Chemistry EM PDF

Intermediate Practical Manual
Chemistry
Authors
Dr. K. Venkateswara Rao
Reader in Chemistry (Retd.)
New Science College
Hyderabad
M. Gopala Krishna
Lecturer in Chemistry (Retd.)
Govt. Junior College
Malkajgiri, Hyderabad
K. Sridevi
Jr. Lecturer in Chemistry
Govt.Junior College
Kachiguda, Hyderabad
Editor
Prof. M. Adinarayana
Professor (Retd.)
Department of Chemistry
Osmania University, Hyderabad
Andhra Pradesh State Board of Intermediate Education

Intermediate Board, Tadepalli, Guntur Dist., A.P.
Intermediate :Chemistry Practical Manual : Authors : Dr. K. Venkateswara Rao, Smt. K. Sridevi,
Sri M. Gopala Krishna, Editor : Prof. M. Adinarayana, Reprint:2021; Pp.x+194+iv+iv.
c
Board of Intermediate Education
Tadepalli
Printing, Publishing and Districution rights

are exclusively with Intermediate Board, Tadepalli, Guntur.
First Edition : 2013

Reprint : 2023
Copies : 4000
All rights whatsoever in this book are stictly reserved and no

portion of it may be reproduced by any process for any purpose
without the written permission of the copyright owners.
Price : Rs.
Printed in India
Laser Typeset by M/s StockAssortment, Bapatla.
Printed at M/s
Academic Review Committee
Syed Omer Jaleel, IAS

Commissioner, Intermediate Education, Telangana State &
Secretary, Telangana State Board of Intermediate Education
Smt. M. Radha Reddy, Member

Director, SCERT, Telangana State
Sri M. Somi Reddy - Member

Telugu Akademi, Hyderabad
Educational Research & Telugu Akademi

Training Wing,BIE Coordinating Committee
Sri M. Somi Reddy, M.A., B.Ed.

Sri V. Ramana Rao Director
Reader
Dr. M. Venkatesham M.A., L.L.B., Ph.D.
Smt K. Vasundhara Devi Deputy Director(FAC)
Asst. Professor
Dr. Nomula Yogi Babu, M.Sc., M.Ed. Ph.D.
Research Assistant (Chemistry)
Dr. S.A.T. Rajyalakshmi, M.Sc., B.Ed., M.A., Ph.D.

Research Assistant (Chemistry)
Academic Review Committee :
Sri M.V. Seshagiri Babu,
Secretary & Commissioner, Intermediate Education. A.P.
Sri K. Chandra Sekhar Rao,

Honorary Advisor, Intermediate Education. A.P.
Educational Research &

Training Wing, BIE
Dr. A. Srinivasulu,
Professor
Dr. D. Gopal Reddy,

Reader
Sri M. Ravi Sankar Naik,

Assistant Professor
Dr. M. Ramana Reddy,

Assistant Professor
Sri J.V. Ramana Gupta

Assistant Professor
Practical Manual Scrutiny Committee Members

G.J.V.S.N.D Lakshmi
JL in Chemistry, VVR GJC, Mylavaram.
G. Aruna Sree
JL in Chemistry, MVN & YVN GJC, Agiripalli.
Layout & Drawings

M/s StockAssortment, Bapatla.
FOREWORD
The importance of Laboratory Practicals in the teaching of science subjects cannot be

over-emphasized. Laboratory Practicals provide a unique opportunity for students to understand
clearly and assimilate theoretical concepts which may seem complex or dry when taught in
the classroom. Practicals, like field work, are an invaluable tool in enhancing the richness of
the learning experience. On the one hand they promote creativity and the spirit of questioning
by drawing out the skills of interpretation and the ability to evaluate evidence. On the other
hand, they foster logical thinking because of the emphasis on systematic procedures to be
followed, correct methods of handling data as well as accurate and authentic reporting of
observations.
The Board of Intermediate Education, has recognized the need for Laboratory Practicals
for Intermediate science students since its inception. Further, an attempt is being made to
constantly update the syllabus, not only in theory, but also in practicals, to reflect the changing
needs of the day. While the textbooks in science subjects were revamped over the last 2 years
in accordance with the NCERT syllabus, the syllabus in practicals too is being modified for
students of both 1st year and 2nd year Intermediate from the academic year 2013-2014. It is
hoped that the new syllabus will make practicals more exciting and interesting for students
and will maximise their learning experience. Practical training would also benefit students by
honing their creative skills, critical thinking and communication skills, thereby making the
students more competent and confident to face the challenges ahead. The present Laboratory
Manual provides in a succinct manner the guidance required for conducting the various
experiments in the laboratory. The Manual will be a useful tool for students and will supplement
the efforts of the teachers in making practicals a challenging the thrilling experience.
I thank the authors, editors and the members of ERTW who are involved in the
preparation of these practical manuals. Constructive suggestions are solicited for the
improvement of these lab manuals in terms of standardization and comprehension.
Secretary
PREFACE
The Practical Manual in Chemistry for Intermediate course is written strictly according
to the revised syllabus in one volume for both first and second years . The syllabus is designed
with a view to impart hands on skills and create awareness about scientific thinking and
scientific methods of analysis among the young students . The experiments are presented
with detailed explanations and illustrations wherever required . Various apparatus used in
chemistry laboratory and basic laboratory techniques such as heating a solution , measuring
volume of liquids , cutting , bending a glass tube , drawing a glass jet , boring a cork , filtration
are included . The titrimetric analysis experiments are presented along with calculations . In
qualitative analysis various tests have been given in a systematic order . Model analysis for
simple salts and identification of functional groups of organic compounds have been included
. Qualitative tests for carbohydrates and proteins are explained . Experiments in chromatography
, electrochemistry , colloidal state are presented with detailed discussion and illustrations .
For each practical work principle , brief theory , material required , procedure , precautions
are given . At the end of each chapter questions for discussion are given , which helps in
knowing the theoretical aspects of experiments . Some investigatory projects are included in
this book and the students themselves have to perform these projects individually with the
guidance of the teacher . The project work is so designed that it would inculcate the ability to
design the experiment , to make observations and to draw the conclusions out of experimental
data . The safety aspects in chemistry laboratory are given for safe carrying out of experiments
with various chemicals . Some common reagents used in chemistry laboratory and their
preparation are included in the manual . Due emphasis has been given to present the topics in
simple and lucid way in this manual.
We consider that this manual will be highly helpful for intermediate students . Though
we tried our best with utmost care there may still be some occasional errors . We will be glad
to correct them in future editions and all constructive suggestions will be taken up for the
improvement “of this manual .
Editor
CONTENTS
FIRST YEAR
CHAPTER 1
INTRODUCTION 1-6
1.1 Do's in a Chemistry Laboratory 1
1.2 Some don'ts in a Chemistry Laboratory 2
1.3 Basic Laboratory Equipment 3
1.4 Safety measures in Chemistry Laboratory 4
1.5 Emergency First - aid in Chemistry Laboratory 5
CHAPTER 2
BASIC LABORATORY TECHNIQUES 7-20
2.1 Bunsen Burner 7
2.2 Cutting a Glass Tube and a Glass Rod 10
2.3 Bending a Glass Tube 11
2.4 Drawing a Glass Jet 12
2.5 Bering a Cork 13
2.6 Heating Solution in a Test Tube 14
2.7 Heating Solution in a Beaker 14
2.8 Filtration 14
2.9 Measuring Volume of Liquids 15
2.10 Wash Bottle 18
CHAPTER 3
MELTING . BOILING POINT OF COMPOUNDS &
PURIFICATION OF CHEMICAL SUBSTANCES 21-26
Experiment : 3.1 Determination of Melting Point of an Organic Compound 21
Experiment : 3.2 Determination of Boiling Point of an Organic Compound 23
Experiment : 3,3 Purification of a Chemical Substance by Crystallisation 24
CHAPTER - 4
pH AND pH CHANGE IN AQUEOUS SOLUTIONS 27-32
Experiment : 4.1 Determination of pH of Same Concentrations of Acids,
Bases and Salts in Aqueous Solution 28
Experiment : 4.2 Determination of pH of Some Fruit Juices 29
Experiment : 4.3 Variation of pH of Acid / Basc / Salt Solutions with Dilution 30
Experiment : 4.4 pH of Solutions of Strong Acid and Weak Acid of
Same Concentration 31
Experiment : 4.5 pH Change During the Titration of Strong Acid and Strong Base 31
CHAPTER - 5
CHEMICAL EQUILIBRIUM 33-37
Experiment : 5.1 Study the Shift in Equilibrium in the Reaction of Ferric Ions
and Thiocyanate Ions by Changing the Concentration
of any one of These Ions 34
Experiment : 5.2 Study the Shift in Equilibrium Between [ Co6( H2O )6] 2+ and
Chloride Ions by Changing the Concentration of either of the Ions 36
CHAPTER 6
QUANTITATIVE ESTIMATION ( TITRIMETRIC ANALYSIS ) 38-49
6.1 Chemical ( Analytical ) Balance 38
6.2 Preparation of Standard Solution of Oxalic Acid 40
6.3 Indicators in Acid - Base Titrations and Redox Titrations 42
6.4 Estimation of NaOH Present in the Given Solution Titrimetrically with
Standard Oxalic Acid Solution 43
6.5 Preparation of Standard Solution of Sodium Carbonate 45
6.6 Determination of the Strength of the Given Hydrochloric Acid 46
6.7 Precautions During Titrimetric Analysis 48
CHAPTER 7
QUALITATIVE ANALYSIS 50-81
7.1 Introduction 50
7.2 Reactions of Anions 51
7.3 Tests for Confirmation of Anions 63
7.4 Reactions of Cations 65
CHAPTER 8
DETECTION OF ELEMENTS IN ORGANIC COMPOUNDS 82-86
8.1 Introduction 82
8.2 Detection of Nitrogen , Sulphur by Lassaigne's Test 82
8.3 Detection of Halogens by Lassaigne's Test 84
PROJECTS 87-92
SECOND YEAR
CHAPTER 1
SURFACE CHEMISTRY 93-97
Experiment : 1.1 Preparation of Some ( a ) Lyophilic Sols and ( b ) Lyophobic Sols 94
Experiment : 1.2 Purification of a Sol by Dialysis 95
Experiment : 1.3 Role of Emulsifying Agents in Stabilizing the Emulsions
of Different Oils 96
CHAPTER 2
CHEMICAL KINETICS 98-106
Experiment : 2.1 Effects of Concentration and Temperature on the Rates of Reaction
A Practical Study of the Rate of Reaction Between Sodium
Thiosulphate and Hydrochloric Acid 98
Experiment : 2.2 Effect of Variation of on the Rate of a Reaction Between 101
lodide Ions and Hydrogen Peroxide at Room Temperature
Experiment : 2.3 Rate of Reaction Between Potassium lodide ( KI ) and Potassium
Peroxodisulphate ( Persulphate ) Solutions 102
Experiment : 2.4 Reaction Between Potassium Iodate ( KIO , ) and
Sodium Sulphite ( Na , SO , ) using Starch Solution as Indicator
( Clock Reaction ) 104
CHAPTER 3
THERMOCHEMISTRY 107-114
Experiment : 3.1 Determination of the Enthalpy of Solution of Potassium Nitrate or
Copper Sulphate in Water 108
Experiment : 3.2 Enthalpy of Neutralization of Strong Acid ( HCI ) with
a Strong Base ( NaOH ) 110
Experiment : 3.3 Experimental Determination of the Enthalpy Change for
the Reaction Between Acetone and Chloroform 112
CHAPTER 4
ELECTROCHEMISTRY 115-118
4.1 Effect of Concentrations of Electrolytes on the Cell Potential of a Galvanic Cell 115
4.2 Conventions Regarding a Galvanic Cell 115
4.3 Nernst Equation 115
4.4 Experiment : 4.1 Study of the Variation in the Cell Potential of Daniel Cell
at Room Temperature with change in concentration 116
CHAPTER 5
CHROMATOGRAPHY 119-122
Experiment : 5.1 Separation of Pigments Present in the Extracts of
Leaves and Flowers 119
Experiment : 5. 2 Separation of Ions Pb²- and Cd² + in a Mixture of
Compounds Using Chromatographic Technique 121
CHAPTER 6
PREPARATION OF INORGANIC COMPOUNDS 123-126
Experiment : 6.1 Preparation of Ferrous Ammonium Sulphate ( Mohr's Salt ) 123
Experiment 6.2 Preparation of Potash Alum 124
Experiment : 6,3 Preparation of Potassium Trioxalatoferrate ( III ) 125
CHAPTER - 7
PREPARATION OF ORGANIC COMPOUNDS 127-131
Experiment : 7.1 Preparation of Acetanilide 127
Experiment :7.2 Preparation of Dibenzalacetone 129
Experiment : 7.3 Preparation of Phenyl - azo-B -Naphthol 130
CHAPTER 8
TESTS FOR FUNCTIONAL GROUPS IN ORGANIC COMPOUNDS 132-140
Systematic analysis for identification of
( i ) Carboxyl Group ( -COOH ) 132
(ii) Aldehydic Group ( -CHO ) 133-134
( iii ) Ketonic Group ( > C = 0 ) 133-134
( iv ) Alcoholic Group ( -OH ) 134
( v ) Phenolic Group ( Ar - OH ) 135
( vi ) Amino Group ( -NH2 ) 135
CHAPTER - 9
CHARACTERISTIC TESTS FOR CARBOHYDRATES AND PROTEINS 141-143
9.1 Carbohydrates 141
9.2 Qualitative Tests for Carbohydrates 141
9.3 Proteins 142
9.4 Qualitative Tests for Proteins 142
CHAPTER - 10
QUANTITATIVE ESTIMATION 144-149
( REDOX REACTIONS )
Experiment : 10.1 Determination of the Strength of Potassium Permanganate 144
Experiment : 10.2 Estimation of Potassium Permanganate 147
10.3 Precautions During Titrimetic Analysis 148
CHAPTER - 11
QUALITATIVE INORGANIC ANALYSIS 150-174
( i ) Preliminary Tests 152
( ii ) Analysis of Anion 153
( iii) Analysis of Cation 156
( iv) Model Analysis of Simple Salts ( I to VI ) 161
PROJECTS 175-182
Appendix - I Syllabus I year and II year 183
Appendix - II Common Reagents Used in Chemistry Laboratory 187
FIRST YEAR
.
CHAPTER-1
INTRODUCTION
Chemistry is an experimental science and deals with experimental observations. Many theo-
ries that are learned are to be verified experimentally and the observations are noted and inferences are
drawn and the results are to be correlated with the theories. As such, experiments are to be performed
with so many instruments apparatus and chemicals in a place known as chemistry laboratory. A
laboratory provides us with an opportunity to become an observer and to draw inferences, explain the
results and verify the theoretical interpretations.
A student need the training skills to perform experimnts in a laboratory like handling various
appartus and chemicals used in the laboratory. Before going to learn the training skills, let us first
know what are the things that a chemistry laboratory is provided with. When you enter a chemistry
laboratory, you find that the laboratory is provided with working tables, water-taps, gas-taps, bunsen
burners, a reagent shelf consists of reagents often used is fixed on the working table. Some other
reagent shelves are fixed to the side walls of the laboratory, where the reagents that are not often used
are kept. Besides this, exhaust fans are provided which facilitates the exhaustion of harmful fumes and
for circulation of fresh air. Apart from these things, a chemistry laboratory is provided with well
ventilated windows and a fume cup board for those experiments in which fumes are produced and a
first-aid box and a balance room.
The students performing experiments in a chemistry laboratory are advised that they should be
familiar with practices, procedures and more importantly with the precautions to be taken while work-
ing in a laboratory. Sometimes the experiments are to be performed with such chemicals which pro-
duces poisonous fumes, causing potential danger. So to become proficient and familiar with basic
principles of a laboratory, you should be familiar with things like handling the equipment (appartus
and chemicals). There are certain safety rules (do’s and don‘ts) to ensure that the work done in the
laboratory is safe for you and to the fellow students.
The following instructions are to be scrupulously followed for safe working in a chemistry laboratory.
1.1 Do’s in a Chemistry Laboratory
1. A student should come to the laboratory with lab coat on and wearing safety glasses. Must
bring a pen or pencil, observation notebook and other materials like fractional weight box,
platinum wire.
2. Read the name of the reagent on the label of the reagent bottle, before using it to ensure that
you are using the right reagent.
3. Thoroughly clean the appartus before its use.
4. Keep the reagent bottles properly closed and keep them at their place after use.
5. As far as possible use small or required quantities of chemicals, avoid excessive use of
reagents.
6. Do only the experiments allotted to you with required appartus and chemicals. Unallotted
experiments should not be done.
7. While performing the experiments, record the observations properly and immediately after a
reaction or experiment is completed. Do not wait till last.
8. Care should be taken to handle glass appartus. If any breakage is noticed do not use that appartus.
9. Clean all the appartus after you finish the experiment.
10. Dispose off the waste liquids in the sink and allow the water to run for sometime by opening
the water tap.
1.2 Some don’ts in a chemistry Laboratory
1. Never mix the chemicals unless it is required in the experiment.
2. Do not handle the glassware roughly, as it may result in their breakage.
3. Do not touch any chemical with hands as some of the chemicals are corrosive.
4. Do not keep the reagent bottles at your seat after you have finished using them.
5. Never throw used match sticks, litmus papers, broken glass appartus, filter papers or any other
material on the floor. Dispose them off in the waste bin provided for that purpose.
6. Do not heat a substance by keeping the test tube near your eyes and the test tube should not be
kept towards yourself. Heat a test tube by keeping it slightly inclined and moving and shaking
to ensure uniform heating.
7. Do not heat the appartus which is made of thick glass, e.g., graduated cylinder, bottles,
measuring flasks etc., as these break on heating. Test tubes may break if they are heated above
the level of the liquid filled in them.
8. Do not heat beakers and other glassware and china dish directly on flame. Use wire gauze.
9. Do not waste water or gas or chemicals as they are expensive.
10. Do not use the same dropper for all reagent bottles. Separate droppers are to be used for
different reagent bottles.
11. Hot appartus 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.
12. Never add water to acid for dilution. Always add acid to water while diluting a concentrated
acid.
13. Do not use broken or cracked glassware like beakers for heating purpose.
14. Do not bring inflammable chemicals near the flame.
15. Do not keep open the reagent bottles after their use. They should be properly closed.
16. Do not throw concentrated acids into the water sink,especially sulphuric
acid. Pour them into the sink after diluting and cooling.
2 Chemestry Practical Manual

