.1 M) : 50 mL
pH chart : One Universal indicator : As per requirement
Procedure
(i) Take 25 mL hydrochloric acid solution (0.1 M) in 100 mL Hydrochloric acid
conical flask.
(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 Total volume of NaOH added pH

added in lots (mL) to the solution in flask (mL)
1. 0 0
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
Precautions
(a) To get good results perform the reaction with solutions of strong acid and strong
base of same concentration.
(b) Handle the bottle of acid and base with care.
(c) 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
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
pH paper/universal indicator: As per need

Boiling tubes : Three 0.1 M NaCl solution : As per need
Test tubes : Three 0.1 M FeCl3 solution : As per need
Glass droppers : Three 0.1 M Na2CO3 solution : As per need
Procedure
(i) Take three boiling tubes and mark them as A, B and C.
(ii) Take 20 mL of 0.1 M solution(s) of NaCl, FeCl3 and Na2CO 3
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, FeCl 3 and Na2 CO3 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) Use freshly prepared solutions.

(b) Do not leave the bottles open after taking out salt.
(c) Use separate and clean test tube for each solution.
(d) 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
Y
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 R EQUIREMENT FOR A REACTION IN THE T ITRIMETRIC ANALYSIS

(i) The substance of which amount is to be determined by
titrimetric analysis must react completely and rapidly with
the other reagent in stoichiometric proportion.
(ii) 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 A LKALIMETRY

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.
number of moles of solute
Molarity, M =
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
TITRIMETRIC A NALYSIS
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
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
H + Ph
+
NaOH Na + OH
H+ + 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 Quinonoid form of the anion

(Yellow in colour) (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 V 2 ...(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) : One

Pipette (10 mL) : One
Oxalic acid : As per need
Conical flask (100 mL) : One
Sodium hydroxide
Burette stand : One
solution : As per need
Funnel : One
Phenolphthalein
White glazed tile : One indicator : As per need
Procedure
(A) Preparation of 0.1M Standard Solution of Oxalic Acid

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 : T itrating 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
Volume of oxalic Burette readings Volume of sodium

acid solution hydroxide solution
Concordant
Sl. No. taken in conical Initial Final used reading in
flask each time reading reading V2 mL = (yx) mL mL
V1 mL (x) (y)
71
Calculations
Molarity of NaOH solution can be calculated by using the equation:
Oxalic acid Sodium hydroxide
a1 M1V1 = a2 M2V2
where, M 1 and V1 are the molarity and volume of the oxalic
acid solution.
M 2 and V2 are the molarity and volume of the sodium hydroxide
solution.
a 1 and a2 are respectively the basicity of oxalic acid and acidity
of sodium hydroxide. In this case a1= 2 and a2 = 1.
1
Also, Molar mass of oxalic acid, (COOH) 2 .2H2O = 126 g mol
and Molar mass of sodium hydroxide (NaOH) = 40 g mol 1
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) Always rinse the burette with the solution, which is to be taken in it.
(b) Remove the air gap if any, from the burette before titrating the solution. Make
sure that the nozzle of burette is also filled.
(c) 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.
(d) Always read the lower meniscus for all transparent solutions and upper meniscus
for coloured solutions.
(e) To note the burette readings place the eye exactly at the level of the meniscus.
(f) Never hold the pipette at the bulb.
(g) Never use the pipette and burette with a broken nozzle.
(h) Never suck a strong acid or an alkali with the pipette.
(i) Always keep the lower end of the pipette dipped in the liquid while sucking the
liquid.
(j) Do not blow out the last drop of the solution from the jet end of the pipette into
the flask.
(k) The concentration (strength) of the solution must be calculated up to the fourth
place of decimal.
72
(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.
K NOW 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
in per litre of solution then N1V1 = N2V2 (i)
Equivalent mass of acids and bases is given by the following expression:
molar mass
Equivalent mass of acid = (ii)
basicity
molar mass
Equivalent mass of base = ... (iii)
acidity
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
Number of gram equivalent mass w/ Equivalent mass
Normality (N)= = (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)]
w
Equivalent mass = ... (v)
N V
If acidity or basicity is a, then by definition of equivalent mass
73
Molar ma ss
Equivalent mass = (vi)
a
From equations (v) and (vi) we can write
w Molar mass
=
N V a
a (w/Molar mass )
Or N=
V
w/Molar mass
But is the molarity (M)
V
Therefore, N = a M (vii)
Equation (vii) is the expression for the relationship between normality and molarity.
By using equation (vii) in equation (i) we have a1M1V1 = a2M2V 2 .... (viii)
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
M1V1 = M2V2 ...(ix)
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 V 1 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 Na2CO 3 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

Watch glass : One
Sodium carbonate : As per need
Funnel : One
Wash bottle : One
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) : One

Pipette (10 mL) : One
Conical flask (100 mL) : One Hydrochloric acid : As per need
Burette stand : One Sodium carbonate : As per need
Funnel : One Methyl orange solution : As per need
Glazed tile (white) : One
Procedure
(A) Preparation of 0.1 M standard solution of sodium
carbonate
Hydrochloric acid
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
Volume V1 of Burette readings Volume of HCl