17. Do not use laboratory water for drinking purposes.
18. Do not inhale poisonous and suffocating vapours evolved during the reactions. Keep the test
tube away and clean the test tube immediately after the test.
19. Do not write your observations in a rough note book. Use observation note book for the
purpose.
20. Follow the instructions of your teacher regarding the conduct of the experiment.
In chemistry laboratory, a substance is tested qualitatively by its colour, physical appearence,
odour etc. But this will not give complete picture of the substance of its chemical nature. Hence, some
tests and reactions are to performed to know its qualitative nature. Thus experiments are to be
conducted for analysing a substance qualitatively. This is known as qualitative analysis. Substances
in chemical reactions react quantitatively to give products. Thus, the experiments performed to
determine the quantity of the chemical substances that take part in chemical reactions comes under the
category of quantitative analysis. So, qualitative analysis is used to detect the elemental composition
of a substance, while quantitative analysis helps in establishing the quantitative relation of the
substances that take part in chemical reactions. We use different appartus in chemistry laboratory to
carry out both qualitative and quantitative analysis. Let us see the basic laboratory equipment used in
chemistry laboratory.
1.3 Basic Laboratory Equipment
1. Test tubes : Test tubes of different volumes are available. 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. The test tubes of bigger diameter are called boiling test tubes, used for boiling large
quantities of liquids.
2. Beakers : Beakers of different volumes such as 500 mL, 250 mL, 100 mL etc., are avail able.
Beakers made of borosilicate glass are durable and withstand high temperatures.
3. Conical flasks : Conical flasks of different volumes such as 250 mL, 100 mL etc., are avail-
able. Conical flasks are used to carry out titrations in quantitative analysis.
4. Funnels : Funels are used for filtration. Separating funnel is used for separation of immiscible
liquids.
5. Measuring cylinders : Measuring cylinders are available in different volumes ranging from 5
mL to 1000 mL. These are used for measuring the volume of liquids.
6. Measuring flasks : Measuring flasks are also called volumetric flasks or standard flasks and
are used for preparing a particular volume of a standard solution in quantitative analysis. These
are available in different volumes like 1000 mL, 500 mL, 250 mL and 100 mL.
7. Burettes : Burettes are made of glass. Now a days plastic burettes are also available. There are
two types of burettes available namely stopper type and pinch cock type. These are available in
50 mL and 25 mL capacities. Burettes are used in quantitative analysis for carrying out
volumetric titrations.
8. Pipettes : Pipettes are used to measure exact volume and transfering of liquids. pipettes are
available in different volumes like 5 mL, 10 mL, 20 mL, etc., Graduated pipettes are also
available to measure lower volumes.
First Year 3
9. Glass rod : Glass rod is used for stirring purpose and for transfering liquids into the funnel.
10. China dish : China dish is a small porcelain vessel used for concentrating a solution in
crystallisation.
11. Tripod stand : Tripod stand is used for supporting a china dish or a beaker so that it can be
heated from below.
12. Wire gauze : It is placed above the flame of the burner so that the glass vessel being heated
does not touch the flame directly and hence prevented from breaking. Wire gauze has asbestos
layer which protects the vessel from high temperatures.
Apart from above equipment, a student must be familiar with other apparatus also. They include
test tube holder, test tube brush, spatula, tongs, watch glass, clamp, stand, water bath, sand bath,
crucible, centrifuge tube, wash bottle, platinum wire, mouth blow pipe, desiccator, reagent bottles,
round bottomed flask etc.
1.4 Safety Measures in Chemistry Laboratory
The teacher/instructor is responsible for instructing the students as to the risks to which they are
subjected when working in a chemistry laboratory, as well as to the basic safety measures, and first
aid. Specific behavioural and safety measures must be obeyed to prevent accidents.
Rules in the lab
1. Use protective clothing all the time (e.g. lab coat and safety glasses)
2. Use a hair band to keep your hair away from your face.
3. Do not place the chemical on the palm of your hand.
4. Work carefully and follow the given instructions.
5. Follow the safety instructions for handling chemicals.
6. Do not leave laboratory without premission.
7. Keep the work place clean and organized.
8. Care should be taken to handle glass apparatus. If any breakage is noticed do not use that
apparatus.
9. Do not cause panic in case an unwanted chemical reaction, equipment damage or injury. Call
the teacher.
10. Work in the fume cupboard, whenever you work using hazardous or toxic substances, for
experiments where easily evaporable substances or chemical are employed. for experiments
where flammable gases and vapours are produced.
11. Use electric heaters to heat the receptacles with flammable substances. Do not expose them to
an open flame.
12. Wear protective gloves and safety glasses while working with concentrated acids or alkalis, or
whenever the mixture might react quickly and aggressively.
13. In case a chemical comes in contact with your skin, immediately rinse the spot with water and
neutralise if necessary. Remove the affected clothing. In case a chemical comes in contact
with your eye(s), wash it (them) with running water for 15 minutes go for medical treatment.

14. Do not pipette harmful or evaporable substances by mouth. Use a pipette-bulb.
15. Disposal of the waste material: You are allowed to pour neutral are very dilute solutions
down the drain, but with a lot of running water. Neutralise any acids and alkalis before pouring
them down the drain.
16. Before leaving the laboratory: Ensure that your work place is neat and clean. All the chemi-
cal containers must be close and returned to their designated places. Shut off the gas and water
valves. Switch off the electric heaters and other equipment.
17. Wash your hands before leaving the laboratory.
1.5 Emergency First-Aid in chemistry Laboratory

While working in the chemistry laboratory, you may encounter cuts, burns, injuries caused by
chemicals (skin, eyes) or poisoning caused by inhaling poisonous vapours or swallowing poisonous
substances. There is always a risk or fires, explosion and electric shocks. In order to avoid all these
dangers in the laboratory, you need to respect the above mentioned safety measures. It is also
important that you react in time to help yourself and others.
CUTS are usually found on hands, and are mostly caused by glassware. verify if there is a shred of
glass, metal or other material in the wound. Use sterile tweezers to pull it out, cover the injury with a
piece of sterile gauze or bandage, and apply pressure to stop the bleeding. In case of profuse bleeding,
apply a compression bandage and seek medical help.
BURNS are usually found on hands too, and are mostly caused by handling hot objects or hot
reagents. If there is no significant damage to the skin, cool the burned spot with cold water (or ice
placed on a sterile cover). In case the clothing has become stuck to the skin and blisters have formed,
use a piece of sterile gauze to cover the burn and immediately seek medical help.
Chemical injuries to skin
If a chemical has come in contact with your skin, rinse the spot with running water and neutralise
if necessary (acids should be neutralised with saturated solution of sodium bicarbonate, and alkalies
with a 2% solution of acetic acid).
In case of more severe skin damage, cover the spot with a piece of sterile gauze and seek medical
help. In case your eye(s) come in contact with any kind of chemical, wash it (them) with running water
(for at least 15 minutes) and seek medical help.
Poisining caused by inhaling poisonous vapours
The affected person has to be carried out, where he or she can inhale fresh air. Remove the affected
clothing and seek medical help if necessary. If the person has lost consciousness, position him or her
on his or her side, and immediately seek medical help. If necessary, apply the CPR technique.
Poisoning caused by swallowing chemicals
The stomach contents have to be diluted with large quantities of water. If you know the
composition of the substance swallowed, you can induce vomiting. Thisis not advisable when
concentrated acid or alkali is swallowed. In such case the person should drink large quantities of water
and seek medical help.
First Year 5
Injuries caused by electric shock
Electric shocks can be caused by faulty wiring. Shut off the source of electric power using insulted
equipment. Remove the affected person from the electric circuit and if necessary, apply the CPR
technique. Seek medical help.
Fires and explosions
The most frequent causes of fires and explosions in the laboratory are the faulty gas fittings,
mishandling of easily flammable substances (white phosphrus etc.,) open-flame heating of easily
flammable solvents, incorrectly assembled and connected equipment, inadequate control of the chemical
reaction (too high temperature, or pressure, too rapid addition of the reagents, etc.,) working with
comprressed gases and explosive mixtures.
In order to extinguish a fire, use sand, fire blankets, fire extinguishers or water (when it is safe to
use it). Small laboratory fires can be extinguished by applying wet towels or sand, while larger ones
are extinguished by using fire extinguishers.
Everyone working in the chemistry laboratory has to be instructed on how to use a fire extenguisher.
Questions for discussion
1. What is the use of fume cup-board?
2. Name some basic laboratory equipment used in chemistry laboratory.
3. What precautions you should take while heating a solution in a test tube?
4. What does the qualitative analysis signify?
5. What does the quantitative analysis signify?
6. What is the use of a pipette?
7. What precautions do you take when handling a reagent?
8. What are the infrastructural facilities with which a chemistry laboratory is provided with?
9. What is the first aid treatment given for the burns caused in a chemistry laboratory?


CHAPTER-2
BASIC LABORATORY TECHNIQUES
The 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 300-400O C 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 700-800O C 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. It is essential to learn about some of the techniques of handling glass tubes, glass rods and
other laboratory apparatus and equipment.
2.1 Bunsen Burner
Bunsen burner is a common heating device used in the chemistry laboratory. This is a single barrel
burner designed by Robert Burner, a German chemist. The Bunsen burner consists of the following
parts.
1. The base
This is a heavy circular metallic disc and 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. The parts of
Bunsen burner are shown in the fig 2.1.
First Year 7
Burner tube
Burner Air holes
Air adjusting disc Air adjusting disc

Air vent
Gas tube Nipple
Gas tube
Base
Base
(a) (b)
Fig 2.1: (a) Bunsen burner (b) 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 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 (fig.2.2).
Oxidising zone Non - luminous outer zone

Dark Blue (Complete combustion)
Reduction zone Luminous tip pale blue
(partial combustion)
Dark zone (Unburnt gas)
Air hole opened

Gas - inlet
Fig. 2.2 Different zones in Bunsen flame
Three distinctly visible parts of the Bunsen flame are described below.
Principal parts of Bunsen flame
1. The inner dark cone
This is innermost dark cone, which is just above the burner tube. It consists of unburnt gases.
Thiszone is the coldest zone of the flame and no combustion takes place here.

2. The middle blue cone
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 com bustion is not complete, the temperature is not high.
3. The outer non-luminous mantle
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.
Bunsen identified six different regions in these three principal parts of the flame. They are
(i) The upper oxidising zone
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 the lower oxidizing zone. It may be used for all oxidation processess in
which highest temperature of the flame is not required.
(ii) Upper reducing zone
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
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
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
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
upper reducing zone and may employed for the reduction of fused borax and similar
beads.
(vi) Lowest temperature zone
This zone of the flame has lowest temperature. It is used for testing volatile substances to
determine whether they impart colour to the flame.
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
First Year 9
gas makes the flame become irregular and it strikes back.
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. Experiments with Bunsen flame
Experiment Observation InfereInference
1. The air holes are opened and Smoke of the incense stick Air is similarly sucked into
burning incense stick is comes out of the barrel at the the barrel through the air
placed near the air holes. top. holes.
Fuel gas is allowed through
burner.
2. A match stick is placed at the The match stick is charred The gas does not burn at
mouth of the barrel across the at both ends and the middle the base of the flame.
flame and removed. portion of it not affected.
3. One end of a glass tube is The gas burns at the other The dark zone consists of
kept in the dark zone of the end and the flame at the unburnt gas. There is not
flame It is lighted at the other other end is put out on rais- unburnt gas in other zones.
end. The glass tube is raised ing the glass tube to other
gradually through other zones.
zones.
4. A small copper wire is placed The copper wire is intensely The non-luminous zone is
in different zones of the bright in non-luminous the hottest part of the
flame and the intensity of the zone. flame.nce
brightness of the wire is ob-
served.
2.2 Cutting a Glass Tube and a Glass Rod

In chemistry laboratory for collecting gases gas delivery tubes made of glass are used. For other
purposes, U-shaped tubes are required. So to make these glass tubes one should know how to cut glass
tube of required length. For cutting glass tube or glass rod, proceed as follows.
Material required
Soda-glass tube: 15 cm in length, soda-glass rod: 15 cm in length and triangular file
Procedure
1. Select a glass tube or glass rod free ofcracks.
2. Place the glass tube over the work bench and press it with your left hand and make a deep
scratch around the glass tube at a required distance from one end with a training file. While
scratching draw the file in one direction only.
3. Place the tumbs on each side of the scratched part and hold the scratch closely with the thumbs.
Apply gentle pressure and give a quick bending motion towards the thumbs until the tube
breaks smoothly.
4. The cut edges of the glass tube are not smooth. So gently heat the edges in the non-luminous
flame of the Bunsen burner for about 2-3 minutes.
5. The glass tube softens at the edges and the edges become round. Removing the glass tube from
the flame and allow it to cool. This process is called fire-polishig.
(a) Making a scratch on glass tube (b) Placing the thumbs (c) Breaking the glass tube
togther opposite to the
scratch
Fig. 2.3: Cutting a glass tube
Precautions
1. Make a single deep scratch at the desired length with one stroke of the triangular file.
2. Do not heat the ends of the glass tube for long time to smoothen the edges as this may seal
the end or make it narrow.
2.3 Bending a Glass Tube

Material required
Glass tube: 20-25 cm in length and triangular file.
Procedure
1. Cut a glass tube of desire length which is to be bent with the help of a triangular file.
2. Place the glass tube in the non-luminous flame of Bunsen burner and heat that portion from
where the glass tube is to be bent.
3. While heating the tube in the flame, keep it slowly rotating along its axis until the portion.
which is to be bent, becomes red hot and soft and starts bending under its own weight.
4. When the heated portion becomes soft, remove the tube from the flame and keep it on asbestos
pad.
5. The tube is gently bent by pressing so that the two arms of the bent tube should lie in the same
plane (coplanar).
6. Allow the tube to cool on asbestos sheet.
7. Bend the tube at different angles of 120O, 90O and 60O or as desired.
First Year 11
Fig, 2.4: Bending a glass tube
Precautions
1. Avoid heating the glass tube only on one side, rather rotate it while heating.
2. Select a glass tube of appropriate length (above 20 cm in length) to keep your hands away and
safe from heat.
3. Do not bend the glass tube by applying force. Otherwise the tube may break.
2.4 Drawing a Glass Jet
Material required
Glass tube: 20-25 cm in length, triangular file and sand paper
Procedure
1. Select a glass tube of appropriate diameter for drawing a jet.
2. Cut the glass tube of desired length with the help of a triangular file.
3. Heat the tube in the non-luminous portion of the Bunsen burner flame by holding it at both the
ends.
4. Rotate the tube slowly until the portion. Which is kept in the flame, becomes red hot and soft.
5. 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.
6. Cut the tube in the middle and make the jet uniform and smooth by rubbing it with sand paper
and by fire polishing.
Fig. 2.5: Drawing a glass jet

Precaution
While drawing a jet, pull apart the two ends of the red-hot tube slowly so that it becomes
thin\uniformly
2.5 Boring a Cork
Material required
Rubber corks, cork borer set and glycerine solution (Shelf reagent)
Procedure
1. Mark the rubber cork on both of its sides at the place where a hole is to be drilled.
2. Choose a borer of diameter slightly smaller in size than that of the tube to be fitted in the cork.
3. Place the rubber cork on the table with its smaller end in the upward direction.
4. 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. By lubricating borer with water
or glycerine a smooth hole is drilled.
5. Now hold and push the borer vertically in the downward direction, and drill the hole by
rotating the borer and simultaneously apply the pressuregently.
6. For making two holes in the same cork, keep appropriate distance between the holes and use
borers of proper size.
Place marked for boring
Fig. 2.6: (a) Marked cork (b) Boring process
Precautions
1. Make a mark on both sides of the cork and select borer of proper size.
2. To obtain a smooth hole, drill half the hole from one side and another half from the other side
of the cork.
First Year 13
2.6 Heating Solution in a Test Tube
If a solution contained in a test tube is to be heated on 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.
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. This can
cause a serious accident, if the mouth of the test tube is 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.
2.7 Heating Solution in a Beaker
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. 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 substance.
(ii) The apparatus, which is used for measuring volume, should not be heated because
heating may distort it and graduations may become invalid.
Fig. 2.7: Heating solution in test tube Fig. 2.8: Heating solution in beaker
2.8 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.
Material required
Beakers, funnel, funnel stand, glass rod and filter paper.
Procedure
Fold the filter paper to fit in the funnel. For this, fold the circular filter paper in half, tear off a small
piece of paper from the corner and once again fold it.
Open the folded filter paper into a cone by keeping three folds on one side and one on the other
such that the torn off corner is outisde. Fit the cone into the finnel. Take care that filter paper cone fits
in one cm below the rim of the funnel. 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. 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.
Filter papr Folded once Folded twice opened
Fig. 2.9: Process of filtration
2.9 Measuring Volume of Liquid

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 appartus.
Central part of the meniscus is rather flat. Calibration of the appartus 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. 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 notted. In flasks and pipettes capacity mark is etched on the narrow part of the
apparatus 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. Now we study how to measure the volume of solutions using different
measuring devices like measuring cylinder, burette, pipette and standard flask.
First Year 15
1. Using measuring cylinder
A measuring cylinder is a long cylindrical apparatus made of thick
glass. The measuring cylinder is marked in millilitres(mL). They are avail-
able in various capacities like 5mL, 10mL, 25mL, 50mL, 100mL, 250mL,
500mL and 1000mL. Measuring cylinder are used to measuring a definite
volume of the solution. However, measuring cylinders used for deliver-
ing 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.
2. Using burette
A burette is simply a long graduated tube of uniform bore with a
stopcock or a pinchcock at one end. 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 read-
ings is the volume of the liquid delivered. The liquid should be delivered
slowly. If the liquid is allowed to run too fast the walls of the burette will
not brain properly and some liquid may remain sticking to the surface of
the walls. This may lead to faulty reading. Measuring capacity of the bu-
rette usually used in the laboratory is 50 mL. Before filling the solution to
be used, the burette should be rinsed with the solution to be filled. For
rinsing the burette, few millilitres of solution are taken into it and the
whole inner surface of burette is wetted with the solution by rotating it.
After rinsing, the solution is drained out of the nozzle of the burette.
After rinsing is completed, the solution is filled in the burette with the Fig. 2.10:
help of a funnel above zero mark. Stopcock is then opened wide and the Measuring cylinder
solution is allowed to run through the nozzle till there are no air bubbles
in it. Reading should be noted after allowing sufficient time for the liquid to drain down the walls.
While taking reading eye must be placed in a level with the lowest part of the meniscus to avoid
parallax error. Reading from the bottom of the meniscus is recommended for colourless solutions and
top for deeply coloured solutions. A thin layer of grease should be applied to the stop-cock for its easy
movement. After the use, the burette should be cleaned.
Fig. 2.11: Burette Fig. 2.12: Filling the burette

Using pipette
Pipette is a long glass tube of narrow bore with cylindrical bulb at the middle. It is drawn into a
nozzle at one end. Near the other end, pipette is provided with a safety bulb. It is provided with a
circular mark at the other end. The capacity of the pipette upto the mark is noted on the other
cylindrical bulb. The pipette is used to transfer a definite volume of the solution from one vessel to
another vessel. Normally pipettes of measuring capacity 1 mL, 2mL, 5mL, 10mL, 20mL, 25mL, etc.,
are used. Graduated pipettes are also used in the laboratory work. Using of a pipette to transfer the
solution is described below.
The nozzle of the pipette should be dipped in the solution. The solution is to be sucked until it
raises just above the mark noted on pipette. Then the mouth of the pipette should be closed with the
fore finger. The excess of the liquid should be allowed to flow out slowly by gently releasing pressure.
The lower meniscus of the liquid in the stem should be made to coincide with the mark on the pipette.
The contents of the pipette should be allowed to run into the required vessel. The last drops of the
liquid remaining near the tip of the pipette should not be blown out. Concentrated acids, corrosive and
poisonous solutions should not be measured with pipette. While transfering the solution, the tip of the
pipette shuld touch the sides of the vessel.
(a) (b) (c) (d)
Fig. 2.13:
(a) Pipette
(b) Using pipette filler bulb
(c) Holding the pipette after removing the bulb
(d) Transferring liquid to the flask
First Year 17
Using volumetric flask (Standard flask)
These are employed for making specific volumes of solutions This
is also called graduated flask. It is a pear shaped vessel with a long
narrow neck and flat bottom. A thin circle etched around the neck
indicates the volume of the liquid that it holds at a definite tempera-
ture. 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 observ-
able in single line. The neck of the flask is made narrow to reduce
error in adjustment of the meniscus. In narrow space small change in
volume makes large effects on the height of the meniscus. Measuring
flasks of various capacities are available. usually at this level of ex-
perimentation flasks of capacity 50mL, 100mL and 250mL are em-
ployed in the work. The method of preparation of solution by using volumetric flask has been de-
scribed below. A funnel of suitable size should be inserted into the neck of the volumetric flask to
transfer any substance into it. The substance in the funnel should be washed with a stream of water
from a wash bottle. The funnel should be removed after washing it inside and outside. The washings
should be collected into the flask.
The substance in the flask should be completely dissolved in a minimum amount of distilled water
and the solution should then made upto the mark. The last few drops may be added with pipette. The
stopper should be replaced now. The contents of the flask should be throughly shaken by inverting the
stoppered flask atleast six times, so that uniform solution is formed.
Using conical flask

The conical flask is a cone shaped vessel. It is provided
with a flat bottom. At the upper part the shape of the
flask is cylindrical. The capacity of the flask is noted
on its conical part. Conical flasks of 100mL, 250mL
and 500mL are available for use in the laboratory.
2.10 Wash Bottle

Wash bottle is a device made of glass used for washing precipitates and other purposes. With the
help of wash bottle a fine stream of water can be obtained which is convenient for washing purposes in
the laboratory.
Construction
A flat bottomed flask of 500mL is taken. Appropriate two bored cork is fitted into it. A long (about
26 cm in length) bent glass tube (bent at an angle of 120O) is inserted into one of the holes of the two
holed rubber cork. Another glass tube of shorter length bent at an angle of 60o is inserted into the other
hole of the rubber cork. The two tubes are arranged in such a way that their upper portions lie in a
straight line. The upper portion of the 120o angled tube is held in mouth while the 60o angled tube is
fitted with a jet.

Working
The 500 mL flat bottomed flask is filled with water about 3/4 of its capacity. The two holed rubber
cork is fitted to the flask. The long tube should nearly reach inside bottom of the flask. The other tube
should be above the water level. The cork (stopper) is prressed with the right hand fingers and air is
blown into the flask through the short tube. Air presses the water which them raises into the long tube
and flows out. Generally distilled water is taken in the wash bottle.
Polythene wash bottle
These days the glass wash bottles are replaced by polythene wash bottles. A polythene wash bottle
consists of flexible plastic material bottle. fitted with a plastic tubing having a jet at its outer end. On
squeezing the bottle fine stream of water comes out of the jet. Polythene wash bottle can be used to
wash the precipitates and for other washing purposes in the laboratory.
Fig. 2.16: (a) Wash Bottle (Glass) (b) Wash Bottle (Polythene)

1. What is the function of air regulator in Bunsen burner?
2. Name different zones in Bunsen flame?
3. Which is the hottest zone of the Bunsen flame?
4. By what name blue and yellow flame are known?
5. Why does glass not possess sharp melting point?
6. Why it is required to round off the freshly cut edges of a glass tube?
7. Why should the tube be rotated while heating?
8. Why is the red hot tube bent slowly?
9. What is fire polishing of glass?
10. What is annealing?
11. What type of glass is preferred for drawing out a jet?
First Year 19
12. Why is glass tube of smaller diametre chosen for drawing out a jet?
13. What is the role of glycerine in the process of boring?
14. What precautions you have to take while heating a solution in test tube?
15. Why wire gauze is used when solution is heated in a beaker?
16. Name some devices for measuring volume of liquids.
17. What precautions you have to take while working with a pipette?
18. On what principle the wash bottle works?
19. What is bumping of a liquid? How to avoid this?


CHAPTER - 3
MELTING, BOILING POINT OF COMPOUNDS &

PURIFICATION OF CHEMICAL SUBSTANCES
Experiment : 3.1
Determination of Melting point of an Organic Compound.
Aim : To determine the melting point of a solid organic substance.
Theory
In the solid substances, strong intermolecular attractive forces keep the molecules closer in
fixed positions. On heating the kinetic energy of these molecules increases and when the kinetic
energy is high enough over the intermolecular attractive forces, the crystal lattice breaks and the solid
starts melting to become aliquid. Thus the melting point of a solid substance is the temperature at
which the solid substance starts melting into liquid state when the pressure is one atmosphere. At
melting point, the solid substance is in equilibrium with its liquid state. The melting point of a
substance is an important criteria to determine its purity. The impurities present in a substance lowers
its melting point. A pure substance melts at a definite temperature and has a sharp melting point.
Apparatus and chemicals required
Thiele’s tube, thermometer, capillary tubes, iron stand with clamps, liquid paraffin or conc.H2SO4
and organic compound (whose M.P. is to be determined)
Procedure
1. Take a capillary tube of approximately 8 cm in length. Seal its one open end by heating it in
a Bunsen burner flame. Rotate the capillary while sealing to ensure complete closure of the
opening.
2. Crush the desired substance (about 100 mg) into fine particles and fill the substance in the
capillary tube up to nearly 1 cm length.
3. Moisten the capillary tube with liquid paraffin (or conc.H 2SO 4) and stick it to the
thermometer. It will stick to the thermometer by cohesive forces. See that the lower ends of
the capillary tube and the thermometer bulb are at the same level. The thermometer is fitted
into a rubber cork, which has a groove on its side for the escape of air and vapours.
4. Take a Thiele’s tube and fill it with 50 to 60 mL liquid paraffin (or conc.H2SO4) so that it
crosses the bent portion of the Thiele’s tube.
5. Dip the thermometer along with the capillary tube in liquid paraffin (or conc.H2SO4) 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 (or conc.H2SO4) and the open end of the
capillary remains in the air. The thermometer and the capillary tube should not touch the sides
of the Thiele’s tube.
First Year 21
6. Now start heating the side arm of the Thiele’s tube with a low flame from the side opposite to
that of the capillary tube and note the temperature when the solid starts melting. This is the
melting point of the solid substance.
Solid
Fig.3.1: Determination of melting point of an organic solid
Precautions
1. Use dry and powdered sample for the determination of melting point.
2. Keep the lower end of the capillary tube and the thermometer at the same level
3. use thin capillary tube.
4. Packing of the powder in the capillary tube should be uniform without any big air gaps in
between the solid particles.
5. Thiele’s tube should be heated at the side arm by using a low flame.
Table 3.1: Melting points of some organic substances

Organic compount Melting point (oC) Organic compount Melting point (oC)
Phenol 42 Acetamide 82
Napthol 95 enzamide 128
Napthol 123 Urea 132
Oxalic acid 101 Fructose 103
Benzoic acid 121 Glucose 146
Napthalene 80 Sucrose 160

Experiment : 3.2
Determination of Boiling point of an Organic Compount
Aim : To determine the boiling point of a liquid organic substance.
Theory
The boiling point of a liquid is the temperature at which the vapour pressure of the liquid
becomes equal to the atmospheric pressure, which the surface of the liquid experiences. As the
atmospheric pressure is different at different places, the boiling point of a liquid also differs from place
to place. At 1.013 bar atmospheric pressure, the boiling point of the liquid is termed as normal boiling
point of the liquid.
Thiele’s tube, thermometer, capillary tube, iron stand with clamps, ignition tube, liquid
paraffin or conc. H2SO4 , organic liquid (whose b.p. is to be determined)
Procedure
1. Take 1-2 drops of the organic liquid in an ignition tubeand tie it to the thermometer with a
rubber band. Note that the lower end of the ignition tube and the thermometer bulb are at the
same level.
2. Take a capillary tube of 5-6 cm in length, seal it at
about 1 cm from one end by heating in a flame. Place
the capillary tube with its open
end dipped in the liquid present in the ignition tube.
3. Fill Thiele’s tube with the liquid paraffin or conc.H2SO4
so that it crosses the bent portion of the Thiele’s tube.
4. The thermometer is then dipped into a Thiele’s con-
taining the liquid paraffin or conc.H2SO4
5. Heat the side arm of Thiele’s tube with a low flame.
At first a few bubbles are seen escaping at the lower
end of the capillary tube dipped in the organic liquid.
Note the temperature when rapid and continu
ous stream of bubbles starts coming out (t1)
6. Stop heating, note the temperature when the bubbles
stop in the capillary tube (t2).
7. The mean of the two temperatures (t1 and t2) gives the
boiling point of the liquid.
 t1  t2 
8. Boiling point of the liquid  oC
 2 
Precautions
1. Keep the lower end of the ignition tube and thermometer bulb at the same level
2. The liquid in the side arm of the Thiele’s tube is heated very slowly. The boiling point of the
liquid filled in Thiele’s tube should be 50-60oC higher than that of the liquid whose boiling point
is to be determined.
First Year 23
3. Record the temperature as the boiling point of the liquid, at which brisk and continuous evolu-
tion of the bubbles starts from the lower end of the capillary dipped in the liquid organic com-
pound.
Boiling points of some organic liquids are given in table 3.2
Table 3.2: Boiling points of some organic liquids

Organic liquid Melting point (oC) Organic liquid Melting point (oC)
Benzene 80 Benzaldehyde 179
thanol 78 Acetone 56
Benzyl alcohol 205 Aniline 184
Phenol(liquid) 182 Nitrobenzene 211
Acetic acid 118 Ethylene glycol 197
Acetaldehyde 20 Chlorobenzene 132
Purification of chemical substances by crystallisation

The chemical substances should be pure to carry out reactions and to obtain the products. As an
example, to carry out qualitative or quantitative analysis pure substance is required. Therefore, the
substance should be purified and then check its purity. There are variety of techniques available for the
purification of substance namely, crystallisation, distillation, sublimation, chromatography etc. The
purity of a substance can be checked with melting point or boiling point. Here we discuss the
crystallisation process of purification of chemical substance.
Experiment : 3.3
Purification of a Chemical Substance by Crystallisation
Aim : Purification of sample of any one of the following compounds viz.,potash
alum or copper sulphate or benzoic acid by crystallisation.
Theory
The crystallisation technique is used for the purification of an impure compound especially
when a compound prepared as a chemical reaction is crude and impure. First step of the crystallisation
process is to choose a suitable solvent or mixture of solvents. The solvent so chosen, should be such
that the impure substance is sparingly soluble at ordinary temperature (in cold condition) but readily
soluble at higher temperature (in hot condition). In this process the crude substance is dissolved in
minimum amount of solvent in hot solution to obtain a saturated solution. The hot solution is filtered
to remove insoluble impurities. It is then cooled slowly when the pure crystals separates out leaving
the impurities in 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 a very small quantity of
pure substance is added to the solution to facilitate the initial crystallisation. This process is called
seeding and this helps in the growth of the crystals. Growth of crystals depends upon the conditions in
which crystallisation is carried out. Sudden and 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 greenish white
respectively. Impurities impart colour to the crystals, therefore, impure crystals have a colour different
from that of pure crystals.
Beaker (250 mL), glass funnel, tripod stand, porcelain dish, glass rod, sand bath, potash alum,
copper sulphate and benzoic acid.
Procedure
1. Prepare a saturated solution of potash alum/copper sulphate at room tem perature by adding the
impure solid sample in small amounts with stirring to 30-50 mL of distilled water taken in a
beaker. Stop adding the solid substance when it does not dissolve any more. Prepare the
saturated solution of benzoic acid in the same manner but using hot water.
2. Filter the saturated solution so prepared and take the filtrate into a porcelain dish. Heat the
filtrate on a sand bath till nearly 3/4 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.
3. Cover the porcelain dish with a watch glass and keep the content of the dish undistrubed for
cooling.
4. When crystals are formed, remove the mother liquor (liquor left after crystallisation) by
decantation.
5. Wash the crystals of potash alum and copper sulphate, so 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. Do not use
alcohol as benzoic acid is soluble in alcohol.
6. Dry the crystals between the folds of a filter paper.
7. Store the dry crystals thus obtained at a safe and dry place free from moisture.
8. Repeat the above process for obtaining maximum amount of pure substance.
Precautions
1. Do not evaporate the entire solvent while concentrating the solution.
2. The solution should be cooled slowly without disturbing it. Avoid rapid cooling.
3. Wash the crystals with the washing liquid in 3-4 times in very small.
1. What is the melting point of a solid substance?
2. How does the impurities present in a substance affect its melting point?
3. How is determination of melting point useful?
4. What is sharp melting point?
5. Can we heat the capillary tube directly for the determination of melting point?
6. Can any other liquid be used in place of liquid paraffin in the determination of the melting
point?
7. Define the boiling point of a liquid.?
8. What is the effect of increase in outside pressure on the boiling point of a liquid?
9. What is the effect of decrease in outside pressure on the boiling point of a liquid?
First Year 25
10. Why different liquids possess different boiling points?
11. What is the effect of addition of a non-volatile liquid on the boiling point of a liquid?
12. Give the formula of potash alum.
13. What is meant by the term ‘water of crystallisation’?
14. Name some purification methods of chemical substance.
15. What do you understand by the term mother liquid?
16. What is the principle involved in the process of crystallisation?
17. Explain the term ‘saturated solution’.
18. Why is the preparation of a saturated solution necessary for making crystals?
19. Name the different steps involved in crystallization process.
20. What is seeding?
21. Why the hot saturated solution not cooled suddenly?


CHAPTER - 4
PH AND PH CHANGE IN
AQUEOUS SOLUTION
The chemical equilibrium is dynamic in nature which would be experienced by carrying out
experiments. Here you 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 small extent.
On the basts of conductivity experiments it can be concluded that ionic equilibrium exists in pure
water also. The ionic equilibrium is represented as
H2O(1)  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(1)  H3O(aq) +OH-(aq)
This is self ionisation of water. Equilibrium constant for this chemical equation is written as
follows:
[H 3O + ][O H - ]
K =
[H 2O ]2
Since water is in large excess, its concentration is assumed to be constant. Combining the
concentration of water with K gives a new constant K, which is written as
K w = [H 3 O + ][O H - ]
Kw is the ionisation constant of water. It is constant at constant temperature.
At 25°C, the value of Kw is 1.0 x 10-14 mol2 L-2. Thus, it is quite evident that at a given temperature
in any aqueous solution, this product i.e., (H2O+][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, the
hydroxyl ion concentration is more than hydronium ion concentration, then the solution is alkaline in
nature. Thus, the concentration of hydronium ion in aqueous solution indicates the acidic, basic and
neutral nature of the solution. The concentration of hydronium ions [H3O+) in a solution is measured in
terms of pH, which is defined as the negative value of logarithm of hydronium ion concentration and
is given by the following equation
pH = -log[H3O+]
The pH of neutral water is 7.0 at room temperature. A solution with pH less than 7.0 is acidic while
the solution with pH greater than 7.0 is basic in nature.
First Year 27
Experiment : 4.1
Determination of pH of Same Concentrations of Acids, Bases and Salts in Aqueous Solution
Aim : To determine the pH of aqueous solutions of same concentrations of different acids, bases
and salts.
Theory
Dyes show different colours at different pH. These dyes act as acid-base indicators. A solution
of mixture of dyes is used to obtain approximate pH value of a solution starting from zero to 14. This
solution of a mixture of dyes is called universal indicator. Infact, 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 (H+). Different forms of a dye have different colours and hence, colour chart for the colour
change of the universal indicator with pH is supplied with the indicator solution and comparison of
observed colour change with the chart gives the pH of the solution.
Materials required
Beakers, test tubes, dropper, universal indicator, colour chart for pH, hydrochloric acid, acetic
acid, ammoniumchloride, sodium acetate, sodium chloride, sodium hydrogen carbonate, sodium car-
bonate and sodium hydroxide
Procedure
1. Prepare solutions of hydrochloric acid and acetic acid by dissolving 1.0 mL of each acid in 100
mL distilled water. Take about 1.0 g each of ammonium chloride, sodium acetate, sodium
chloride, sodium hydrogen carbonate, sodium carbonate and about 6 pellets of sodium
hydroxide, dissolve each of them in 100 mL distilled water separately and shake well for
uniform concentration.
2. Take 8 test tubes and label them as 1,2,3,4,5,6,7 and 8. Take 5.0 mL of each solution and
transfer into test tubes in the same order mentioned above i.e., hydrochloric acid(1), acetic
acid(2), ammonium chloride(3), sodium acetate(4), sodium chloride(5).sodium hydrogen
carbonate(6), sodium carbonate(7) and sodium hydroxide(8).
3. Add two drops of universal indicator in each test tube and mix it uniformly. Observe the
colour and record in the table.
4. Match the colour appearing in each test tube with the standard pH chart.
Table 4.1: pH values of different solutions
S.No. Name of the solution Colour with universal pH value Inference

indicator
1 Hydrochloric acid
2 Acetic acid
3 Ammonium chloride
4 Sodium acetate
5 Sodium chloride
6 Sodium hydrogen carbonate
7 Sodium carbonate
8 Sodium hydroxide
Precautions
1. Match the colour of the solution with pH chart carefully.
2. Store universal indicator or pH paper at a safe place to avoid contact with acidic or basic reagents.
3. Add equal number of drops of universal indicator to all the solutions.
Further activity
Carry out the same set of experiments with red cabbage extract instead of universal indicator.
Red cabbage acts as universal indicator.
Fig. 4.1: Universal indicator as test papers

Experiment : 4.2
Determination of pH of Some Fruit Juices

Aim: To determine the pH of lemon, orange, apple, pine apple and grape juices.
Materials required
Beakers (100 mL)- 4, test tubes, droppers, universal indicator/ pH papers, pH chart, lemon,
orange, apple, pine apple and grape juices.
Procedure
1. Extract fresh juices of lemon, orange, apple, pine apple and grape (not black) fruits in separate
beakers.
2. Transfer approximately 5 mL of each of the fresh juice into five test tubes marked as 1,2,3,4 and
5 respectively.
3. Add two drops of universal indicator to each test tube and mix the contents of each test tube by
shaking.
4. Match the colour appearing in each test tube with the standard pH chart.
5. Record your observations in a table.
Table 4.2: Determination of pH of different fruit juices

S.No. Name of the fruit juice Colour with universal pH value Inference
indicator
1. Lemon
2. Orange
3. Apple
4. Pine Apple
5. Grapes
First Year 29
Result : What is your conclusion from the observations of the pH values of different fruit juices?
Experiment : 4.3
Variation of pH of Acid /Base /Salt Solutions with Dilution
Aim : To study the variation of pH values of acid. base and salt solutions with dilution.
Theory
The change in concentration of acid, changes the hydronium ion concentration. Therefore,
change in pH is expected with the change in concentration of acid. Similarly hydronium ion concen-
tration changes with change in concentration of base or some salts.
Materials required
Test tubes, glass droppers. pH paper. universal indicator solution, 0.1 M NaOH solution. 0.1
M HCl solution and 1.0M NH4Cl solution
Procedure
1. Take four test tubes and label them as A, B, C and D.
2. Take 2.0 mL of 0.1 M HCl solution in test tube A.
3. Take 2.0 mL of 0.1 M HCl solution in test tube B and add 18 mL of water and mix thoroughly.
4. Take 2.0 mL of HCl solution from test tube B into test tube C and add 18 mL of water and mix
thoroughly.
5. Take 2.0 mL of HCl solution from test tube C into test tube D and add 18 mL of water and mix
thoroughly
6. Cut a pH paper into small pieces and spread them on a clean glazed tile.
7. Take solution from test tube A with a dropper and put a drop on one of the pieces of pH paper.
Compare the colour of the pH paper with the standard pH chart.
8. Similarly, test the pH of solutions of test tubes B, C and D respectively and
record your results in a table.
9. Similarly, observe the change in pH of 0.1 M NaOH and 1.0M NH4.CI
solutions with dilution as explained above and record your observations in a table.
Table 4.3 : pH change on dilution

Test tube HC1 solution NaoH solution NH4C1 solution
Colour pH Colour pH Colour pH
A
B
C
D
Result : What is your conclusion about the variation of pH with dilution in all the cases?
Precaution : Match the colour of the solution with pH chart carefully.

Experiment : 4.4
pH of Solutions of Strong Acid and Weak Acid of Same Concentration
Aim: To determine the pH of strong acid and weak acid solutions of the same concentration.
Theory
Strong acids like HCl in aqueous solution is in completely ionised form, while weak acids like
ethanoic acid is in weakly ionised form. Therefore, the hydronium ion concentration of both the acids
is different. Hence, the pH values will also be different.
Materials required
Test tubes, droppers, pH paper or universal indicator, pH chart, 0.1 M HCl and 0.1 M acetic
acid solutions.
Procedure
1. Take 2 ml of 0.1 M HCl solution in test tube 'A' and 2 mL of 0.1 M acetic acid solution in test
tube 'C'.
2. Take 2 mL of 0.1 M HCl solution in test tube 'B' and add 18 mL of distilled water. Take 2 mL
of 0.1 M acetic acid solution in test tube 'D' and add 18 mL of distilled water.
3. Take solution from test tube A with a dropper and put a drop on a piece of pH paper. Compare
the colour of the pH paper with the standard pH chart.
4. Similarly, test the pH of solutions of test tubes B, C and D respectively.
5. Compare the pH values of solutions of test tubes A & C and B & D.
Result : What are your conclusions from the observations made with HCl and acetic acid solutions?
Experiment : 4.5
pH Change During the Titration of Strong Acid and Strong Base
Aim : To study the change in pH values during the titration of a strong acid with a strong base
using universal indicator.
Theory
Strong acids and strong bases usually exists as completely dissociated form in aqueous
solutions. When strong acid is added to strong base, the H+ ions produced from acid combines with
OH: ions produced from strong base to form water. This reaction is called neutralisation. 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 rapid change in the pH of the solution.
Materials required
Burette (50 mL), beakers (100 mL), conical flask (100 mL), dropper, pH chart, universal indicator,
0.1 M hydrochloric acid and 0.1 M sodium hydroxide solutions
First Year 31
Procedure
1. Take 25 mL of hydrochloric acid solution (0.1 M) in conical flask.
2. Add 3 to 4 drops of Universal indicator solution to the solution in conical flask.
3. Add sodium hydroxide solution(0.1 M) from the burette as shown in table 4.4.
4. After each addition of sodium hydroxide solution, shake the contents of the conical flask well.
Note the colour of the solution in the conical flask each time and find out the pH by comparing its
colour with pH chart.
Table 4.4: pH change during the neutralisation of 25 ml 0f

0.1 M HCI with 0.1 M NaOH solution
S.No. Volume of NaOH solution added Total volume of NaOH added to the pH
in lots (ml) solution in the conical flask (mL)
1 0 0
2 10 10
3 10 20
4 2 22
5 2.5 24.5
6 0.2 24.7
7 0.1 24.8
8 0.1 24.9
9 0.1 25
10 0.1 25.1
11 0.1 25.2
12 0.1 25.3
13 0.2 25.5
14 0.5 26
Result : Write your result on the basis of above data.