Na2 CO3 solution solution used Concordant
Sl. No. taken in the Initial Final reading
conical flask reading reading V2 mL = (yx) mL in mL
each time in mL (x) (y)
76
Calculations
Calculate the strength of HCl solution by using the equation
Na2CO3 solution HCl solution
a1M1V1 = a2M2V2
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 Na 2CO 3 solution).
a1 = 2
M 2 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
Molar mass of Na2CO3 = 106 g mol1, Molar mass of HCl = 36.5 g mol1 ,
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) Care should be taken while handling the acid and base.
(b) Always rinse the burette and the pipette with the solution which is to be taken in
them.
(c) Remove the air gap if any, from the burette before titration.
(d) 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.
(e) Always read the lower meniscus for all transparent solutions and upper meniscus
for the coloured solutions.
(f) Never use burette and pipette with a broken nozzle.
(g) Never suck a strong acid or an alkali with the pipette, use pipette bulb.
(h) Always keep the lower end of the pipette dipped in the liquid while sucking the
liquid.
(i) While transferring the solution to the flask, do not blow out the last drop of the
solution from the jet of the pipette.
(j) The strength of the solution must be calculated up to the fourth decimal place.
77
K NOW THIS ALSO
Potassium hydrogenphthalate is primary standard for standardisation of sodium hydroxide

solution. Formula of potassium hydrogen phthalate is C6H 5O 4K. 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
A
NALYSIS 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
NaCl, Cu2+ and Na+ ions are cations and SO2 4
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:
(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 ,
Mg , NH+4
2+
2
Anions - CO2
3
, S , SO2
3
, 2 3
SO4 , NO2 , NO3 , Cl , Br , I , PO 4 , C2 O4 ,
2

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
Boiling tube : As per need

Test tubes : As per requirement
Measuring cylinder : One
Test tube stand : One Reagents : As per need
Test tube holder : One
Delivery tube : One
Corks : As per need
Filter paper : As per need
80
SYSTEMATIC QUALITATIVE ANALYSIS
SYSTEMATIC ANALYSIS OF A NIONS
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.
Carbonate ( CO2
3
), sulphide (S2), sulphite ( SO2
3
), nitrite ( N O 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
Fig. 7.1 : Testing a Gas
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).
Table 7.1 : Preliminary test with dilute sulphuric acid
Inference
Observations
Gas evolved Possible Anion
A colourless, odourless gas is evolved

with brisk effervescence, which turns CO2 2
Carbonate ( CO 3 )
lime water milky.
Colourless gas with the smell of rotten

2
eggs is evolved which turns lead acetate H 2S Sulphide (S )
paper black.
Colourless gas with a pungent smell, like

burning sulphur which turns acidified SO2 2
potassium dichromate solution green. Sulphite ( SO 3 )
Brown fumes which turn acidified

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

vinegar. Vapours turn blue litmus red. CH3COOH vapours Acetate, (CH3 COO )
81
2- 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
insoluble in water. Confirmation of CO2 3
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 2 2
Table 7.2 : Confirmatory tests for CO3 , S , SO3 , NO3 , CH3 COO
Anion Confirmatory test
Carbonate ( CO
2 -) Take 0.1 g of salt in a test tube, add dilute sulphuric acid.
3
CO2 gas is evolved with brisk effervescence which turns lime
water milky. On passing the gas for some more time, milkiness
disappears.
2
Sulphide (S ) 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.
2
*Sulphite ( SO3 ) (a) 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.
(b) Take the precipitate of step (a) in a test tube and add
a few drops of potassium permanganate solution
acidified with dil. H 2 S O4 . Colour of potassium
permanganate solution gets discharged.
(a) Take 1 mL of water extract in a test tube. Add a few
Nitrite ( NO )
2
drops of potassium iodide solution and a few drops of
starch solution, acidify with acetic acid. Blue colour
appears.
(b) 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

Acetate (CH3COO ) (a) Take 0.1 g of salt in a china dish. Add 1 mL of ethanol
and 0.2 mL conc. H 2 SO4 and heat. Fruity odour
confirms the presence of acetate ion.
(b) 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 CaCO 3 (Fig. 7.1)
Na2CO3 + H2SO4 Na2SO 4 + H 2O +CO2
Ca(OH)2 + CO2 CaCO3 + H2O
If CO 2 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
2. Test for Sulphide ion [S ]
(a) 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
(CH 3COO)2Pb + H2S PbS + 2CH3COOH

Lead sulphide
Black precipitate
(b) 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 + Na 2 [Fe(CN)5NO] Na 4 [Fe(CN)5NOS]
Sodium nitroprusside Complex of Purple colour
2
3. Test for Sulphite ion [SO3 ]
(a) On treating sulphite with warm dil. H2SO 4, SO 2 gas is evolved which is
suffocating with the smell of burning sulphur.
Na2SO 3 + H2SO 4 Na2SO4 + H2O + SO2
Barium
The gas turns potassium dichromate paper acidified with dil. H2SO4, green.
compounds K2Cr2O7 + H 2SO 4 + 3SO2 K2SO4 + Cr2 (SO4)3 + H2O
Chromium
sulphate (green)
Potassium (b) An aqueous solution or sodium carbonate extract of the salt produces a
permanganate white precipitate of barium sulphite on addition of barium chloride solution.
Na2SO 3 + BaCl 2 2NaCl + BaSO 3
This precipitate gives following tests.