Further activity
Carry out the neutralisation of 25 mL of 0.1 M weak acid (ethanoic acid) with 0.1 M of
strong base (sodium hydroxide) solution using universal indicator and record your observations.
1. Define pH.
2. Give the pH range of acids and bases.
3. What is pH of pure water at 25°C?
4. What is the nature of solution formed when co2, gas is passed into water?
5. What is ionic product of water?
6. What is universal indicator?
7. What is an acid-base indicator?


CHAPTER-5
CHEMICAL EQUILIBRIUM
Chemical reactions are classified as reversible and irreversible reactions. Under the same
conditions of temperature and pressure reversible reactions take place in the forward and backward
directions simultaneously. In the case of reversible reactions a state is reached in which the rate of
forward reaction becomes equal to the rate of backward reaction. This appears as though the reaction
has come to stand still. This state is called state of dynamic equilibrium. Consider the simple
reversible reaction at constant temperature.
A+B  C +D
Guldberg and Wage (1867) stated the law of mass action as "the velocity of a chemical reaction is
proportional to the product of the active masses of reacting substances. Active mass was interpreted as
concentration and expressed in moles per litre. By applying the law to homogeneous system – the
system in which all the reactants and products are present in one phase, the rate of forward reaction, r1,
is directly proportional to the products of concentrations of A and B. The rate of backward reaction, r2,
is directly proportional to the product of concentrations of C and D.
Thus, r1 = k1 [A] [B] and r2 = k2 [C] [D]
k1 and k2 are the rate constants for the forward and the backward reactions respectively and (A),
[B], [C] and [D] are the molar concentrations of A, B, C and D respectively.
At equilibrium r1 is equal to r2 Therefore
 C  D 
k1 [A] [B] = k2 [C] [D] and k1/k2 = A B
  
KC is equilibrium constant which is equal to the product of concentrations of the products divided
by product of concentrations of the reactants.
 C  D 
KC = A B
  
The equilibrium constant (KC) is independent of initial concentrations of reactants and remains
constant at constant temperature. At a given temperature, if the concentration of any one of the
reactants or products is changed, then the 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.
First Year 33
The state of equilibrium in any reaction is realized by the constancy of an observable property
(macroscopic property) like colour intensity of the solution.
Experiment : 5.1
Study the Shift in Equilibrium in the Reaction of Ferric Ions and Thiocyanate Ions by
Changing the Concentration of any one of these Ions
Aim : Study the shift in equilibrium in the reaction of ferric ions and thio cyanate ions by
changing the concentration of any one of these ions.
Theory
The equilibrium reaction between ferric chloride and potassium thiocyanate is studied through
the change in the colour of the solution. The equilibrium reaction is:
Fe+3+(aq) + SCN– (aq)  [Fe(SCN)]+2(aq)
(blood red colour)
The equilibrium constant for the above reaction can be written as :
 Fe(SCN) 
2+
KC =
 Fe 3+ (aq)  SCN - (aq) 
KC is constant at a constant temperature. Increasing the concentration of either Fe+3 ion or

thiocyanate ion results in a corresponding increase in the concentration of [Fe(SCN)]2+ ions. In order
to keep the value of KC, constant, there will be a shift in equilibrium, in the forward direction and
consequently increase in the intensity of the colour which is due to [Fe(SCN)]2+, At equilibrium the
colour intensity remains constant.
Materials required
Standard flasks (100 ml): 2, beakers (100 ml): 2, boiling tubes: 10, burettes: 3, test tube stand: 1, glass
rod: 1, glass droppers: 2, ferric chloride: 0.1 g, potassium thiocyanate: 0.1 g, and dil.hydrochloric acid
This is a qualitative experiment therefore preparation of solution in terms of molarity is not stressed.
Procedure
1. Dissolve 0.10 g ferric chloride in 100 mL dil. HCl in a standard flask and 0.10 g potassium
thiocyanate in 100 mL water in other standard flask.
2. Take 5 mL of above ferric chloride solution and dilute to 100 mL.
3. Mix 20 mL of this ferric chloride solution with 20 mL of potassium thiocyanate solution. Blood
red colour will be obtained for this solution. Fill this solution in a burette mark this burette as
'A'.
4. Fill another burette with ferric chloride solution obtained in step 2 mark this burette as 'B'. Fill
another burette with potassium thiocyanate solution and mark this as 'C'.
5. Take 5 boiling tubes of same size and mark them as I, II, III, IV and V.
6. Take 3 mL of blood red colour solution from Burette 'A' into each of the boiling tubes I, II, III, IV
and V.

7. Add 17 mL of water to the boiling tube I so that the total volume of the solution becomes 20 mL
keep it as reference.
8. Add 1.0 mL, 2.0 mL, 3.0 mL and 4.0 mL of ferric chloride solution from step 2, to boiling tubes
II, III, IV and V respectively from burette 'B'.
9. Now add 16.0 mL, 15.0 mL, 14.0 ml, and 13.0 mL of water to boiling tubes II, III, IV and V
respectively from burette 'C' so that the total volume of solution in each boiling tube is 20 mL.
10. Compare the colour intensity of the solution in each boiling tube with the colour intensity of
reference solution in boiling tube I.
11. Collect another set of four boiling tubes. Take 3.0 mL of blood red colour solution in each of the
boiling tubes from the burette 'A'. Add 1.0 mL, 2.0 mL, 3.0 mL and 4,0 mL of potassium
thiocyanate solution from burette 'B' to the boiling tubes marked as VI, VII, VIII and IX
respectively followed by adding 16.0 mL, 15.0 mL, 14.0 mL and 13.0 mL of water respectively
to the boiling tubes. Again compare the colour intensity of the solution of these test tubes with
reference solution.
12. Record your observations in the tables.
Table 5.1: Change in colour intensity on increasing the concentration of ferric chloride
Boilling tube Volume of Volume of volume of Change in Direction of
blood red ferric chloride water in mL colour shift in
colour solution intensity with equilibrium
solution taken in mL reference to
taken in mL reference
boilling tube I
I 3 0 17
II 3 1 16
III 3 2 15
IV 3 3 14
V 3 4 13
Table 5.2: Change in colour intensity on increasing the concentration of potassium thiocyanate
Boilling tube Volume of Volume of volume of Change in Direction of

blood red thiocyanate water in mL colour shift in
colour solution intensity with equilibrium
solution taken in mL reference to
taken in mL reference
boilling tube I
I 3 0 17
II 3 1 16
III 3 2 15
IV 3 3 14
V 3 4 13
First Year 35
Experiment : 5.2
Study the Shift in Equilibrium Between [Co(H20)6]2+ and Chloride Ions by
Changing the Concentration of either of the Ions
Aim : Study the shift in equilibrium between [Co(H20)6]2+ and chloride ions by changing the concen
tration of either of the ions.
Theory :
The following reaction takes place between [Co(H20)6]2+ and C1- ions in solution.
[Co(H20)]2+ +4C1-  [CoC14]2- + 6H20
This reaction is known as ligand displacement reaction and the equilibrium constant KC
 CoCl 4 ) 
2-
KC =
is.  Co(H 2 O) 2+   Cl - 
4
Since the reaction occurs in aqueous medium, the concentration of H2O is taken as constant
and is included in the value of KC itself.
At equilibrium if the concentration of either (Co(H2O)]+2 ion or Cl– ions is increased, then the equilib-
rium shifts to right and increases the concentration of (CoCl4]2- to maintain the value of KC as constant,
this will increase the blue colour.
Materials required
Standard flask (100 mL): 1, test tubes: 6, beakers (100 mL): 3, test tube stand: 1, burettes: 3, glass rod,
acetone: 60 mL, conc.HCl and cobalt chloride: 0.600 g
This is a qualitative experiment therefore preparation of solution in terms of molarity is
not stressed.
Procedure .
1. Dissolve 0.600 g of Cocl2, in 60 mL of acetone in the standard flask to get blue colour solution.
Take this solution in a burette and label it as 'A'. Fill another burette with acetone and label it as
'B'. A third burette is filled with water and labeled it as 'C'.
2. Take 5 test tubes and label them as I, II, III, IV and V. Add 3.0 mL of cobalt chloride solution in
each test tube from burette ‘A’. Add 1.0 mL, 0.8 mL, 0.6 ml. 0.4 mL andl 0.2 mL of acetone to
test tubes I, II, III, IV and V respectively from burette 'B'. Now, add 0.2 ml. 0.4 mL, 0.6 mL, and
0.8 ml, water from burette 'C' to the test tubes II. III, IV and V respectively and mix them
thoroughly for uniform concentration. The total volume in each test tube is 4.0 mL.
3. Note the gradual change in colour of the solution in each test tube with an increase in the amount
of water from blue to pink.
4. Take 10 mL cobalt chloride solution prepared in acetone in step 1 and add 5 mL distilled water
to it. Observe the colour of the solution (pink).
5. Take five test tubes and label'them as A, B, C, D and E, add 1.5 mL of pink solution prepared in
step 5 in each test tube.. Add 2.0 mL, 1.5 mL, 1.0 mL and 0.5 mL of water to the test tubes
labeled as A, B, C and D respectively. Then add 0.5 mL, 1.0 mL, 1.5 mL.
6. 2.0 mL and 2.5 mL concentrated HCl respectively in test tubes A, B, C and D and E, the total
volume in each test tube is 4.0 mL.
7. Observe the colour change with increasing amounts of hydrochloric acid.
8. Record your observations in the table.
Table 5.3: Shift in equilibrium on adding water

S.No Test tube Volume of Volume of Volume of Colour of
CoC12 acetone in mL water in mL solution
solution in
mL
1 I 3.0 1.0 0.0
2 II 3.0 0.8 0.2
3 III 3.0 0.6 0.4
4 IV 3.0 0.4 0.6
5 V 3.0 0.2 0.8
Table 5.4: Shift in equilibrium on adding Cl–. ions

S.No Test tube Volume of Volume of Volume of Colour of
CoC12 concentrated water in mL solution
solution in HC1 in mL
mL
1 A 1.5 0.5 2.0
2 B 1.5 1.0 1.5
3 C 1.5 1.5 1.0
4 D 1.5 2.0 0.5
5 E 1.5 2.5 0

1. Explain the shift in the colour by writing the equilibrium constant for the equilibrium [Fe (H20)]2+
+ SCN–(aq) = [Fe (H20)5 (SCN)]+2 + H2O
2. How do you explain the dynamic nature of the equilibrium?
3. Why very dilute solutions are required to carry out this experiment?
4. Carry out the experiment by adding solid potassium chloride to one of the boiling tubes and
explain your observation.
5. Use aqueous NaCl solution instead of concentrated HCl and record your observations.
6. Observe the effect of increasing temperature on solution at equilibrium and record it.
First Year 37
CHAPTER-6
QUANTITATIVE ESTIMATION
(TITRIMETRIC ANALYSIS)
The term titrimetric analysis refers to the quantitative chemical analysis. It is carried out by
determining the volume of the solution of exactly known concentration which is required to react
quantitatively with a substance present in a measured volume of the solution. The solution of
accurately known concentration is called the standard solution. The mass of the substance to be
determined is calculated from the volume of the standard solution used and balanced chemical
equation and the relative molecular masses of the reacting substances.
In the titrimetric analysis the substance of known concentration is called the titrant and the
substance being titrated is called the titrand. The standard solution is generally taken in a burette. The
process of adding the standard solution until the reaction is complete is called titration. Here, the
concentration of the substance to be determined is titrated. The reaction is complete is called the
equivalence point or the theoritical end point or stoichiometric end point. The completion of the re-
action is detected by some change produced sometimes by the standard solution itself or in most of the
cases by the addition of auxiliary reagent called indicator or by some other measurement. If an
indicator is used it may change its colour at the end point or cause turbidity etc., The point where the
observable change occurs is known as the end point of the titration.
The titrimetric analysis is useful mainly in the following conditions:
1. The reaction should be simple and could be expressed by a chemical equation.
2. The substances should reset completely in stoichiometric proportions.
3. The reactions should be fast. For this if necessary a catalyst may be used.
4. Equivalence point should be detected by a clearly observable change like colour in a direct
reaction or a reaction involving an indicator.
5. Indicator and the experimental conditions selected should be such that the difference between
the observed end point and the theoritical end point is the minimum possible.
6.1 Chemical (Analytical) Balance
The balance used for weighing the substances in titrimetric analysis is called analytical
(chemical) balance. The construction and the principle of working of the analytical balances are same
as those of physical balance except sensitivity and accuracy which are more for analytical balance.
Here, the mass of a substance upto + 0.0002 g accuracy can be weighed which is known as the least
count of the balance.

Description
The beam of the balance 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 agate or corun-
dum, a hard material. The plate is fixed on
the central pillar. The two terminal agate
knife edges are at equal distances from the
central edge. These two knife edges carry
suspension called strriups. There is a sharp
pointer attached at the centre of the beam
which can move on a scale at the bottom of
the pillar. A plumb line is also suspended
near the pillar to keep the balance horizontal. The balance gets operated when it is released with a knob
arranged at the centre of the base.
Weights: Weights include those in the main weight box (100, 50, 20, 20, 10, 5, 2, 2, 1 gram) and
fractional weight box (500, 200, 200, 100, 50, 20, 20, 10 mg and a rider to weigh 0.2 mg to 10 mg).
Fig. 6.2: Weighing bottle Fig. 6.3: Weight box and fractional weights
Setting of a chemical balance and weighing
Procedure
1. Level the balance with the help of travelling screws and plumb line. Using the screws on the
two sides of the beam adjust the pointer to zero point. If the balance is adjusted it should move
to equal number of divisions on both sides of the zero of the base scale. .
2. Place the weighing bottle on the left pan. Keep the weights nearly equal to the weighing bottle in
right pan with the help of forceps. Release the balance beam arrest and note the movement of the
pointer on the scale. If the weights are not appropriate the pointer would move towards less weight side.
If this happens, get the pans to rest and beam arrest with the help of the arrest and release the knob.
First Year 39
Add or remove weights accordingly so that on further release of beam arrest the. pointer should
move equal distances on the bottom pointer scale.
3. Rider is to be used for adjustment of weights between 0.0002 g and 0.01 g i.e maximum weight
that can be weighed with rider is 10 mg (0.01g). Main divisions on the beam give the weights in
the third decimal and sub divisions give the weights in the fourth decimal as multiples of 0.001g
and 0.0002 g respectively.
4. Suppose that the rider is after 6th main division and before the 7th main division and at 3rd sub
division on weights pan side, then the mass to be added to the weights is 0.0066 g.
Precautions
1. Carry necessary adjustments in the balance before starting the weighing.
2. To keep or remove the object in or from the left side pan use the left side door and for keeping or
removing weights into or from the right pan use right side door. Don't use the front shutter.
3. Before releasing the beam arrest gently, see that all side and the front doors are closed.
4. Pans should be always clean.
5. Use forceps for handling the weights.
6.2 Preparation of Standard Solution of Oxalic Acid
Aim: To prepare 250 mL of 0.05 M standard solution of oxalic acid.
Principle
Suppose that we want to determine the concentration of a given base solution that is unknown.
For this we can prepare an acid solution of known concentration with an acid that is available as a
primary standard and using this acid solution (which is also known as standard solution) we can find
out the concentration of the given base solution. Let us understand how a standard solution of oxalic
acid can be prepared. In titrimetric analysis we will use molar concentrations for the solutions. Then
the concentration would have units mol L-1
Oxalic acid is available as a hydrated crystalline substance. Its formula is (COOH)22H,0 and
molecular mass is 126.0 u.
If 126 g of oxalic acid is present in one litre of the solution, it is 1 M solution. We have to prepare 250.0
mL of 0.05 M solution of oxalic acid.
Mass of solute in grams
Molarity(M) =
Molar mass of solute  V in mL
1000 mL L-1
Mass of solute(g)  1000 mL L-1
Molarity(M) = = mL L-1
Molar mass of (gm of)-1  V(mL)
W ‘g’ of oxalic acid  1000 mL L-1

0.05 M =
126 g mol-1  250 mL

250 mL
W = 0.05 mol L-1  126 g mol-1  = 1.575 g
1000 mL L-1
Procedure
1. Using an analytical balance find the weight of a weighing bottle. Now in the same balance add about
1.58 g to weights pan and to that extent oxalic acid to the weighing bottle. Now find the weight of
weighing bottle with oxalic acid. The weight of weighing bottle with oxalic acid be W1g. Now
transfer oxalic acid carefully into a 250 mL standard flask using a funnel. Find the weight of the
weighing bottle after the transfer of oxalic acid into the measuring flask using analytical balance. Let
the weight of the weighing bottle after transfer of oxalic acid be W2. g. Weight of oxalic acid
transferred = W1(g) – W2(g) = Wg
Now wash the funnel number of times with distilled water into the standard flask to get any solute
sticking to the walls of the funnel to go into the solution. Remove the funnel. See that the flask gets
filled to an extent of 1/4 to 1/3 of its volume with water. Keep the stopper of the flask back and shake
the solution by giving rotatory motion to dissolve the solute completely. Now remove the stopper.
Add distilled water slowly until the lower miniscus of the solution coincides with the mark on the
flask. Shake the solution thoroughly to have uniform concentration to the solution. 1.575 g of oxalic
acid in 250 mL solution is 0.05 M. 'W' g of oxalic acid in 250 mL solution is
W2g
X 0.05 M = M1 mol L-1
1.575 g
where ‘M1' is the molarity of standard oxalic acid solution.
Note : A primary standard is a compound of sufficient purity from which a standard solution can be
prepared by direct weighing of a quantity of it, followed by dilution to give a defined volume of a
solution. The solution so produced is called a primary standard solution.
A primary standard should have the following requirements.
1. Easy to obtain, to purify, to dry at about 110 - 120°C and to preserve in pure state.
2. Should have high relative molecular mass. It should not be (i) hygroscopic (ii) oxidised by air
(iii) affected by Co2, and it should not have impurities.
3. Should be readily soluble, should participate in the reaction instantaneously and stoichiom
etrically.
In acid base titrations sodium carbonate (Na2CO3), benzoic acid (C6H5 COOH) etc. are used
as primary standards. In redox reactions potassium dichromate (K2Cr2O7), sodium oxalate (Na2C2O4)
etc., are used as primary standards. A secondary standard is a chemical substance that may be used for
standardizations and its content of the active substance is found by comparison against a primary
standard. It is to state that a secondary solution is a solution, the concentration of which is found not on
the basis of the weighed amount of the substance in the solution but by titrating the given volume of its
solution against a measured volume of a primary standard solution.
First Year 41
6.3 Indicators in Acid- Base Titrations and Redox Titrations
Acid-base indicators: These are also called neutralisation indicators. These indicators change their
colours according to the change in the concentration of hydrogen-ion in the solution i.e. pH of the
solution. They change their predominantly acid medium colour to a predominantly alkaline medium
colour not suddenly but slowly within a small interval of pH, about two units of pH generally,
Different indicators have the positions of the colour change intervals of pH different. For a given acid
base titration it is possible to select a suitable indicator based on the change of pH at its equivalence
point.
Ostwald theory of acid base indicators: This is based upon the concept that indicators generally
used are weak organic acids or bases. This theory of the colour change has been revised. Now it is
believed that the colour changes of indicators are due to structural changes including the formation of
quinonoid and resonance forms. Let us illustrate this theory with phenolphthalein indicator.
Phenolphthalein : Phenolphthalein is a weak acid. In relatively stronger acid medium it would be in
the unionized form which is colourless.
Hph  H+ + Ph-
Colourless Pink
H–
Lactone ring structure Triphenyl carbinol structure Resonating ion

I II III
Colourless in acid medium Pink in alkaline medium
Fig. 6.4: Structure of phenolphthalein
In acidic medium, the equilibrium shifts to the left i.e. the phenolphthalein solution is colourless.
Due to colourless phenolphthalein molecules formed in excess, in the alkaline medium the ionization
of phenolphthalein increases and the pink coloured Ph: increases and the solution gets pink colour.
Phenolphthalein is generally the most suitable indicator for 'weak acid-strong base titrations in addition
to strong acid-strong base titrations. Phenolphthalein changes its colour sharply in the pH range of 8.3 to
10.0. In the weak acid strong base titration also the end point appears on the addition of the last drop of
alkali at this pH range only. Chemical name of phenolphthalein is also phenolphthalein.
Methyl orange (dimethyl aminophenyl azobenzene sulphonic acid sodium salt)
Fig. 6.5: Structure of methyl orange

Methyl orange is a weak base. It has yellow colour in the unionized form. Generally it is taken
in the form of its sodium salt. The anion of this salt is the active species. It accepts a proton as Bronsted
Lowry base and changes from yellow benzenoid form to Pink quinonoid. The quinonoid form is deeper
in colour and it is responsible for the colour change at the end point. In alkaline medium it is in
benzenoid form and the solution would have yellow colour and on adding one drop excess of acid to
get the end point after neutralization the indicator changes predominantly to quinonoid form and the
solution becomes pinkish red in colour.
Yellow coloured benzenoid form Pinkish red coloured qunonoid form

Fig. 6.6: Different forms of methyl orange
Methyl orange anion changes its colours in the pH range of 2.9 to 4.6. Below 2.9 pH it gives
red colour and above 4.6 pH it gives yellow colour to the solution. This indicator is useful mainly for
strong acid-strong base titrations or strong acid-weak base titrations that get end points in this pH
range.
Detection of end point in redox reactions
We know that in acid-base titrations we use indicators which change their colours with the
sudden change in pH during the titrations. Similarly an oxidation - reduction indicator generally marks
the sudden change in the reduction potential in the neighbourhood of the equivalence point in an
oxidation - reduction titration. An ideal redox indicator is that which has reduction potential
intermediate between that of the solution titrated and that of the titrant and it should exhibit a sharp
and clearly detectable colour change.
In(ox) + ne-  In(red)
One such redox indicator for example is 1,10- phenanthroline iron(II) sulphate (ferroin). It has
pale blue colour in the oxidized form and red colour in the reduced form. At formal potential of 1.06 V
at pH =O it changes its colour.
In permanganate redox titrations Mno-4 acts as self indicator,
Acidimetry and Alkalimetry
6.4 Estimation of NaOH Present in the Given Solution Titrimetrically with
Standard Oxalic Acid Solution
Aim : Determination of the strength of a given solution of sodium hydroxide by titrating it against
standard solution of oxalic acid.
Principle
This titration involves a weak acid (oxalic acid) titration with a strong base (NaOH solution).
As the salt so formed is of strong base and weak acid it undergoes hydrolysis in water. Due to this,
even before reaching the equivalence point the pH of the solution is above 7. Therefore. the suitable
indicator is phenolphthalein.
H2C2O4 + 2 NaOH  Na2C2O4 + 2 H2O
First Year 43
Formula to calculate the concentration of NaOH solution: Generally we use molar concentrations
for the solutions. If M1. V1, and n1, are the molarity, volume and number of moles in the stoichiometric
equation of oxalic acid solution and M2, V2, and n2, are the molarity. volume and number of moles
(formula units) in the stoichiometric equation of sodium hydroxide then
M2 V2 M1V1 M Vn
= or M2 = 1 1 2
n2 n1 n1V2
Instead of stoichiometric coefficients we may use the basicity and acidity of respective acid
(oxalic acid) and base (sodium hydroxide).
Chemicals and apparatus required
Chemicals : Known molar (0.05 M) oxalic acid solution. Unknown molar
(nearly 0.1 M) NaOH solution Phenolphthalein indicator
Apparatus : Burette (50 ml), pipette (20 mL), conical flask (250 mL), burette
stand, funnel, white glazed tile
Procedure
1. Prepare 0.05 M oxalic acid solution by following the procedure given already.
2. Titration of oxalic acid solution against NaOH solution.
(a) Take a clean burette, wash it with distilled water, and finally with sodium
hydroxide solution which is to be taken into the burette.
(b) Fill the burette with the given NaOH solution through a funnel above zero mark. Remove the
excess of NaOH solution so that the lower miniscus of the NaOH solution coincides with zero
mark of the burette. There should be no air bubbles in the solution including in the nozzle.
Remove the funnel. If the initial reading is not at zero mark, note the exact reading. Let it be
(Vi) mL
(c) Take a 20 mL pipette. Wash it with distilled water and rinse it with the given 0.05M oxalic acid
solution. Pipette out 20 mL of oxalic acid solution into a clean washed and dried (not rinsed)
conical flask ( of 100 mL or 250 mL volume).
(d) Add 1 or 2 drops of phenolphthalein to oxalic acid solution taken in the conical flask and
shake the solution to mix the indicator and the solution. Keep the conical flask with oxalic
acid solution over a white glazed tile arranged under the burette.
(e) Titrate the oxalic acid solution against NaOH solution until just by adding one drop excess of
NaOH the colour of the solution changes from colourless to very faint permanent pink colour.
Note the burette reading with reference to the lower miniscus of the solution. Let it be V1.
(f) Repeat the experiment each time filling the burette upto zero mark with NaOH solution,
pipette out 20 mL (V1) of oxalic acid into washed conical flask and add a drop or two drops of
phenolphthalein indicator and titrate the oxalic acid solution against NaOH solution until the
solution in the conical flask turns faint permanent pink colour,
(g) Note the burette reading. Let it be Vf mL

(h) The experimental should be repeated to get the volumes of NaOH consumed to neutralize
oxalic acid the same atleast twice successively.
Table 6.1: Titration of sodium hydroxide solution Vs oxalic acid solution
SI. Volume of oxalic acid Burette Readings Volume of NaOH
No. solution pipetted out Initial V1 (mL) Final Vf (mL) solution run down
v1(mL) (Vf-Vi) = V2 (mL)
1 20
2 20
3 20
4 20
Molarity of oxalic acid solution = M1 = mol L-1
Volume of oxalic acid solution = V1 = 20 mL
Number of moles of oxalic acid (its stoichiometric coefficient) n1 = 1
Volume of NaOH solution = V2 = mL (From the table)
Number of moles of NaOH = n2 = 2
Molarity of NaOH solution = M2 = ? mol L-1
M 2V2 M 1V1 MVn

 orM 2  1 1 2
n2 n1 n1V2
Amout of NaOH per litre of solution
= M2 mol L-1 X 40 g mol-1 = M2 X 40 gL-1
Amount of NaOH per ‘V’ mL of solution
VmL  M 2 molL1  40 g.mol 1 V  M 2  40 g

= 
1000 1000 Fig. 6.4:
Process of titration
6.5 Preparation of Standard Solution of Sodium carbonate
Aim : To prepare 0.05 M solution of sodium carbonate of 250 mL volume.
Principle
Na2CO3 has characteristics almost of a primary standard. Its known molar (standard solution
may be prepared by dissolving a known weight of Na2CO3 in a known volume of the solution.
weight of the Na2CO3(w)g 1000 mL L-1

Molarity [M] = =
Gram molecular weight of volume of the solution
Na2CO3 (g mol-1) in mL
First Year 45
As we want 250 mL of 0.05 M Na2CO3 solution weight of Na2CO3 required is
V1 mL of solution
W = M x g. molecular wt. of Na2CO3 
1000 mL L-1
250 mL
W = 0.05 mol L  106 g mol-1 
-1
= 1.325 g.
1000 mL L-1
1.325 g in 250 mL  0.05 M
a x 0.05 M
‘a’ g in 250 mL  ? =
1.325
procedure
1. Using analytical balance weigh nearly 1.325 g of Na2CO3 (but exact amount of Na2CO3 weighed
and transferred should be clearly known) and transfer it into a cleanly washed 250 mL standard
flask with the help of a funnel.
2. Wash the funnel thoroughly and transfer the substance into the standard flask with distilled water.
Remove the funnel. Add some more distilled water to the flask (by this time the volume of the
solution in the flask may be about 100-125 mL).
3. Keep the stopper of the flask to close its mouth and shake the solution by rotator motion to
dissolve the solute Na2CO3 completely. Take out the stopper and add distilled water further until
the lower meniscus of the solution coincides with the mark on the neck of the flask.
4. Mix the solution thoroughly to have uniform concentration for it.
6.6 Determination of the Strength of the Given Hydrochloric Acid
Aim: To determine the strength (amount of it in 'g' per given volume of the solution) of the given
approximately 0.1 M hydrochloric acid. You would be provided with M1 molar (which is nearly 0.05
M but not exactly known concentration).
Principle
To determine the strength of the given hydrochloric acid using standard (M1 molar) sodium
carbonate solution.
Na2CO3 + 2HCl ––> 2NaCl + H2O + CO2
The reaction is an example for strong acid - weak base titration. Therefore methyl orange is a
suitable indicator for this titration. The indicator possesses red colour in acidic medium (pH < 2.9) and
yellow colour in basic medium pH>4.6. The end point comes at about 3.7 PH when 0.1 M Na2Co3 and
0.1 M HCl are used for titration. Here we neglect the secondary ionization and loss of H2CO3 due to
escape of CO2
If M1 V1 n1 are molarity, volume and number of stoichiometric moles of Na2CO3 in the solution
and M2 V2 and n2 those of hydrochloric acid, Then
M 2V2 M 1V1

n2 n1 From this relation M2 may calculated
M2  gram molecular mass of HCl = g of HCl per litre of solution

Burette (50 mL). pipette (20 ml), conical flask (250 mL). burette stand, funnel, white glazed
tile sodium Carbonate solution (0.05 M), hydrochloric acid (approximately 0.1 M) and methyl orange
Procedure
1. Preparation of 0.05 M Na2CO3, solution of 250 mL volume by weighing as already discussed.
2. You would be provided with approximately 0.1 M HCl which you would take in the cleanly
washed and rinsed burette with the help of funnel upto zero mark without any air bubbles in the
solution or in the nozzle.
Transfer 20.0 mL of Na2CO3, solution with a washed rinsed 20 ml pipette into a cleanly washed
conical flask. Add a drop or two of methyl range solution to it. The solution turns yellow. Titrate
Na2,CO3, solution against hydrochloric acid until just by adding one drop of excess of hydrochloric
acid the colour of the solution changes from yellow to light pinkish red. Note the volume of hydrochlo-
ric acid run down from burette readings. Repeat the experiment to get atleast two successive constant
values for the volumes of hydrochloric acid required to neutralize 20 mL of Na2,CO3, solution in each
experiment with methyl orange indicator.
Table 6.2: Titration of Na2CO3, solution against HCl solution
SI. Volume of Na2 CO3solution Burette Readings Volume of hydrochloric

No. in the conical flask Initial V1 (mL) Final Vf (mL) acid run down
v1(mL) (Vf-Vi) = V2 (mL)
1 20
2 20
3 20
4 20
Molarity of Na2CO3 solution (M1) = 0.05M Molarity of hydrochloric acid=(M2)=?

Volume of Na2CO3 solution (V1) = 20mL Volume of hydrochloric acid =((V2)=
Number of moles of Na2CO3 (n1) = 1 Number of moles of hydrochloric acid (n2)=2
(from stoichiometric equation) (from stoichiometric equation)
M 2 V2 M 1V1 M Vn
= or M 2 = 1 1 2
n2 n1 n 1V2
Molar mass of Na2CO3 = 106 g mol-1; molar mass of hydrochloric acid = 36.5 g mol-1Strength (or)
concentration of hydrochloric acid in gL-1 =M2xmolar mass of HCI
Result: The strength or concentration of given HCl solution = gL-1
Note
You may consider n1, as the number of moles of OH-given by 1 mole of base (here the base is Na2CO3)
i.e., the acidity of the base (Na2CO3 + 2H2O  2NaOH.+ H2CO3) and n2, the number of moles of H+
ions produced by 1 mole of acid i.e., basicity of the acid. Here basicity of HCl (HCl  H+ + Cl-) is one.
First Year 47
6.7 Precautions During Titrimetric Analysis
Part A
Weighing
1. The pans of the balance should be clean and the balance should be properly adjusted for equal
oscillations of the pointer on both sides of the ivory plate on its release. The side doors should
only be opened and closed during weighing.
2. Substances should be weighed with the weights including fractional weights with forceps.
Substances should not be spilled on the pans of the balance.
3. For colourless solution the lower meniscus should coincide with the marking. The solution should
be thoroughly mixed to have uniform concentration.
Part B
1. Always wash and rinse the burette and pipette with the respective solutions which are to be taken
in them in the beginning, but, never rinse the conical flask. Why it should not be rinsed?
2. All readings should be taken without parallax error.
3. For colourless transparent liquids or solutions the lower meniscus must
coincide with the marking but for coloured non transparent solutions the upper meniscus must
coincide with the marking.
4. See that no air gaps are present in the solutions of burette or pipette.
5. Don't blow the last drop of the solution in the pipette from its nozzle into the conical flask.
1. What difference do you find between a physical balance and an analytical balance?
2. Do you know about the maximum weight you can weigh with analytic balance?
3. What is the principle involved in the use of a rider?
4. You have to handle the weights with forceps. Why?
5. What are fractional weights? Why a weight like 0.2043 or 0.5265 we don't get with analytical
balance? (i.e., odd numbers in the fourth decimal division)
6. The rider rests between 5 and 6 main and 3rd sub division on the left side. What is its contribution
to the weights if weights are taken in the right pan?
7. Why the burette and pipette are rinsed with the solutions with which they are to be filled ?
8. What is an indicator ? Suggest with explanation the suitable indicators in the titration of
(i) strong acid-strong base (HCI Vs NaOH)
(ii) strong acid- weak base (HCI Vs NH4OH)
(iii) weak acid- strong base (oxalic acid Vs NaOH)
(iv) weak acid -weak base (CH,COOH VS NH4OH)

9. How can you titrate a mixture of Na2CO3, and NaHCO3, against HCI ?
10. What is quantitative analysis?
11. What is end point?
12. What is the principle in titrimetric analysis?
13. What is the maximum weight that can be weighed in a chemical balance?
14. What indicator is used in the titration of sodium carbonate against hydrochloric acid and what
is the colour change at the end point?

First Year 49
CHAPTER - 7
QUALITATIVE ANALYSIS
7.1 Introduction
Inorganic compounds such as Ammonium carbonate, Barium chloride, Calcium nitrate are
generally reffered to as simple salts. These simple salts are formed by neutralization of an acid with a
base. Thus a simple salt contains two constituents or parts. The part of the salt contributed by acid
(generally non-metallic entity) is anion and the part contributed by base(generally metallic entity) is
cation. Anions are negatively charged ions and cations are positively charged ions. Let us see some
examples of simple salts.
Name of the simple salt Formula Cation Anion
1. Ammonium carbonate, (NH4)2CO3, Ammonium (NH4+), Carbonate (CO32-)
2. Barium chloride, BaCl2, Barium(Ba2+), Chloride (Cl-)
3. Calcium nitrate, Ca(NO3)2, Calcium (Ca2+), Nitrate (NO3-)
4. Ferrous Sulphate, FeSO4, Ferrous (Fe2+), Sulphate(SO42-)
5. Ammonium acetate, CH3COONH4 Ammonium (NH4+), Acetate(CH3COO-)
In qualitative analysis of simplesalt, we identify the anion and the cation present in the simple
salt. Thus it is necessary to study the reactions of different anions and cations. The reactions of anions
are studied in the following order.
1. Test with dilute acid (dil.HCl/dil.H2SO4) for anions CO32-, CH3COO-, NO2- , S2-, SO32-
2. Test with conc. H2SO4 for anions Cl-, Br-, I-, NO3-
3. Individual tests for anions SO42- and PO43-
In the qualitative analysis of simple salt identification and confirmation of anion and cation is
necessary. As such the reactions of anions and cations includes both identification and confirmatory
tests for various anions and cations.

7.2 Reactions of Anions
In qualitative analysis of simple salt, we have to identify anions and cations. We now see the
individual reactions of anions and cations. For that we should be familiar with various anions and their
reactions. The following are the anions whose reactions we are going to study.
Name of the anion Formula

1. Acetate ion CH3COO-
2. Carbonate ion CO32-
3. Sulphide ion S2-
4. Sulphite ion SO32-
5. Nitrite ion NO2-
6. Chloride ion Cl-
7. Bromide ion Br-
8. Iodide ion I-
9. Nitrate ion NO3-
10. Sulphate ion SO42-
11. Phosphate ion PO43-
First Year 51
Reactions of Acetate ion (CH3 COO-)
(With Sodium acetate, CH3COONa)
Experiment Observation
1. Action of heat:
Take a small quantity of salt in a Colourless vapours with characteristic
dry test tube and heat strongly. vinegar like smell are evolved.
2. Action of dil.HCl:
Take a small quantity of the salt in Colourless vapours of acetic acid with
test tube and add a few drops of vinegar smell are evolved which turns
dil.HCl blue litmus red.
CH3COONa + HCl CH3COOH + NaCl
3. Test with solid Oxalic acid:

Take a small quantity of the salt in Characteristic vinegar like smell is
a watch glass and mix it with solid observed.
oxalic acid, paste the mixture with
water and rub the paste and ob-
serve the smell.
2CH3COONa + H2C2O4 Na2C2O4 + 2CH3COOH
4. Esterification test:
Take a small quantity of the salt in Fruity odour is observed due to the for-
a test tube, add conc.H2SO4 and mation of the ester ethly acetate.
heat. Now add ethanol and shake.
Pour the contents of the test tube
in a beaker contining full of water.
2CH3COONa + H2SO4 Na2SO4 + 2CH3COOH

CH3COOH + C2H5OH CH3COOC2H5 + H2O
5. Action of neutral FeCl3 solution:

To the salt solution add neutral Deep red filtrate is formed
ferric chloride solution and filter.
3CH3COONa + FeCl3 (CH3COO)3 Fe + 3NaCl

To the filtrate add water and boil Brown -red precipitate is formed
(CH3COO)3Fe + 2 H2O (CH3COO)(OH)2 Fe  + 2CH3COOH

Reactions of Carbonte ion (CO32-)
(With Sodium Carboante, Na2CO3, 10H2O)
1. Action of heat:
Take a small quantity of salt in a Colourless and odourless gas of
dry test tube and heat strongly. carbondioxide is evolved which puts
out the burning splinter.
CaCO3 CaO + CO2 
2. Action of dil.HCl:
Take a small quantity of the salt in Colourless and odourless gas of
a test tube and add a few drops of carbondioxide is evolved with brisk
dil.HCl effervescence.
Na2CO3 + 2HCl 2NaCl + H2O + CO2 
(i) Introduce a burning splinter The burning splinter puts out.

into the gas evolved in the above
test.
(ii) Pass the gas evolved in the Lime water turns milky.
above test into a test tube contain-
ing lime water.
Ca(OH)2 + CO2 CaCO3 + H2O
3. Action of BaCl2 solution : Take A white precipitate of barium carbon-

the salt solution in a test tube and ate is formed.
add a few drops of barium chlo-
ride solution.
Na2CO3 + BaCl2 BaCO3 + 2NaCl
(i) Solubility of the above precipi- The precipitate is soluble in dil.HCl.

tate is tested in dil.HCl
First Year 53
Reactions of Nitrite ion (NO2-)
(With Potassium nitrite, KNO2)
Experiment
Observation
1. Action of heat: Take a small Reddish brown vapours with pungent
quantity of salt in a dry test tube smell is evolved which turns ferrous
and heat strongly. sulphate solution black.
2. Action of dil.H2SO4: Take a small Reddish brown vapours with pungent

quantity of the salt in a test tube smell is evolved.
and add a few drops of dil.H2SO4.
2KNO2 + H2SO4 2HNO2 + K2SO4
3HNO2 HNO3 + 2NO + H2O
2 NO + O2 2NO2 
Introduce a paper soaked in acidified Starch - Iodide paper turns blue.

potassium iodide solution containing
strach solution into the test tube.
3. Action of FeSO4 solution: Take A dark brown or black colouration is

the salt solution in a test tube and obtained due to the formation of
add a few drops of dil.H2SO4 and FeSO4.NO
ferrous sulphate solution.
2KNO2 + H2SO4 2HNO2 + K2SO4
3HNO2 HNO3 + 2NO + H2O
FeSO4 + NO FeSO4.NO
4. Acton of KI+Starch solution: A blue coloured soluton is obtained.