(i) 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 + H2SO 4 BaSO4 + H2O + SO2
2KMnO4 + 3H2SO4 K 2SO4 + 2MnSO4 + 3H2O + 5 [O]

SO2 + H2O + [O] H2SO 4

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 + H2SO 4 Na2SO 4 + 2HNO2
3HNO2 HNO3 + 2NO + H2O
2NO + O2 2NO2
Brown gas
84

(ii) NO2 + CH3COOH HNO2 + CH 3COO
2HNO 2 + 2KI + 2CH3COOH 2CH3 COOK + 2H2O + 2NO + I 2
I 2 + 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 + CH 3COO
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 CH 3COONa + H 2SO4 Na2SO4 + 2 CH3COOH
+
H
CH3COOH + C 2H 5OH CH 3COOC 2H5 + 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 HCl Chloride, (Cl )
brought near the mouth of the test tube.
Reddish brown gas with a pungent

odour is evolved. Intensity of reddish gas

increases on heating the reaction Br2 vapours Bromide, (Br )
mixture after addition of solid MnO2 to
the reaction mixture. Solution also
acquires red colour.
Violet vapours, which turn starch paper

blue and a layer of violet sublimate is I2 vapours Iodide, (I )
formed on the sides of the tube. Fumes
become dense on adding MnO2 to the
reaction mixture.
Brown fumes evolve which become dense
upon heating the reaction mixture after
NO2 Nitrate, ( NO )
addition of copper turnings and the 3
solution acquires blue colour.
Colourless, odourless gas is evolved

which turns lime water milky and the 2
CO and CO 2 Oxalate, ( C2O 4 )
gas coming out of lime water burns with
a blue flame, if ignited.
86
Confirmatory tests for the anions which react with concentrated sulphuric
acid are given in Table 7.4.
2
Table 7.4 : Confirmatory tests for Cl , Br , I , NO 3 and C2 O 4
Anion Confirmatory test

Chloride (Cl ) (a) 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.
(b) 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 .
(c) Take 0.1 g salt and a pinch of solid potassium
dichromate in a test tube, add conc. H2 SO4 , 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.

Bromide (Br ) (a) 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.
(b) 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.
(c ) 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.

Iodide ( I ) (a) 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 or ganic layer.
(b) 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 ( NO3 ) Take 1 mL of salt solution in water in a test tube. Add 2 mL

conc. of H2 SO4 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.
2 (a) Take 1 mL of water extract or sodium carbonate
Oxalate ( C O )
2 4
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.
(b) Take the precipitate from test (a) and dissolve it in
dilute H 2SO4. Add very dilute solution of KMnO 4 and
warm. Colour of KMnO 4 solution is discharged. Pass
the gas coming out through lime water. The lime water
turns milky.

1. Test for Chloride ion [Cl ]
(a) 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
Manganese
dioxide
Sodium Hydrogen chloride
hydrogen sulphate Colourless gas
HCl + NH3 NH4Cl
Silver nitrate Ammonium chloride
White fumes
(b) 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 + 2H 2SO 4 Na2SO4 + MnSO4 + 2H2O + Cl2
(c) 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 NaNO3 + Ag Cl
Silver chloride
(White precipitate)
AgCl + 2NH4OH [Ag(NH3)2 ]Cl + 2H2O

Diammine silver (I)
chloride
* 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 + 6H2SO 4 2KHSO4 + 2CrO2Cl2 + 4NaHSO4 + 3H2O Chromyl
(Chromyl chloride
chloride)
CrO2Cl2 + 4NaOH Na 2CrO4 + 2NaCl + 2H2O
Lead
(CH 3COO)2Pb + Na2CrO4 PbCrO4 + 2CH3COONa chromate
Sodium Lead chromate
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
organic layer turns blue. CrO24 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 + 2H2O 2 Cr O5 + 3H2O
Chromium
pentoxide

2. Test for Bromide ion (Br )
If on heating the salt with conc. H2SO 4 reddish brown fumes of bromine are
evolved in excess, this indicates the presence of Brions. The fumes get intensified
on addition of MnO 2. Bromine vapours turn starch paper yellow.
Bromine
2NaBr + 2H 2SO4 Br2 + SO2 + Na2SO 4 + 2H2O very toxic by
inhalation
2NaBr + MnO 2 + 2H2SO4 Na 2SO 4 + MnSO4 + 2H2O + Br 2 corrosive
(a) 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 + Cl 2 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 NaNO 3 + AgBr
Silver bromide
Pale yellow precipitate

3. Test for Iodide ion ( I )
(a) 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.
Iodine,
harmful by
2NaI + 2H2SO 4 Na2SO4 + SO2 + 2H2O + I2
inhalation
and contact I2 + Starch Blue colour
with skin solution
Chlorine, NaI + H2SO4 NaHSO 4 + HI

toxic by
inhalation
2HI + H2SO 4 2H2O + I2 + SO 2
Chloroform, 6NaI + 4H2SO4 3I2 + 4H2O +S + 3Na2SO4

harmful and
toxic by 8NaI + 5 H2SO4 4I2 + H 2S + 4Na2SO4 + 4H2O
inhalation
On adding MnO2 to the reaction mixture, the violet vapours become
dense.
2NaI + MnO2 + 2H2SO4 I2 + MnSO4 + Na2SO 4 + 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 + NaNO3
silver iodide
(Yellow precipitate)
90

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. H 2SO 4. Evolution of excess of brown fumes indicates
the presence of nitrate ions. The solution turns blue due to the formation
of copper sulphate. Copper
sulphate
NaNO3 + H2SO4 NaHSO4 + HNO 3
4HNO3 4NO2 + O2 + 2H2O
2NaNO3 + 4H2SO4 + 3Cu 3 CuSO4 + Na2SO4 + 4H2O + 2NO
Nitric
Copper sulphate acid
(Blue)
2NO + O 2 2NO2
(Brown fumes)
(b) Take 1 mL of an aqueous solution of the salt and add 2 mL conc. H 2SO 4 Oxalates
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.
Fig. 7.2 : Formation of brown ring
NaNO3 + H2SO4 Na HSO 4 + HNO 3

6 FeSO4 + 3H2SO4 + 2HNO3 3Fe 2 (SO 4)3 + 4H2O + 2NO
FeSO4 + NO [Fe(NO)]SO4
Nitroso ferrous sulphate
(Brown)
2
5. Test for Oxalate ion [C 2O4 ]
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. H 2SO 4 Na 2SO4 + 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 + Na2C2O 4 CaC 2O 4 + 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 + H 2SO 4 CaSO 4 + 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
Ion Confirmatory Test
2 (a) Take 1 mL water extract of the salt in water or sodium

Sulphate ( SO 4 )
carbonate and after acidifying with dilute
hydrochloric acid add BaCl 2 solution. White
precipitate insoluble in conc. HCl or conc. HNO 3 is
obtained.
(b) Acidify the aqueous solution or sodium carbonate
extract with acetic acid and add lead acetate solution.
Appearance of white precipitate confirms the presence
of SO 24 ion.
3 (a) Acidify sodium carbonate extract or the solution of

Phosphate ( PO 4 )
the salt in water with conc. HNO3 and add ammonium
molybdate solution and heat to boiling. A canary
yellow precipitate is formed.
92
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 .
Na2SO4 + BaCl2 BaSO4 + 2NaCl

Barium sulphate
(White precipitate)
(b) 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 + (CH 3COO)2Pb PbSO 4 + 2CH 3COONa

Lead sulphate
(White precipitate)
3
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,
(NH 4)3[P (Mo3O10)4] is formed. Each oxygen of phosphate has been
replaced by Mo 3O 10 group.
Na2HPO4 + 12 (NH4)2 MoO4 + 23 HNO3 (NH4)3[P (Mo3O10 )4] + 2NaNO3 + 21NH4NO3 + 12H2O
Canary yellow
precipitate
SYSTEMATIC A NALYSIS 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
Light green, Yellow, Brown Fe2+, Fe3+

Blue Cu2+
Bright green Ni2+
Blue, Red, Violet, Pink Co2+
Light pink Mn2+
2. Dry Heating Test
(i) Take about 0.1 g of the dry salt in a clean and dry test tube.
(ii) 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 Colour of the flame
observed by naked eye observed through blue glass Inference
Green flame with Same colour as observed Cu2+

blue centre without glass
Crimson red Purple Sr 2+
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. (a) (b)
(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
confirm that the bead is transparent and colourless. If it flame (b) Heating in
is coloured this means that, the platinum wire is not clean. oxidising flame
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 Na2B4O 7 + 10H2O
Borax
Na2B4O7 2NaBO2 + B2O3
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 + B2O 3
Non -lu minou s flam e Cu(BO2)2 + SO3
Cupric metaborate
Blue-green
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 + Na2 B4 O7 + CO
or (ii) Cupric metaborate may be reduced to metallic copper and the bead appears
red and opaque.
Luminous flame
2Cu(BO2 )2 + 4NaBO 2 + 2C 2Cu + 2Na 2B4O 7 + 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 Heating in reducing

(non-luminous) flame (luminous) flame
Inference
Colour of the salt bead Colour of the salt bead
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+
96
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.
(a) (b)
Fig. 7.6 : (a) Making charcoal cavity (b) Heating salt in the cavity
(iii) Moisten the salt in the cavity with one or two drops of water, otherwise
salt/mixture will blow away.
(iv) 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.
(v) Always bore a fresh cavity for testing the new salt.
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.
(a) (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.