Take the salt solution in a test tube
and add a few drops of dil.H2SO4
and add a few drops of potassium
iodide solution followed by freshly
prepared strach solution.
2KNO2 + H2SO4 K2SO4 + 2HNO2
2KI + 2H2SO4 + 2HNO2 2KHSO4 + I2 + 2NO + 2H2O
6. Action of Sulphanilic acid solu- A red colouration is obtained due to the

tion: Take the salt solution in a test formation of azodye.
tube and add a few drops of
sulphanilic acid solution and 2-3
drops of 1-naphthyl amine reagent.

Reactions of Sulphide ion (S2-)
(With Sodium sulphide, Na2S)
Experiment
Observation
1. Action of heat: Take a small Colourless gas with rotten eggs smell
quantity of salt in a dry test tube is evolved which turns lead acetate
and heat strongly. paper black.
2. Action of dil.HCl: Take a small Colourless gas with rotten eggs smell
quantity of the salt in a test tube is evolved which turns lead acetate
and add a few drops of dil.HCl paper black.
Na2S + 2HCl H2S  + 2NaCl
3. Action of Lead acetate solution: Black precipitate of lead sulphide is

Take the salt solution in a test tube formed.
and add a few drops of lead ac-
etate solution.
Na2S + (CH3COO)Pb PbS  + 2 CH3COONa
4. Action of Sodium Nitro Prusside Purple or voilet colouration is obtained

solution: Take the salt solution in due to formation of a complex com-
a test tube and add a few drops of pound.
ammonium hydroxide and to this
alkaline solution add sodium nitro
prusside solution.
Na2S + Na2[Fe(CN)5NO] Na4 [Fe(CN)5NOS]
5. Action of CdCO3 solution: Take An yellow precipitate of cadmium sul-

the salt solution in a test tube and phide is formed.
add a few drops of cadmium car-
bonate solution (a suspension of
cadmium carbonate in water).
Na2S + CdCO3 CdS  + Na2CO3
First Year 55
Reactions of Sulphite ion (SO32-)
(With Sodium sulphite, Na2SO3)
1. Action of heat: Take a small Colourless gas with pungent smell like
quantity of salt in a dry test tube burning sulphur (SO2) is evolved which
and heat strongly. turns acidified potassium dichromate
paper green.
Na2SO3 Na2O + SO2 
2. Action of dil.HCl: Take a small Colourless gas with pungent smell like
quantity of the salt in a test tube burning sulphur (SO2) is evolved which
and add a few drops of dil.HCl turns acidified potassium dichromate
paper green.
Na2SO3 + 2HCl 2NaCl + SO2 + H2O
3. Action of Lead acetate solution: A white precipitate of barium sulphite

Take the salt solution in a test tube is formed.
and add a few drops of barium
chloride solution.
Na2SO3 + BaCl2 BaSO3 +2NaCl
To the precipitate add a fefw drops of The pink colour of potassium

potassium permanganate solution permaganate solution gets discharged.
acidified with dil.H2SO4.
5BaSO3 + 2KMnO4 + 3H2SO4 5BaSO4 + 2MnSO4 + K2SO4 + 3H2O
4. Action of acidified K2Cr2O7

solution: Take the salt solution in A green colouration is obtained due to
a test tube and add a few drops of the formation of chromic sulphate.
potassium dichromate solution
acidified with dil.H2SO4.
3Na2SO3 + K2Cr2O7 + 4H2SO4 3Na2SO4 + Cr2 (SO4)3 + K2SO4 + 4H2O

Reactions of Chloride ion (Cl-)
(With Sodium chloride, NaCl)
1. Action of heat: Take a small quan- Colourless gas of hydrogen chloride is
tity of salt in a dry test tube and heat evolved.
strongly.
2. Action of conc.H2SO4: Take a small Colourless gas of hydrogen chloride
quantity of the solid salt in a test tube with pungent smell is evolved which
and add a few drops of conc.H2SO4 fumes in moist air.
2NaCl + H2SO4 Na2SO4 + 2 HCl
(i) A glass rod dipped in ammonium Dense white fumes of ammonium chlo-
hydroxide is brought near the mouth ride are formed.
of the test tube.
HCl(g) + NH3(g) NH4Cl(g)
3. Action of MnO2 and conc.H2SO4 Greenish yellow gas of chlorine with

: Take a small quantity of the solid salt pungent irritating smell is evolved
in a test tube and add a pinch of man- which turns moist starch-iodide paper
ganese dioxide and a few drops of blue.
conc.H2SO4 and heat
2Nacl + MnO2 + 3H2SO4 2NaHSO4 + MnSO4 + 2H2O +Cl2 
4. Chromyl chloride test: Take a small Deep red vapours of chromy1 chloride
quantity of the solid salt and mix (CrO2Cl2) are evolved.
with an equal amount of solid po-
tassium dichromate. Take this mix-
ture in a test tube and add a few
drops of conc.H2SO4 and heat.
4NaCl + K2Cr2O7 + 4H2SO4 2KHSO4 + 2Na2SO4 + 2CrO2Cl2 
(i) Pass the vapours into a test tube Yellow colour solution of sodium
containing sodium hydroxide solution. chromate is obtained
CrO2Cl2 + 4NaOH Na2CrO4 + 2H2O + 2NaCl
(ii) Acidify the yellow solution with Yellow precipitate of lead chromate is
acetic acid and add lead acetate formed.
solution.
Na2CrO4 + (CH3COO)2Pb PbCrO4  2CH3COONa
5. Action of AgNO3 solution: Take the Curdy white precipitate of silver
salt solution in a test tube and add a chloride is formed which is soluble in
few drops of silver nitrate solution. ammonium hydroxide.
NaCl + AgNO3 AgCl  + NaNO3
AgCl +2NH4OH [Ag (NH3)2Cl] + 2H2O
First Year 57
Reactions of Bromide ion (Br-)
(With Potassium bromide, KBr)
1. Action of heat: Take a small quan- Reddish brown vapours are evolved
tity of solid salt in a dry test tube and which turns starch paper yellow.
heat strongly.
2. Action of conc.H2SO4: Take a small Reddish brown vapours of bromine

quantity of the solid salt in a test tube along with colourless vapours of hydro-
and add a few drops of conc.H2SO4 gen bromide are evolved which turns
starch paper yellow.
KBr + H2SO4 KHSO4 + HBr
2HBr + H2SO4 SO2  + Br2  + 2H2O
A glass rod dipped in silver nitrate so- Pale yellow precipitate of silver bro-
lution is brought near the mouth of mide is formed on the glass rod.
the test tube.
HBr + AgNO3 AgBr  + HNO3
3. Actioin of MnO2 and conc.H2SO4: Reddish brown vapours of bromine with

Take a small quantity of the solid salt pungent smell are evolved in which
in a test tube and add a pinch of man- turns starch paper yellow.
ganese dioxide and a few drops of
conc.H2SO4
2KBr + MnO2 + 3H2SO4 2KHSO4 + MnSO4 + Br2  + 2H2O
4. Action of AgNO3 solution: Take the Pale yellow precipitate of silver bro-
salt solution in a test tube and add a mide is formed which is partially
few drops of silver nitrate solution. soluble in ammonium hydroxide.
KBr + AgNO3 AgBr  + KNO3
5. Chlorine water test: Take the salt The organic layer (non-aqueous layer)
solution in test tube and add a few drops acquires reddish brown colouration.
of chloroform (or carbon tetrachloride)
and excess of chlorine water dropwise
and shake the test tube vigorously.
2KBr + Cl2 2KCl + Br2
6. Action of Pb(CH3COO)2 solution: White precipitate of lead bromide is

Take the salt solution in a test tube and formed which dissolves when heated
add a few drops of lead acetate with water.
solution
2KBr + Pb(CH3COO)2 PbBr2  + 2 CH3COOK
Reactions of Iodide ion (I-)
(With Potassium iodide, KI)
1. Action of heat: Take a small quan- Violet vapours are evolved which turns
tity of solid salt in a dry test tube and starch paper blue.
heat strongly.
2. Action of conc.H2SO4: Take a small Violet vapours of iodine are evolved

quantity of the solid salt in a test tube which turns starch paper blue and a layer
an d add a f ew d r o p s o f co n c.H 2SO4 of violet sublimate is formed on the
sides of the test tube.
KI + H2SO4 KHSO4 + HI
2HI+ H2SO4 SO2  + I2  + 2H2O
3. Actioin of MnO2 and conc.H2SO4: Violet vapours of iodine are evolved

Take a small quantity of the solid salt which turns starch paper blue.
in a test tube and add a pinch of man-
ganese dioxide and a few drops of
conc.H2SO4
2KI + MnO2 + 3H2SO4 2KHSO4 + MnSO4 + I2  + 2H2O
4. Action of AgNO3 solution: Take the Yellow precipitate of silver iodide is

salt solution in a test tube and add a formed which is insoluble in ammonium
few drops of silver nitrate solution. hydroxide.
KI + AgNO3 Ag I  + KNO3
5. Chlorine water test: Take the salt The organic layer (non-aqueous layer)
solution in test tube and add a few acquires a violet colouration.
drops of chloroform and excess of
chlorine water dropwise and shake
the test tube vigorously.
2KI + Cl2 2KCl +I2
First Year 59
Reactions of Nitrate ion (NO3-)
(With Lead nitrate, Pb(NO3)2)
1. Action of heat: Take a small quan- Reddish brown vapours are evolved.
tity of solid salt in a dry test tube and
heat strongly.
2Pb(NO3)2 2 PbO + N O 2  + O2 
2. Action of conc.H2SO4: Take a small Reddish brown vapours of nitrogen di

quantity of the solid salt in a test tube oxide are evolved.
and add a few drops of conc.H2SO4 and
warm if necessary.
Pb(NO3)2 + H2SO4 PbSO4 + 2HNO3
4HNO3 4NO2  + O2+ 2H2O
3. Action of copper turnings and Reddish brown vapours of nitrogen di

conc.H2SO4: Take a small quantity of oxide are evolved vigorously and the
the solid salt in a test tube and add a solution in the test tube becomes blue
few pieces of copper turnings and a few due to the formation of copper sulphate.
drops of conc.H2SO4 and heat.
Cu + 4HNO3 Cu(NO3)2 + 2NO2  2H2O
4. Brown ring Test: Take the salt solu- A dark brown ring is formed at the junc-
tion (or sodium carbonate extract of the tion of the two layers (acid and solu-
salt) in a test tube and add freshly pre- tion layers) due to the formation of
pared ferrous sulphate solution in ex- nitroso ferrous sulphate (FeSO4.NO)
cess. To this, conc.sulphuric acid is
added slowly along the sides of the test
tube keeping the test tube in an inclined
position.
6FeSO4 + 3H2SO4 +2HNO3 3Fe2(SO4)3 + 2NO + 4H2O
FeSO4 + NO + 5 H2O Fe[(NO)(H2O)5]SO4
Fig.7.1 Brown ring test for nitrate ion

Reactions of Sulphate ion (SO42-)
(With Potassium sulphate, K2SO4, 10H2O)
1. Action of heat: Take a small Most of the sulphates are stable and do
quantity of solid salt in a dry test tube not decompose on heating. However
and heat strongly. certain sulphates decomposes on heat-
ing and liberates SO2 and SO3 gases.
2FeSO4 Fe2O3 + SO3  + SO2 
CuSO4 CuO + SO3
2. Action of BaCl2 solution: Take the White crystalline precipitate of barium

salt solution in a test tube and add sulphate is formed.
barium chloride solution.
K2SO4 + BaCl2 BaSO4  + 2KCl
The solubility of the precipitate is tested The precipitate is insoluble in conc.HCl

in conc.HCl.
3. Action of Lead acetate solution: White precipitate of lead sulphate is

Take the salt solution in a test tube and formed which is soluble in excess of
add a few drops of lead acetate ammonium acetate solution.
solution.
K2SO4 + (CH3COOH)2 Pb PbSO4  + 2CH3COOK
4. Match stick test: Take a small Violet streaks are produced.

amount of the salt, sodium carbonate
and powdered charcoal in a watch glass.
Make it into a paste and take some of
the paste on one end of a wooden
splinter and heat in the reducing flame
till the mass fuses. Dip the fused mass
into sodium nitroprusside solution
taken in a china dish.
First Year 61
Reactions of Phosphate ion (PO43-)
1. Ammonium molybdate test: To the A canary yellow precipitate of ammo-
aqueous salt solution add conc.nitric nium phosphomolybdate
acid and excess of ammonium mo-
lybdate solution and boil.
Na2HPO4 + 12 (NH4)2 MoO4 + 23 HNO3 (NH4)3[P (MoO10)4]  + 2NaNO3+21NH4NO3+12H2O
2. Magnesia mixture test: To the A white precipitate of magnesium ammo-

aqueous salt solution add magnesia nium phosphate is formed.
mixture and allow to stand.
Na2HPO4 + MgCl2 + NH4OH Mg(NH4)PO4  + 2NaCl + H2O
(Magnesia mixture is prepared by

adding solid ammonium chloride to
magnesium chloride solution and
boil. Cool the solution and add am-
monium hydroxide till strong smell
of ammonia is observed.)

7.3 Tests for confirmation of Anions
In qualitative analysis of inorganic salts tests are to be carried out for confirmation of anion in
the given salt. For this original salt solution is to be prepared and the confirmation tests are performed
with their solutions. Depending upon the solubility of the given salt, the original solution may be
prepared in any one of the following manner.
1. Aqueous solution or water extract
Take a pinch of salt in a test tube and add distilled water and shake throughly. If the salt
dissolves completely in water, this aqueous solution is used for tests for anions. But if the salt does not
form clear solution upon dissolving in water, then filter the solution and the filtrate is called water
extract and is used for confirmatory tests for anions.
2. Preparation of sodium carbonate extract
In qualitative analysis, the confirmatory tests for anions are performed with the salt solutions.
In this process in some cases the cations interfere and form precipitate leading to incorrect to incorrect
inference. In such cases, the cations which interfere are to be eliminated by replacing them with soluble
cations like sodium.
Preparation of sodium carbonate extract

Mix about 1.0 g of the salt with 3.0 g of solid sodium carbonate in a beaker and add about
20mL of distilled water. Boil this for about 10-15 minutes and filter and cool. The filtrate is called
sodium carbonate extract. This is used for confirmation of anions chloride. bromide, iodide, nitrate
and sulphate.
Note
1. For carbonate ion do not use sodium carbonate extract of the salt for performing wet tests, as
the extract contains carbonate.
2. Sodium carbonate extract always contains unreacted sodium carbonate, which is alkaline. So
the extract is to be neutralised with suitable dilute acid depending on the anion to be identified.
First Year 63
Test with Sodium carbonate extract
(For confirmation of anions)
1. Test for chloride: Neutralise the A white precipitate of silver chloride is
extract with dil.HNO 3 till the formed, which is completely soluble in
efferverscence ceases and add siver ni- ammonium hydroxide.
trate solution to it.
Ag+ + Cl– Agcl 
AgCl + 2NH3 [Ag(NH3)2] Cl
2. Test for Bromide: Neutralise the A pale yellow precipitate of silver bro-
extract with dil.HNO3 till the efferve- mide is formed, which is partially
scence ceases and add siver nitrate so- soluble in ammonium hydroxide.
lution to it.
Ag+ + Br- AgBr 
3. Test for Iodide: Neutralise the ex- An yellow precipitate of silver iodide
tract with dil.HNO3 till the efferves- is formed. Which is insoluble in ammo-
cence ceases and add siver nitrate so- nium hydroxide .
lution to it.
Ag+ + I- AgI
4. Brown ring test for Nitrate: A dark brown ring is formed at the junc-
Nuetralise the sodium carbonate extract tion of the layers of the acid and the
of the salt with dil.H2SO4 till the effer- solution.
vescence ceases. Add freshly prepared
saturated solution of ferrous sulphate
and Conc.H2SO4 dropwise along the
sides of the test tube, keeping the test
tube in inclined position.
6FeSO4 + 3H2SO4 + 2HNO3 3Fe2(SO4)3 + 2NO + 4H2O
FeSO4 + NO + 5H2O Fe[(NO)(H2O)5]SO4
5. Test for sulphate: Neutralise the A white crystalline precipitate of barium

sodium carboante extract of the salt sulphate is formed, which is insoluble
with dil.HCl till the effervescence in conc.HCl
ceases. Add barium chloride solution.
Ba+2+ SO42- BaSO4 
7.4 Reaction of cations
The basic part of a simpel salt is cation. In qualitative analysis, the preliminary tests such as
action of heat, flame test, charcoal cavity test and borax bead test gives an indication of cation present
in the simple salt. Finally the cations are confirmed by a systematic analysis of the salt. For the
systematic identification, the cation are tested with suitable group reagent. Let us now see various
group reagents, the cation present in various groups and the precipitates formed in various groups
which are given below.
Group Cations Group reagent Colour of the Precipi-

Precipitate tate
Group I Pb2+ Dil.HCl White PbCl2
Group II Pb2+ Black PbS

Dil.HCl + H2S
Cu2+ Black CuS
Al3+ White Al(OH)3
Group III Fe2+ NH4Cl+NH4OH Light green Fe(OH)2
Fe3+ Brown Fe(OH)3
Zn2+ White Zns
Group IV Mn2+ Flesh colour MnS
NH4Cl+NH4OH + H2S
Co2+ Black CoS
Ni2+ Black NiS
Ba2+ White BaCO3

Ca2+ NH4Cl+NH4OH + (NH4)2CO3 White CaCO3
Group V
Sr2+ White SrCO3
Group VI Mg2+ No spacific group reagent ----- -----
Let us now study some preliminary tests like flame test, borax bead test and char-
coal cavity test which gives an indication of the cation present in the given salt in
the qualitative analysis.
First Year 65
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 follows:
Procedure
Clean the platinum wire by dipping it in conc. HCI taken in a watch glass find heat the plati-
num wire strongly in the flame. Continue this process till the wire imparts no colour to the flame.
Prepare a paste of the salt and conc. HCl in a watch glas. Take some paste on the platinum wire loop
and introduce it into the non-luminous flame of the burner. Note the colour imparted to the flame.
Depending upon the colour imparted to the flame the cation present in the salt may be predicted.
Platinum loop
Paste
(a) Making a loop of (b) Dipping the platinum (c) Introducing the
platinum wire wire in the paste of platinum wire
salt and conc. HCI in the flame
Fig. 7.2: Flame test
Colour of the flame Inference (Cation present)
1. Brick red Calcium (Ca2+)
2. Light apple(grassy) green Barium (Ba2+)
3. Crimson red Strontium (Sr2+)
4. Bluish green Copper (Cu2+)
5. Green flashes Zinc (Zn2+)
Borax bead test

This test is performed only for coloured salts. Because borax reacts with metal salts to form
metal borates or metals. These metal borates or metals have characteristic colours.
Procedure
Make a loop at the end of a platinum wire and heat it in a flame to red hot. Dip the hot loop into
borax powder and heat it again until borax forms a colourless transparent bead on the loop. Then dip
the borax bead in the coloured salt and heat it in the flame. Observe the colour imparted to the bead in
the luminous and non-luminous flame in both cold and hot conditions. The colour imparted to the bead
gives an indication of the cation present in the salt.