Heat
CuSO 4 + Na 2CO3 CuCO3 + Na 2 SO 4
He at
CuCO 3 CuO +CO 2
He at
Cu O + C
Cu + CO
Red c olour
In case of ZnSO4 :
Heat
ZnSO 4 + Na2 CO 3 ZnCO3 + Na 2 SO 4
Heat
ZnCO 3 ZnO + CO 2
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.
Heat
2Co (NO3 )2 2CoO + 4NO 2 + O 2
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 (NH 4+ ion)
(a ) 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.
(b) 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.
(NH 4) 2 SO4 + 2NaOH Na2SO 4 + 2NH 3 + 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.
Mercury 2K2HgI4 + NH3 + 3KOH HgO.Hg(NH2)I + 7KI + 2H2O
Salts
Basic mercury (II)
amido-iodine
(Brown precipitate)
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
Precipitate, Group I If no precipitate is formed

2+
(Pb ) as chloride Pass H2S gas
Precipitate, Group II If no precipitate, take original solution

(Pb , Cu , As )
2+ 2+ 3+
Heat (O.S.) with conc. HNO3,
as sulphides
cool and add solid NH4Cl + NH4OH
solution in excess
Precipitate, Group III If no precipitate

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

2+ 2+ 2+ 2+
(Co , Ni , Mn , Zn ) Add NH4OH and
as sulphides solid (NH4)2 CO3
Precipitate, Group V If no precipitate, take original

2+
(Ba , Sr , Ca ) 2+ 2+ solution to test Group VI,
as carbonates Mg2+
* This flow chart is for the detection of one cation only.

For detection of more than one cation modification will be required.
100
Table 7.11 : Group reagents for precipitating ions
Group Cations * Group Reagent
+
Group zero NH4 None
2+
Group-I Pb Dilute HCl
2+ 2+ 3+
Group-II Pb , Cu , As H 2S gas in presence of dil. HCl
3+ 3+
Group-III Al , Fe NH4OH in presence of NH4Cl
2+ 2+ 2+ 2+
Group-IV Co , Ni , Mn , Zn H 2S in presence of NH4 OH
2+ 2+ 2+
Group-V Ba , Sr , Ca (NH4)2CO3 in presence of NH4 OH
2+
Group-VI Mg 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 A yellow precipitate is obtained.
part.
2. To the second part add potassium chromate A yellow precipitate is obtained which
solution. is soluble in NaOH and insoluble in
ammonium acetate solution.
3. To the third part of the hot solution add few A white precipitate is obtained
drops of alcohol and dilute sulphuric acid. which is soluble in ammonium
acetate solution.
Chemistry of the Confirmatory Tests of Pb2+ 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 + 2KI PbI2 + 2KCl
(Hot solution) Yellow precipitate
* Here only those cations are given which are in the syllabus.
101
This yellow precipitate (PbI2) is soluble in boiling water and reappears

on cooling as shining crystals.
2. On addition of potassium chromate (K2CrO4) solution a yellow precipitate
of lead chromate is obtained. This confirms the presence of Pb2+ ions.
PbCl2 + K2CrO4 PbCrO4 + 2KCl
(Hot solution) Lead chromate
The yellow precipitate (PbCrO4) is soluble in hot NaOH solution.
PbCrO4 + 4NaOH Na2[Pb(OH)4] + Na2CrO4
Sodium tetra
hydroxoplumbate (II)
3. A white precipitate of lead sulphate (PbSO4) is formed on addition of
alcohol followed by dil. H2SO4.
PbCl2 + H2SO4 PbSO4 + 2 HCl
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.
Hydrogen PbSO4 + 4 CH3COONH4 (NH4)2 [Pb(CH 3COO)4] + (NH4) 2SO 4
sulphide 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
indicates the presence of Cu2+ or Pb2+ ions.
If it is yellow in colour, then presence of
As3+ 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 H 2S gas
102
Table 7.13 : Confirmatory tests for Group-II A and II B cations
2+ 2+
Black precipitate of Group II A ions (Pb , Cu ) If a yellow precipitate soluble in
insoluble in yellow ammonium sulphide is formed. yellow ammonium sulphide is
3+
formed then As ion is present.
Boil the precipitate of Group II A with dilute nitric Acidify this solution with dilute
acid and add a few drops of alcohol and dil. H2SO4 . HCl. A yellow precipitate is formed.
Heat the precipitate with
concentrated nitric acid and add
White precipitate confirms If no precipitate is
2+ ammonium molybdate solution. A
the presence of Pb ions. formed, add excess of
canary yellow precipitate is formed.
Dissolve the precipitate in ammonium hydroxide
ammonium acetate solution. A blue solution
solution. Acidify with is obtained, acidify it
acetic acid and divide the with acetic acid and add
solution into two parts. potassium ferrocyanide
(i) To the first part add solution. A chocolate
potassium chromate brown precipitate is
solution, a yellow formed.
precipitate is formed.
(ii) To the second part,
add potassium iodide
solution, a yellow
precipitate is formed.
Group-II A (Copper Group)

Alcohol
Chemistry of confirmatory tests of Group-II A cations
1. Test for Lead ion (Pb 2+)
Lead sulphide precipitate dissolves in dilute HNO 3. 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(NO 3) 2 + H2SO4 PbSO 4 + 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.
PbSO 4 + 4CH3COONH4 (NH4)2[Pb (CH3COO)4] + (NH4)2SO 4
(NH4)2 [Pb(CH3COO)4] + K2CrO4 PbCrO4 + 2CH3COOK + 2(NH4) 2SO 4

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 H2SO 4 + 2NO
2Cu2+ + SO24 +2NH3+2H2O Cu(OH) 2. CuSO4+ 2NH +4
2
Cu(OH)2.CuSO4 + 8NH 3 2 [Cu(NH3)4]SO4 + 2OH + SO4
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.Cu 2[Fe(CN)6].
[Cu(NH3)4] SO4 + 4CH3COOH CuSO4 + 4CH3COONH4
2CuSO4 + K4[Fe(CN)6] Cu2[Fe(CN)6] + 2K2SO4

Potassium Copper
hexacyanoferrate (II) hexacyanoferrate (II)
(Chocolate brown precipitate)
Group-II B (Arsenic Group)
If group- II precipitate dissolves in yellow ammonium sulphide and the colour of

the solution is yellow, this indicates the presence of As3+ 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
precipitate is formed. This confirms the presence of As3+ 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
H 3AsO4 + 12(NH4)2 MoO4 + 21HNO3 (NH4)3[As (Mo3 O10)4] + 21NH4NO3 +12H2O

Arsenic acid Ammonium Ammonium
molybdate 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 Fe 3+ 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
precipitate indicates the presence of aluminium ion (A13+ ). 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
Brown precipitate White precipitate

3+ 3+
Fe Al
Dissolve the precipitate in dilute HCl Dissolve the white precipitate in dilute
and divide the solution into two parts. HCl and divide into two parts.
(a) To the first part add potassium (a) To the first part add sodium hydroxide
ferrocyanide solution [Potasium solution and warm. A white
hexacyanoferrate (II)]. A blue gelatinous precipitate soluble in
precipitate/colouration appears. excess of sodium hydroxide solution.
(b) To the second part add potassium (b) To the second part first add blue
thiocyanate solution. A blood red litmus solution and then ammonium
colouration appears. 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.
1. Test for Aluminium ions (A13+ )
(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
Al(OH)3 + NaOH NaAlO 2 + 2H2O

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] Fe 4[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] KFe[Fe(CN)6] + 3KCl
(Soluble prussian blue)
(b) 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.
Fe3+ + SCN [Fe(SCN)] 2+
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 Flesh coloured precipitate Black precipitate

2+ 2+ 2+ 2+
(Zn ) (Mn ) (Ni , Co )
Dissolve the precipitate Dissolve the precipitate in Dissolve the precipitate in

in dilute HCl by boiling. dilute HCl by boiling, then add aqua regia. Heat the
Divide the solution into sodium hydroxide solution in solution to dryness and
two parts. excess. A white precipitate is cool. Dissolve the residue
formed which turns brown on in water and divide the
(a) To the first part add
keeping. solution into two parts.
sodium hydroxide
solution. A white (a) To the first part of the
precipitate soluble solution add ammonium
in excess of sodium hydroxide solution till it
hydroxide solution becomes alkaline. Add
confirms the a few drops of dimethyl
2+
presence of Zn glyoxime and shake the
ions. test tube. Formation of
a bright red precipitate
(b) Neutralise the
confirms the presence
second part with 2+
of Ni ions.
a m m o n i u m
hydroxide solution (b) Neutralise the second
and add potassium part with ammonium
ferrocyanide hydroxide solution.
solution. A bluish Acidify it with dilute
white precipitate acetic acid and add
appears. 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.
1. Test for Zinc ion (Zn2+ )
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.
This confirms the presence of Zn2+ ions.
ZnCl2 + 2NaOH Zn(OH)2 + 2NaCl
Zn(OH)2 + 2NaOH Na2ZnO2 + 2H2O

Sodium zincate
(b) 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
MnCl2 + 2NaOH Mn(OH)2 + 2NaCl

(White precipitate)
Mn (OH)2 + [O] MnO(OH)2

Hydrated manganese dioxide
(Brown colour)
3. Test for Nickel ion (Ni2+)