Colour of the bead in oxidising Colour of the bead in reducing Inference (cat-
flame flame ion present)
1. Green when hot, blue when Colourless when hot, red Copper (Cu+2)
cold opaque when cold
2. Yellowish brown when hot, Green in both hot and cold Iron (Fe2+ or Fe3+)
yellow when cold conditions
3. Light violet in both hot and Colourless in both hot and Manganese (Mn2+)
cold condition cold conditions
4. Reddish brown when hot, Grey when hot, opaque when Nickel (Ni2+)
violet when cold cold
Charcoal cavity test
Charcoal cavity test is based on the fact that metallic carbonates when heated in a charcoal
cavity decompose to give corresponding oxides. The oxides appear as coloured residue in the charcoal
cavity. In certain cases, the oxides formed partially undergo reduce metals to produce metallic beads.
Procedure
Make a small cavity on a charcoal block with the help of a borer. Mix a small quantity of the
salt with double its quantity of sodium carbonate. Place it in the cavity made on the charcoal block and
moisten it with a drop of water. Now, direct the reducing flame of the Bunsen burner on the cavity by
means of a mouth blow pipe. Heat strongly for some time and observe the colour of the residue and of
metallic bead both in hot and cold conditions.
Observation Inference
1. Yellow residue when hot and grey metal when cold Lead (Pb2+)
2. Yellow residue when hot and white when cold Zinc (Zn2+)
3. Red metallic beads Copper (Cu2+)
4. White residue which glows Ba2+, Ca2+, Mg2+
Cobalt nitrate test
This test is performed for those salts which leaves a white residue in charcoal cavity test. To
perform this test put 1 or 2 drops of cobalt nitrate solution on the white residue left after charcoal
cavity test. Heat for two minutes in oxidizing flame by means of a blow pipe. Observe the colour of the
residue. This gives an indication of the cation present in the salt.
Colour of the residue Inference

1. Green Zinc (Zn2+)
2. Pink Magnesium (Mg2+)
3. Blue Aluminium (Al3+)
In qualitative analysis of simple salt, we have to identify anions and cations. We now see the
individual reactions of anions and cations. For that we should be familiar with various cations and
their reactions. The following are the cations whose reactions we are going to study.
Lead (Pb2+), Copper (Cu2+), Aluminium (A13+), Ferrous (Fe2+), Ferric (Fe3+), Zinc (Zn2+).
Manganese (Mn2+), Nickle (Ni2+), Cobalt (Co2+), Barium (Ba2+), Strontium (Sr2+), Calcium (Ca2+).
Magnesium (Mg2+), Ammonium (NH4+).
First Year 67
Reactions of Lead ion (Pb2+)
(With 5% Lead nitrate, Pb(NO3)2 solution containing some acetic acid)
1. Action of heat: Take a small quantity of Salts like Pb(NO3)2 on heating gives crack-
solid salt in a dry test tube and heat strongly. ling sound with liberation of reddish bro
vapours of NO2
2 Pb(NO3)2 2PbO + 4NO2 + O2
2. Action of dil.HCl: Take a small quan- A white precipitate of lead chloride is

tity of the salt solution in a test tube and formed which is soluble in hot water. The
add a few drops of dil.HCI. precipitate settles on cooling as PbCI2 is
not soluble in cold water.
Pb(NO3)2 + 2HCl PbCl2 + 2HNO3
3. Action of K2CrO4 solution: Take the An yellow precipitate of lead chromate is

salt solution in a test tube and add a few formed which is soluble in hot sodium hy-
drops of potassium chromate (K2CrO4) droxide solution and insoluble in ammo-
solution. nium hydroxide.
Pb(NO3)2 + K2CrO4 PbCrO4  + 2KNO3
4. Action of KI solution: Take the salt An yellow precipitate of lead iodide is

solution in a test tube and add a few drops formed which is soluble in hot water. On
of potassium iodide (KI)solution. cooling the colourless solution 'Golden yel-
low spangles of lead iodide separates.
Pb(NO3)2 + 2KI Pbl2  + 2KNO3
5. Action of dil.H2SO4: Take the salt A white precipitate of lead sulphate is

solution in a test tube and add a few drops formed | which is soluble in dil.nitric acid
of dil.H2SO4 and sodium hydroxide solution.
6. Flame test: Perform flame test and Dull bluish white coloured flame is ob-
observe the colour imparted to the flame. served.
7. Charcoal test: Perform charcoal cavity

test and observe the colour of the residue The residue is brown when hot and
in both cold and hot conditions. yellowishgrey when cold

Reactions of Copper ion (Cu2+)
(With 4% CuSO4.5H2O solution containing 0.5 mL of dil.H2SO4)
1. Action of heat: Take a small quantity of Salts like CuSO4.5H2O on heating loses its
solid salt in a dry test tube and heat blue colour and becomes white and loses
strongly. water molecules.
CuSO4.5H2O CuSO4 + 5H2O
Blue Colourless
2. Action of dil.HCl and H2S: Take a small A black precipitate of cupric sulphide is
quantity of the salt solution in a test tube formed which is soluble in hot dilute nitric
and add a few drops of dil.HCl and pass acid.
H2S gas.
CuSO4 + 2HCl CuCl2 + 2H2SO4
CuCl2 + H2S CuS  + 2HCl
3. Action of caustic soda solution: Take A blue precipitate of cupric hydroxide is
the salt solution in a test tube and add a formed which on heating changes to black
few drops of sodium hydroxide (NaOH) cupric oxide.
solution.
CuSO4 + 2NaOH Cu(OH)2  + Na2SO4
Cu(OH)2 CuO + H2O
4. Action of K4[Fe(CN)6) solution: Take A chacolate brown precipitate of cupric
the salt solution in a test tube and add a ferrocyanide is formed which is soluble in
few drops of potassium ferrocyanide dil.HCI.
K4[Fe(CN)6) solution.
2CuSO4 + K4[Fe(CN)6) Cu2[Fe(CN)6)  + 2K2SO4
5. Action of Ammonium hydroxide: Take A greenish blue precipitate of the basic salt
the salt solution in a test tube and add a is formed which is soluble in excess of
few drops of ammonium hydroxide ammonium hydroxide due to the formation
(NH4OH) solution. of the complex tetra ammine cupric sul-
phate.
2 CuSO4 + 2 NH4OH (NH4)2SO4 + Cu(OH)2.CuSO4
(NH4)2SO4 + Cu(OH)2.CuSO4 + 6 NH3 2 [Cu(NH3)4 SO4) + 2 H2O
6. Flame test: The characteristic colour Blue or bluish green flame is observed.
imparted to the flame is observed.
7. Borax bead test: The colour of the bead Heating in non-luminous(oxidising)

is observed separately in oxidizing and re- flame: Green when hot and light blue in cold.
ducing flames both in hot and cold condi- Heating in luminous(reducing) flame:
tions. Colourless when hot and red in cold.
First Year 69
Reactions of Aluminium ion(Al3+)
(With 12.5% Al2(SO4)3.18H2O solution containing 2 mL of dil.H2SO4)
1. Action of heat: Take a small quantity of Salts like Al2(SO4)3.2H2O on heating loses
solid salt in a dry test tube and heat strongly. water molecules as water of crystallisation.
2. Action of NH4OH: Take a small quan- A white precipitate of aluminium hydrox-
tity of the salt solution in a test tube and ide is formed which is slightly soluble in
add ammonium hydroxide drop wise. excess of ammonia solution.
A12(SO4)3 + 6 NH4OH 2 Al(OH)3  + 3 (NH4)2SO4
3. Action of Caustic soda solution: Take
the salt solution in a test tube and add a A white gelatinous precipitate of aluminium
few drops of sodium hydroxide (NaOH) hydroxide is soluble in excess of NaOH
solution. solution to form sodium meta aluminate.
Al2(SO4)3 + 6 NaOH 2 Al(OH)3  + 3Na2SO4
Al(OH)3 + NaOH NaAlO2 + 2 H2O
4. Action of NH4Cl and NH4OH: Take the A white gelatinous precipitate of aluminium
salt solution in a test tube and saturate it hydroxide is formed which is soluble in
with solid ammonium chloride and add sodium hydroxide solution but insoluble in
ammonium hydroxide in excess. mineral acids.
Al2(SO4)3 + 6 NH4OH 2 Al(OH)3  + 3 (NH4)2 SO4
5. Action of sodium carbonate solution:
Take the salt solution in a test tube and add A white precipitate of aluminium carbon-
a few drops of sodium carbonate (Na2CO3) ate is formed which is soluble in excess of
solution. sodium carbonate solution.
Al2(SO4)3 + 3 Na2CO3 Al2(CO3)3  + 3Na2SO4
6. Action of Na2 HPO4 solution: Take the A white gelatinous precipitate of aluminium
salt solution in a test tube and add a few phosphate is formed which is soluble in so-
drops of disodium hydrogen phosphate dium hydroxide solution and in mineral
(Na2HPO4) solution. acids.
A12(SO4)3 + 4 Na2HPO4 2A1PO4  + 3Na2SO4 + 2NaH2PO4
7. Lake test: Take the salt solution in a Blue coloured mass (precipitate) floating
test tube and add a few drops of ammo- in the solution is observed.
nium hydroxide (NH4OH). Dissolve the (As the blue mass floats in the solution, the
aluminium hydroxide precipitate formed in test is called 'Lake test)
dil.HCl and add 2-3 drops of blue litmus
solution. Add NH4OH till blue colour ap-
pears.
Al(OH)3 + 3HCl AICI3 + 3H2O
AICI3 + 3 NH4OH NH4CI + AÍ(OH)3
Blue colour - adsorbs on this ppt.

Reactions of Ferrous ion (Fe2+)
(With FeSO4(NH4)2SO4.6H2O solution containing 2 mL of dil.H2SO4)
1. Action of heat: Take a small quantity of Salts like FeSO4,decomposes on heating.
solid salt in a dry test tube and heat strongly.
2FeSO4 Fe2O3 + SO3  + SO2 
2. Action of NH OH: Take a small quan- A light green precipitate of ferrous hydrox-
tity of the salt solution in a test tube and ide is formed which is soluble in dilute acids.
add ammonium hydroxide.
FeSO4 + 2NH4OH Fe(OH)2 + +(NH4)2 SO4
3. Action of caustic soda solution: Take A light green precipitate of ferrous hydrox-
the salt solution in a test tube and add so- ide is formed which on aerial oxidation
dium hydroxide (NaOH) solution. changes to reddish brown precipitate of
ferric hydroxide.
FeSO4 + 2NaOH Fe(OH)2  + Na2SO4
4Fe(OH)2 + 2 H2O 4Fe(OH)3 
4. Action of NH4 Cl and NH4OH: Take A light green precipitate of ferrous hydrox-
the salt solution in a test tube and saturate ide is formed which is soluble in sodium
it with solid ammonium chloride and add hydroxide solution in mineral acids.
ammonium hydroxide in excess.
FeSO4 + 2NH4OH Fe(OH)2  + (NH4)2 SO4
5. Action of K [Fe(CN).] solution: Take A white precipitate of ferrous ferrocyanide
the salt solution in a test tube and add po- is formed which changes to light blue pre-
tassium ferrocyanide solution. cipitate of ferric ferrocyanide due to aerial
oxidation.
FeSO4 + K4[Fe(CN)6] K2Fe[Fe(CN)6]  + K2SO4
6. Action of K3(Fe(CN)6l solution: Take A deep blue precipitate (Turnbull's blue) of
the salt solution in a test tube and add po- potassium ferric ferrocyanide is formed.
tassium ferricyanide solution.
FeSO4 +K4[Fe(CN)6] KFe[Fe(CN)6]  + K2SO4
7. Action of KMnO4 solution: Take the The pink colour of potassium permangan-
salt solution in a test tube and add a few ate decolourises.
drops of dil. H2SO4 and potassium perman-
ganate solution
10FeSO4 + 8H2SO4 + 2KMnO4 K 2SO 4+ 2MnSO 4 + 5Fe2(SO 4)3 +8H20
8. Action of K2Cr2O7 solution: Take the Green colouration is obtained due to the
salt solution in a test tube and add a few formation of chromic sulphate.
drops of dil. H2SO4 and potassium dichro-
mate solution.
6FeSO4 + K2Cr2O7 + 7H2SO4 3Fe2(SO4)3 + Cr2(SO4)3 + K2SO4 + 7H2O
9. Borax bead test: The colour of the bead Heating in non-luminous(oxidising)
is observed separately in oxidizing and re- flame: Yellowish brown when hot and pale
ducing flames both in hot and cold condi- yellow when cold.
tions. Heating in luminous(reducing) flame:
Greenish in both hot and cold conditions.
First Year 71
Reactions of Ferric ion (Fe3+)
(With Ferric sulphate, Fe2(SO4)3 solution containing 2mL of dil.H2SO4)
1. Action of heat: Take a small quantity of Salts like Fe2(SO4)3 decomposes on heating
solid salt in a dry test tube and heat strongly. giving SO3 gas.
Fe2(SO4)3 Fe2O3 + 3SO3 
2. Action of NH4OH: Take a small quantity A reddish brown precipitate of ferri hydroxide
of the salt solution in a test tube and add ex- is formed which is soluble in dilute HCI.
cess of ammonium hydroxide.
Fe2(SO4)3 + 6NH4OH 2Fe(OH)3  + 3(NH4)2SO4
3. Action of caustic soda solution: Take the A reddish brown precipitate of ferric hydrox-
salt solution in a test tube and add sodium hy- ide is formed which is soluble in dilute HCI.
droxide (NaOH)solution.
Fe2(SO4)3 + 6NaOH Fe(OH)3 + 3Na2SO4
4. Action of NH4Cl and NH2OH: Take the A reddish brown precipitate of ferric hydrox-
salt solution in a test tube and saturate it with ide is formed which is soluble in sodium hy-
solid ammonium chloride and add ammonium droxide solution and in mineral acids.
hydroxide in excess.
Fe2(SO4)3 + 6NH4OH 2Fe(OH)3  +3(NH4)2SO4
5. Action of K4[Fe(CN)6] solution: Take the A light blue (Prussian blue) precipitate of fer-
salt solution in a test tube and add potassium ric ferrocyanide is formed.
ferrocyanide solution.
2Fe2(SO4)3 + 3K4[Fe(CN)6] Fe4[Fe(CN)6]3  + 6K2SO4
Excess of potassium ferrocyanide solution A colloidal solution of potassium ferric ferro
is added. cyanide.
Fe2(SO4)3 +2K4[Fe(CN)6] 2K Fe[Fe(CN)6] + 3K2SO4
6. Action of KCNS solution: Take the salt so- A blood red colouration is formed due to the
lution in a test tube and add potassium thiocy- formation of ferric sulphocyanide.
anate solution.
Fe2(SO4)3 + 6KCNS 2Fe(CNS)3 + 3K2SO4
7. Borax bead test: The colour of the bead is Heating in non-luminous (oxidising) flame:
observed separately in oxidizing and reduc- Yellowish brown when hot and pale yellow
ing flames both in hot and cold conditions. when cold.
Heating in luminous (reducing) flame: Green
in both hot and cold conditions.

Reactions of Zinc ion(Zn2+)
(With 4.4% ZnSO4. 7H2O solution)
1. Action of heat: Take a small quantity of Salts like ZnCo3 decomposes on heating and
salt in a dry test tube and heat strongly. liberates Co2 gas. The salt appears yellow when
hot and white when cold.
ZnCO3 ZnO + CO2 
2. Action of Caustic soda: Take a small quan- A white precipitate of zinc hydroxide is formed
tity of salt solution in a test tube and add so- which is soluble in excess of the reagent to give
dium hydroxide solution. sodium zincate.
ZnSO4 + 2NaOH Zn(OH)2  + Na2SO4
Zn(OH)2 + 2NaOH Na2ZnO2 + 2H2O
3. Action of NH4OH: Take a small quantity A white gelatinous precipitate of Zn(OH)2 is

of the salt solution in a test tube and add am- formed which dissolves in excess of
monium hydroxide. ammonium hydroxide.
ZnSO4 + 2NH4OH Zn(OH)2  + (NH4)2SO4
4. Action of NH4CI, NH4OH and H2S: Take A white precipitate of zinc sulphide is formed
the salt solution in a test tube and saturate it which is soluble in dilute acids and alkalies.
with solid ammonium chloride and add am-
monium hydroxide and pass H2S gas through
the solution.
ZnSO4 + H2S ZnS + H2SO4
5. Action of K4[Fe(CN)6) : Take the salt A grey-white precipitate of zinc potassium

solution in a test tube and add potassium ferro ferro cyanide is formed which is soluble in
cyanide solution. sodium hydroxide solution.
3 ZnSO4 + 2 K4[Fe(CN)6] Zn3K2 (Fe(CN)6]  + 3K2SO4
6. Action of K3[Fe(CN)6): Take the salt An orange precipitate of zinc ferri cyanide is
solution in a test tube and add potassium ferri- formed.
cyanide solution.
7. Flame test: The characteristic colour Green flashes are observed.

imparted to the flame is observed
8. Charcoal test/ Cobalt nitrate test: The residue is yellow when hot and white when
Perform charcoal cavity test. If white residue cold. On performing cobalt nitrate test green
is obtained in hot or cold condition, then per- residue of ZnO.CoO is obtained.
form cobalt nitrate test.
ZnO + CoO ZnO.CoO (Green)
First Year 73
Reactions of Manganese ion (Mn2+)
(With 4% Manganous chloride. MnCl2. 2H2O solution)
1. Action of caustic soda: Take a small A white precipitate of manganous hydroxide,
quantity of salt solution in a test tube and add formed which changes to brown on exposure
sodium hydroxide solution. air. The precipitate is insoluble in excess of
the reagent.
MnCl2 + 2NaOH M n(OH) 2  + 2NaCl

Mn(OH)2 + (O) MnO.(OH)2
2. Action of NH4OH: Take a small quantity A dull white precipitate of Mn(OH)2 is formed
of the salt solution in a test tube and add am- which dissolves in excess of ammonium hy-
monium hydroxide. droxide.
MnCl2 + 2NH4OH Mn(OH)2  + 2NH4Cl
3. Action of NH4Cl, NH4OH and H2S: Take A flesh coloured (buff coloured) precipitate of
the salt solution in a test tube and saturate it manganous sulphide is formed.
the solution.
MnCl2 + H2S MnS + 2HCl
4. Action of NaOH and Br2:Take the salt so- A white precipitate of Mn(OH)2 is formed
lution in a test tube and add sodium hydroxide which turns brown on addition of bromine
in excess and bromine water and boil. water due to its oxidation to manganic hydrox-
ide [MnO(OH)2]
MnCl2 + 2NaOH Mn(OH)2  + 2NaCl
Br2 + H2O 2HBr + (O)
Mn(OH)2 + (O) MnO(OH)2 
5. Action of Na2HPO4: Take the salt solution A white precipitate of manganous phosphate
in a test tube and add disodium hydrogen phos- is formed which is soluble in dilute acetic acid.
phate solution.
3 MnCI2 + 4Na2HPO4 Mn3(PO4)2  + NaH2PO4 +6NaCl
6. Action of PbO2 and HNO3: Take the salt Pink coloured solution is formed due to the
solution in a test tube and add a few drops of formation of permanganic acid (HMnO4)
conc.nitric acid and a pinch of solid lead per-
oxide. Boil and allow it to stand.
MnCl2 + 2HNO3 Mn(NO3)2 + 2HCl
Mn(NO3)2 + 5PbO2 + 6HNO3 2 HMnO4 + 5 Pb(NO3)2 +2H20
observed separately in oxidizing and reduc- Pinkish bead both in cold and hot conditions.
ing flames both in hot and cold conditions. Heating in luminous (reducing) flame:
Colourless both in cold and hot conditions.
Reactions of Cobalt ion (Co2+)
(With CoCl2.6H2O solution)
1. Action of heat: Take a small quantity of Pink salts like CoCI, 6H,O on heating loses
solid salt in a dry test tube and heat strongly. water of crystallization and changes to blue (or
purple) colour.
CoCl 2.6H2O CoCl2 + 6H2O
2. Action of NH4OH: Take a small quantity A pink coloured precipitate of Co(OH), is

of the salt solution in a test tube and add ex- formed which on boiling with water gives
cess of ammonium hydroxide. brownish black precipitate of Co(OH)3.
CoCl2 + 2 NH4OH Co (OH)2  + 2NH4CI