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
(NH 4)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+
Ba ions Sr ions Ca ions
(a) To the first part add (a) If barium is absent, take (a) If both barium and
potassium chromate second part of the solution strontium are absent,
solution. A yellow and add ammonium take the third part of
precipitate appears. sulphate solution. Heat the solution. Add
and scratch the sides of the ammonium oxalate
(b) Perform the flame test tube with a glass rod solution and shake
test with the and cool. A white well. A white
preserved precipitate. precipitate is formed. precipitate of calcium
A grassy green flame oxalate is obtained.
is obtained. (b) Perform the flame test with
the preserved precipitate. (b) Perform the flame test
A crimson-red flame with the preserved
confirms the presence of precipitate. A brick red
Sr2+ ions. 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.
1. Test for Barium ion (Ba2+ )
(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 + 2CH 3COOH (CH 3COO)2 Ba + H2O + CO2
(CH3COO)2Ba + K 2CrO4 BaCrO4 + 2CH3COOK

Barium chromate
(yellow precipitate )
(b) 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. Test for Strontium ion (Sr2+ )
(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 SrSO 4 + 2CH 3COONH4

Strontium
sulphate
(White precipitate)
(b) Flame test Perform the flame test as given in the case of Ba2+. A crimson
red flame confirms the presence of Sr2+ 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 + 2CH 3COOH (CH 3COO)2 Ca + H2O + CO2
(CH3COO)2Ca + (NH4)2C2O4 (COO)2Ca + 2CH3COONH4

Ammonium Calcium oxalate
oxalate (White precipitate)
(b) Flame test Perform the flame test as mentioned above. Calcium imparts
brick red colour to the flame which looks greenish-yellow through blue glass.
110
(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
Note :
is soluble in water in the presence of ammonium salts because the Some times
equilibrium is shifted towards the right hand side. precipitate of
magnesium
NH4+ + CO 2-
3

NH3 + HCO 3 ammonium
phosphate
The concentration of carbonate ions required to produce a precipitate is appears
not attained. When disodium hydrogenphosphate solution is added and after some
the inner walls of the test tube are scratched with a glass rod, a white time. So
crystalline precipitate of magnesium ammonium phosphate is formed which warm the
indicates the presence of Mg2+ ions. solution and
scrach the
2+
Mg + Na2HPO4 Mg (NH 4)PO4 + NH4OH + 2Na+ + H2O sides of test
tube after
a d d i n g
Magnesium ammonium s o d i u m
phosphate (White precipitate) hydrogen
phosphate
Note down the observations and the inferences of the qualitative analysis solution.
in tabular form as given in the specimen record given in pages 114-115.
Precautions
(a) Always use an apron, an eye protector and hand
gloves while working in the chemistry laboratory.
(b) Before using any reagent or a chemical, read the
label on the bottle carefully. Never use
unlabelled reagent.
(c) Do not mix chemicals and reagents
unnecessarily. Never taste any chemical.
(d) Be careful in smelling chemicals or vapours.
Always fan the vapours gently towards your
nose (Fig. 7.9).
(e) Never add sodium metal to water or throw it in
the sink or dustbin.
(f) Always pour acid into water for dilution. Never
add water to acid.
(g) Be careful while heating the test tube. The test
tube should never point towards yourself or
towards your neighbours while heating or
Fig. 7.9 : How to smell a gas
adding a reagent.
111
(h) Be careful while dealing with the explosive compounds, inflammable substances,
poisonous gases, electric appliances, glass wares, flame and the hot substances.
(i) Keep your working surroundings clean. Never throw papers and glass in the
sink. Always use dustbin for this purpose.
(j) Always wash your hands after the completion of the laboratory work.
(k) 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 H2SO 4?
(v) Why is dilute H2SO 4 preferred over dilute HCl while testing anions?
(vi) Name the anions detected by conc. H2SO 4.
(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 White Cu , Fe , Ni ,Co ,
2+
salt. Mn are absent.
2 2
2. Noted the smell of the salt. No specific smell. S , SO3 , CH3 COO
may be absent.
2
3. Heated 0.5 g of the salt in a (i) No gas was evolved. (i) CO 3 may be

dry test tube and noted the present, NO3 , NO2 ,

colour of the gas evolved and Br may be
change in the colour of the absent.
2+
residue on heating and (ii) No particular (ii) Zn may be
cooling. change in colour of absent.
the residue is
observed when
heated and when
cooled.
2+ 2+ 2+ 2+
4. Prepared a paste of the salt No distinct colour of the Ca , Sr , Ba Cu
with conc. HCl and performed flame seen. may be absent.
the flame test.
5. Borax bead test was not

performed as the salt was
white in colour.
2 2 2
6. Treated 0.1 g of salt with 1 mL No effervescence and CO3 , SO 3 , S , NO2 ,
dil.H2 SO4 and warmed. evolution of vapours. CH3COO absent.

7. Heated 0.1 g of salt with 1 mL No gas evolved. Cl , Br , I , NO3 , C2 O4
conc. H2SO4. are absent.
3
8. Acidified 1mL of aqueous salt No yellow precipitate PO4 absent.
solution with conc. HNO 3 .
Warmed the contents and then
added 4-5 drops of ammonium
molybdate solution.
114
2
9. Acidified water extract of the A white ppt. is obtained SO4 present.
salt with dil. HCl and then which is
added 2mL of BaCl2 solution. insoluble in conc. HNO3
and conc. HCl.
+
10. Heated 0.1 g of salt with 2 mL Ammonia gas is not NH4 absent.
NaOH solution. evolved.
11. Attempted to prepare original Clear solution formed Water soluble salt is
solution of the salt by present.
dissolving 1g of it in 20 mL
water.
12. To a small part of the above No white precipitate GroupI absent.

salt solution added 2 mL of formed.
dil. HCl.
13. Passed H 2S gas through one No precipitate formed. GroupII absent.

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

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.
15. Passed H2 S gas through the No precipitate formed. GroupIV absent.

above solution.
16. Added excess of ammonium No precipitate formed. GroupV absent.

hydroxide solution to the
original solution and then
added 0.5 g of ammonium
carbonate.
2+
17. To the original solution of salt White precipitate. Mg confirmed.
added ammonium hydroxide
solution, followed by disodium
hydrogen phosphate solution.
Heated and scratched the
sides of the test tube.
Result
The given salt contains:
2
Anion : SO4
Cation : Mg2+
115
PROJECTS
BACKGAROUND INFORMATION
ABOUT I NVESTIGATORY 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.
M ANAGING 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
L ABORATORY 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, card-
board 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 W ORK
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 Na 2S2O 3, 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 H 2S. 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
Fe2+ 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) To determine the amount of acids present in various
vegetables and fruits.
(b) To detect the presence of iron, carbohydrate, protein and
sugar etc. in vegetables and fruits.
124
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 HNO 3 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
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
Hazard Warning and densities are d1 and respectively d2 then the following relation
Acetone and alcohols are holds:
inflamable, do not let the
bottles open when not in
1 d1 t 1
use. =
Keep the bottles away 2 d2 t 2
from flames.
Wash your hands after
use. Hence if the viscosity of one liquid is known, the viscosity of
Wear safety spectacles. 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
Time of flow Density Viscosity

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

Sl. No. Name of the compound
mass (Seconds) (g/mL) (millipoise)
1. Water 18 180 1 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

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Laboratory Manual

P ROFESSOR YASH PAL

UNIT-2 : Basic Laboratory Techniques 16

UNIT-3 : Purification and Criteria of Purity 38

UNIT-4 : Chemical Equilibrium (Ionic Equilibrium in Solution) 46

UNIT-5 : pH and pH Change in Aqueous Solutions 53

UNIT-6 : Titrimetric Analysis 65

UNIT-7 : Systematic Qualitative Analysis 79

In order to become proficient in basic principles underlying

1.1 DO S AND DON TS IN A CHEMISTRY LABORATORY

The practices outlined below are designated to guide you in

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

Fig. 1.1 : Correct method of heating

The indication for cleanliness of glass apparatus is that

1.2 A NALYTICAL METHODS

Elements and their compounds may be detected by their physical

1.3 BASIC LABORATORY EQUIPMENT AND PROCEDURES

Heating, filtration, decantation, measuring volumes and

Fig. 1.2 : Common laboratory equipments

Fig. 1.3 : Common laboratory glass apparatus

Fig. 1.4 : Stand carrying boiling tubes and

Condensers Fig. 1.5 : Separating funnels

Ground Glass Joints

Fig. 1.7 : Apparatus with ground glass joints

1.4 HANDLING REAGENT BOTTLES

Correct methods for taking out solid and liquid reagents

Fig. 1.9 : Methods of pouring liquids

If dropper is used for transferring the

1.5 HEATING DEVICES

Heating during the laboratory work can be

(A) Parts of Bunsen Burner

2. The Burner Tube

3. The Air Regulator

Fig. 1.11 : Bunsen burner Fig. 1.12 : Parts of Bunsen burner

Fig. 1.13 : Zones of flame of Bunsen burner

(B) Principal Parts of Bunsen Flame

1. The Inner Dark Cone, A E C

2. The Middle Blue Cone, A D C E A

3. The Outer Non-luminous Mantle, A B C D A

Bunsen identified six different regions in these three

(i) The upper oxidising zone (f)

(ii) Upper reducing zone (e)

(iii) Hottest portion of flame (d)

(iv) Lower oxidising zone (c)

(v) Lower reducing zone (b)

(vi) Lowest temperature zone (a)

(C) Striking Back of the Bunsen Burner

KEROSENE HEATING LAMP

Working of the Kerosene Lamp

Fig. 1.15 : Parts of Kerosene Heating Lamp

2.1 CUTTING OF GLASS TUBE AND G LASS ROD

Soda-glass tube : 15 cm long

(a) (b) (c)

Fig. 2.1 : (a) Marking a glass rod or a glass tube

After continuously warming Properly Overheated

(i) Why does glass not possess a sharp melting point?

2.2 BENDING OF A GLASS TUBE

Glass tube : 20-25 cm long