4Co(OH)2 + 2H2O + O2 4Co (OH)3 
3. Action of KNO2 and acetic acid: Take the An yellow precipitate of potassium cobalti ni-
salt solution in a test tube and add small trite is formed.
amount of acetic acid and few crystals of po-
tassium nitrite.
CoCl2 + 7KNO2 + 2CH3COOH K3[Co(NO2)6] + 2KCl + 2CH3COOK + NO +

H2O
4. Action of NH4Cl, NH4OH and H2S: Take A black precipitate of cobalt sulphide is
the salt solution in a test tube and saturate it formed, which is soluble in aqua regia.
the solution.
CoCl2 + 2 NH4OH Co(OH)2  + 2NH4Cl
Co(OH)2 + H2S CoS  + 2H2O
5. Action of ether and NH4CNS: Take the Blue colouration is obtained due to the forma-
salt solution in a test tube add a few drops tion of ammonium cobalti thiocyanate in ethe-
(about ImL) of ether and few crystals of am- real layer.
monium thiocyanate. Shake well and allow it
to settle.
CoCl2 + 4NH4CNS (NH4)2[Co(CNS)4] + 2NH4Cl
observed separately in oxidizing and reducing Deep blue both in hot and cold conditions.
Heating in luminous (reducing) flame: Deep
flames both in hot and cold conditions.
blue in both hot and cold conditions.
First Year 75
Reactions of Nickel ion (Ni2+)
(With 5% Nickel nitrate, Ni(NO3)2 solution)
1. Action of caustic soda: Take a small A green gelatinous precipitate of nickel hydroxide
quantity of salt solution in a test tube and add is formed which is insoluble in excess of the
sodium hydroxide solution. reagent.
Ni(NO3)2 + 2NaOH Ni(OH)2  + 2NaNO3
2. Action of NH4OH: Take a small quantity A green coloured precipitate of Ni(OH), is

of the salt solution in a test tube and add formed which dissolves in excess of
excess of ammonium hydroxide. ammonium hydroxide to form blue violet
nickel ammine complex.
Ni(NO3)2 + NH4OH Ni(OH)NO3 + NH4NO3
Ni(OH)NO3 + 7 NH3 + H2O [Ni(NH3)6] (OH)2 + NH4NO3
3. Action of NH,OH and dimethyl A bright red coloured precipitate is formed.

glyoxime: Take the salt solution in a test tube
and add ammonium hydroxide and a few drops
of dimethyl glyoxime (CH3CNOH)2 solution.
4. Action of NH4Cl, NH4OH and H2S: Take A black precipitate of nickel sulphide is
the salt solution in a test tube and saturate it formed, which is soluble in aqua regia.
with solid ammonium chloride and add
ammonium hydroxide and pass H 2S gas
through the solution.
Ni(NO3)2 + 2NH4OH Ni(OH)2 + 2 NH4NO3
Ni(OH)2 + H2S NiS + 2 H2O
5. Action of NaOH and Br2: Take the salt A green precipitate of Ni(OH)2 is formed which
solution in a test tube and add sodium hydroxide oxidises to a black precipitate of nickelic
solution in excess and bromine water and boil. hydroxide.
Ni(NO3)2 + 2NaOH Ni(OH)2  + 2NaNO3
Br2 + H2O 2HBr + (O)
2Ni(OH)2 + H2O + (O) 2Ni(OH)3
observed separately in oxidizing and reducing Brown when hot and pale brown when cold.
Heating in luminous (reducing) flame: Green
flames both in hot and cold conditions.
when hot and opaque when cold.

Reactions of Barium ion (Ba2+)
(With 1.8% BaCl2. 2H2O solution)
1. Action of Dilute H2SO 4: Take a small A white precipitate of barium sulphate is
quantity of the salt solution in a test tube formed which is insoluble in mineral acids.
and add dilute sulphuric acid.
Bacl2 + H2SO4 BaSO4  + 2HCI
2. Action of NH4Cl, NH4OH and (NH4)2Co3: A white precipitate of barium carbonate is

Take the salt solution in a test tube and formed which is soluble in hot acetic acid.
saturate it with solid ammonium chloride
and add ammonium hydroxide and
ammonium carbonate solution.
BaCl2 + (NH4)2CO3 BaCO3  + 2 NH4Cl

BaCO3 + 2CH3COOH (CH3COO)2 Ba + CO2 +H2O
3. Action of K2CrO4: Take the salt solution in An yellow precipitate of barium chromate is
a test tube and add potassium chromate formed which is soluble in dil. HCI.
solution.
BaCl2 + K2CrO4 BaCrO4  + 2KCl
4. Action of (NH 4) 2C 2O 4: Take the salt A white precipitate of barium oxalate is formed
solution in a test tube and add ammonium which is soluble in hot acetic acid and mineral
oxalate solution. acids.
BaCl2 + (NH4)2C2O4 BaC2O4  + 2NH4C1
5. Flame test : Clean the platinum wire by Light apple (grassy) green coloured flame is
dipping it in conc. HCl taken in a watch observed.
glass and heat the platinum wire strongly
in the same. Continue this process till the
wire imparts no colour to the flame.
Prepare a paste of the salt and conc. HCI in
a watch glass. Take some paste on the
platinum wire loop and introduce it into the
non-luminous flame of the burner. Note the
colour imparted to the flame.
First Year 77
Reactions of Calcium ion (Ca2+)
(With 3.7% Calcium chloride solution. CaCl2.2H2O)
1. Action of Dilute H2SO 4: Take a small A white precipitate of calcium sulphate is
quantity of the salt solution in a test tube formed which is insoluble in mineral acids.
CaCl2 + H2SO4 CaSO4  + 2HCI
2. Action of NH4CI, NH4OH and (NH4)2CO3: A white precipitate of barium carbonate is

Take the salt solution in a test tube and formed which is soluble in hot acetic acid.
saturate it with solid ammonium chloride
and add ammonium hydroxide and
CaCl2 + (NH4)2CO3 CaCO3  + 2 NH4Cl
CaCO3 + 2CH3COOH (CH3COO)2 Ca + CO2  + H2O
3. Action of K4 [Fe(CN)6) : Take the salt An white precipitate of calcium ammonium

solution in a test tube and saturate it with ferrocyanide is formed which is soluble in
solid NH 4C1 and add NH 4OH and dilute acids.
potassium ferrocyanide solution.
CaCl2+ 2NH4OH + K4 [Fe(CN)6] Ca(NH4)2[Fe(CN)6]  + 4KC1+2H2O
4. Action of (NH 4) 2C 2O 4: Take the salt, A white precipitate of calcium oxalate is

solution in a test tube and add ammonium formed which is soluble in mineral acids and
oxalate solution. insoluble in acetic acid.
CaCl2 + (NH4)2C2O4 CaC2O4  + 2NH4Cl
5. Flame test: Clean the platinum wire by Brick red coloured flame is observed.
dipping it in conc. HCl taken in a watch
in the flame. Continue this process till the

Reactions of Strontium ion (Sr2+)
(With Strontium nitrate, Sr(NO3)2 solution)
1. Action of dilute H 2SO 4: Take a small A white precipitate of strontium sulphate is
quantity of the salt solution in a test tube formed which is soluble in mineral acids.
Sr(NO3)2 + H2SO4 SrSO4  + 2HNO3
2. Action of NH4Cl, NH4OH and (NH4)2CO3: A white precipitate of strontium carbonate is

Take the salt solution in a test tube and satu- formed which is soluble in hot acetic acid.
rate it with solid ammonium chloride and
add ammonium hydroxide and ammonium
carbonate solution.
Sr(NO3)2 + (NH4)2CO3 SrCO3  + 2 NH4NO3
SrCO3 + 2CH3COOH (CH3COO)2Sr + CO2  +H2O
3. Action of (NH 4 ) 2SO 4 : Take the salt A white precipitate of strontium sulphate is
solution in a test tube and add ammonium formed which is soluble in mineral acids.
sulphate solution.
Sr(NO4)2 + (NH4)2SO4 SrSO4  + 2NH4NO3
4. Flame test: Clean the platinum wire by Crimson red coloured flame is observed.
dipping it in conc. HCl taken in a watch
in the flame. Continue this process till the
First Year 79
Reactions of Magnesium ion (Mg2+)
(With 10% Magnesium sulphate. MgSO4.7H2O Solution)
1. Action of Heat: Take a small quantity of Salts like MgCO3 decomposes on heating and
the salt solution in a dry test tube and heat liberates CO2 gas.
strongly.
MgCO3 MgO + CO2 
2. Action of NH4OH: Take the salt solution A white precipitate of magnesium hydroxide
in a test tube and add ammonium is formed (Note: Ammonium hydroxide only
hydroxide(NH4OH). partially precipitates Mg(OH)2
MgSO4 + 2NH4OH Mg(OH)2 + (NH4)2SO4
3. Action of Na2CO3: Take the salt solution in A white precipitate of basic magnesium
a test tube and add sodium carbonate carbonate is formed on boiling with water.
solution.
5MgSO4 + 5Na2CO3 + 6 H2O Mg(OH)2. 4MgCO3. 5H2O + 5Na2SO4 + O2
4. Action of NaOH : Take the salt solution in A white precipitate of magnesium hydroxide
a test tube and add sodium hydroxide is formed which is insoluble in excess of the
(NaOH) solution. reagent.
MgSO4 + 2NaOH Mg(OH)2  + Na2SO4
5. Action of NH4C1, NH4OH and Na2HPO4: A white crystalline precipitate of magnesium

Take the salt solution in a test tube and ammonium phosphate is formed which is
saturate it with solid ammonium chloride and soluble in mineral acids and acetic acid.
add ammonium hydroxide and disodium
hydrogen phosphate solution. The sides of
the test tube are scratched with a glass rod.
MgSO4 + Na2HPO4 +NH4OH Mg(NH4) PO4 + Na2SO4 + H2O
6. Charcoal test/ Cobalt nitrate test : A white residue of MgO is left behind and on
Perform charcoal cavity test. If the residue performing cobalt nitrate test and heating hot pink
is white, then carry out cobalt nitrate test. mass of the double salt MgO.CoO is obtained.
MgO + CoO MgO.CoO
(Pink)
Reactions of Ammonium ion (NH4+)
(With 3% Ammonium chloride solution (NH4Cl))
1. Action of Heat: Take a small quantity of Salts like NH4Cl undergo sublimation and a
the salt solution in a dry test tube and heat white sublimate is formed on the sides of the
strongly. test tube.
NH4Cl(s) NH4Cl(g)  NH4Cl(s)
White
sublimate
2. Action of NaOH : Take the salt in a test Colourless gas of ammonia with pungent smell
tube and add sodium hydroxide(NaOH) so- is evolved, which produces dense white fumes
lution and heat. with a glass rod dipped in Con.HCl.
NH4Cl + NaOH NaCl + NH3 + H2O
NH3 + HCl NH4Cl(g)
3. Action of Nessler's reagent: To the salt A reddish brown precipitate or colouration is

solution Nessler's reagent (K2[HgI4]) is obtained which is called 'lodide of million's
added. base'.
2 K2[HgI4]+ NH3 + 3KOH H2N.HgO.Hg I + 7KI + 2H20
4. Action of Picric acid: To the salt solution An yellow precipitate of ammonium picrate is
of picric acid (2,4,6 Trinitro phenol) is formed.
added and the inner sides of the test tube is
scratched with a glass rod.
NH4Cl + C6H2(NO2)3OH C6H2(NO2)3ONH4  + HCI
=
5. Action of Tartaric acid: To the salt, solution A white crystalline precipitate of ammonium
tartaric acid is added. tartarate is formed.
2 NH4Cl + H2C4H4O6 (NH4)2C4H4O6  + 2HCI
First Year 81
CHAPTER - 8
DETECTION OF ELEMENTS IN
ORGANIC COMPOUNDS
8.1 Introduction
Detection of elements present in organic compound constitutes an important step in its
analysis. All the organic compounds contain carbon and hydrogen. In addition to these elements. other
elements like oxygen, nitrogen, sulphur and halogens are generally present in organic compounds.
Since almost all organic compounds contain carbon and hydrogen, it is not necessary to carry out the
tests to detect them and their presence can be assumed without testing for them. Therefore, we shall
study the tests for the detection of nitrogen, sulphur and halogens only.
Theory
The elements nitrogen, sulphur and halogens present in an organic compound are detected by
Lassaigne's test. The elements bound by covalent bonds in the original organic compound are
converted into the ionic form compounds by fusing the compound with sodium metal. Nitrogen,
sulphur and halogens present in the organic compound are converted into cyanide, sulphide and
halides repectively. The following reactions takes place.
Na + C + N NaCN
2Na + S Na2S
Na + X NaX (X = Cl, Br, I).
The cyanides, sulphides and halides so formed are extracted from the fused mass by boiling it
with distilled water. This is filtered and the filtrate is known as Lassaigne's extract (or sodium fusion
extract).
8.2 Detection of Nitrogen, Sulphur by Lassaigne's Test
Lassaigne's test is also known as sodium fusion test. To do this test first of all Lassaigne's
extract (or sodium fusion extract) is to be prepared.
Preparation of Lassaigne's extract: A small quantity of the organic compound is fused with
small quantity of sodium metal in a fusion tube. The red hot fusion tube is then plunged into a china
dish containing distilled water. Crush the content with a glass rod and heat to boiling. Then cooled and
filtered. The filtrate is called Lassaigne's extract (or sodium fusion extract) and is usually alkaline.
This extract is used to detect the elements nitrogen, sulphur and halogens.

Sodium
compound Holder
(a) Heating sodium and compound (b) Plunging ignition tube in distilled water
Lassaigne’s
extract
(c) Boiling the content (d) Filtering to get extract
Fig. 8.1: Preparation of Lassaigne's extract
Detection of Nitrogen: To a small portion of Lassaigne's extract 2 mL of freshly prepared

ferrous sulphate solution is added and warmed. Then about 2-3 drops of ferric chloride solution is
added and acidified with conc.HCl, appearance of Prussian blue colour confirms the presence of
nitrogen.
Chemistry of the test: The nitrogen present in the organic compound is in the form of sodium
cyanide (NaCN) which is formed during fusion. Sodium cyanide first reacts with ferrous sulphate and
forms sodium hexa cyano ferrate(II), which reacts with FeCl, (acidified with conc.HCI) to form ferric
ferrocyanide (iron(III) hexacyanoferrate(II)) which has Prussian blue colour.
Na + C + N  NaCN
FeSO4 + 2NaOH  Fe(OH)2  + Na2SO4
Fe(OH)2 + 2NaCN  Fe(CN)2 + 2 NaOH
Fe(CN)2 + 4NaCN  Na4[Fe(CN)6]
3Na4[Fe(CN)6] + 4FeCl3  Fe4[Fe(CN)6]3 + 12 NaCl
Note: The purpose of acidifying the reaction mixture in the end is to dissolve any green precipitate
of Fe(OH)2 since it may interfere with Prussian blue colour.
First Year 83
Nitrogen and Sulphur present together: If the organic compound contains both nitrogen and
sulphur, sodium sulphocyanide (NaCNS) is formed during the preparation of Lassaigne's extract.
Sodium sulphocyanide react with ferric chloride and gives deep blood red colouration due to the
formation of ferric sulphocyanide.
Na + C +N+S NaCNS
From organic
compound
3NaCNS + FeCl3 Fe(CNS)3 + 3Nacl
blood red
colouration
Thus, appearance of blood red colouration on performing Lassaigne's test for nitrogen
indicates the presence of both nitrogen and sulphur in the organic compound.
Detection of Sulphur : The presence of sulphur in organic compound is detected by the following
tests.
1. Sodium Nitroprusside test: To a small portion of Lassaigne's extract add a few drops of sodium
nitroprusside solution. A purple colouration indicates the presence of sulphur in the organic
compound.
Chemistry of the test: During the preparation of Lassaigne's extract, sulphur from the organic
compound combines with sodium to form sodium sulphide.
2Na + S Na2S
(from organic
compound)
Na2S + Na2[Fe(CN)6NO] Na4[Fe(CN)6NOS]
(From sodium (Sodium (Purple colouration)
extract) nitroprusside)
2. Lead acetate test: To a small portion of Lassaigne's extract add acetic acid and a few drops of lead
acetate solution. The formation of black ppt. indicates the presence of sulphur in the organic
compound.
Na2S + (CH3COO)2Pb PbS  + 2CH3COONa
8.3 Detection of Halogens by Lassaigne's Test
1. Silver nitrate test: To 2 mL of Lassaigne's extract add 1 mL of conc.nitric acid and-boil for
sometime. Cool the contents and then add silver nitrate solution.
(i) Formation of white precipitate soluble in ammonium hydroxide indicates the presence
of chlorine in the organic compound.
Heat
Na + Cl NaCl
NaCl + AgNO3 AgCl + NaNO3

White ppt
(Silver Chloride)
AgCl + 2NH4OH [Ag(NH3)2]C1 + 2H2O

(ii) Formation of pale yellow precipitate, sparingly soluble in ammonium hydroxide indicates the
presence of bromine in the organic compound.
Na + Br NaBr
NaBr + AgNO3 AgBr  + NaNO3
Pale yellow ppt
(Silver bromide)
(iii) Formation of yellow precipitate insoluble in ammoniumhydroxide indicates the presence of

iodine in the organic compound.
Heat
Na + I NaI
NaI + AgNO3 AgI  + NaNO3
Yellow ppt
(Silver iodide)
Note: Addition of conc.HNO, and boiling is to decompose traces of sodium cyanide or sodium
sulphide present in the extract, or else these compounds will interfere with the tests for halides as
sodium cyanide gives white ppt. with silver nitrate solution, while sodium cyanide gives black
precipitate with silver nitrate solution.
2. Carbon disulphide test (for detection of bromine and iodine)

Acidify a small portion of Lassaigne's extract with dil.HCl and add a few drops of carbon
disulphide (or CCI4). To this add freshly prepared chlorine water and shake vigorously.
(i) Appearance of orange colour in the carbon disulphide layer indicates the presence of
bromine in the organic compound.
2NaBr + Cl2 Br2 + 2NaC1

(From sodium extract)
(ii) Appearance of violet colour in the carbon disulphide layer indicates the presence of
iodine in the organic compound.
2NaI + Cl2 12 + NaC1
(From sodium extract)
Table 8.1: Summary sheet of Lassaigne's test
Experiment Observation Inference
1. Test for nitrogen (i) Prussian blue colour is Nirogen is confirmed.

To small portion (about 2 mL) observed.
of lassaigne’s extract add 2 mL Both nitrogen and sulphur
of freshly prepared ferrous (ii) Blood red colouration are confirmed.
sulphate solution and boil. Then is observed.
add a few drops of ferric
chloride solution and conc.HCl
First Year 85
2. Test for sulphur A purple colouration is ob- Sulphur is confirmed.
(i) To 2 mL of Lassaigne’s extract served.
add a few drops of sodium
nitroprusside solution.
(ii) To 2 mL of Lassaigne’s extract A black precipitate is formed. Sulphur is confirmed.
and a few drops of acetic acid
and 1 mL of lead acetate
solution.
3. Test for halogens (i) A curdy white precipitate is Chloride is present, hence
Acidify a little of Lassaigne’s formed which soluble in chlorine is confirmed.
extract with conc.HNO3 boil, excess of NH4OH.
cool and add silver nitrate (ii) A pale yellow precipitate is Bromide is present, hence
solution. formed which is sparingly bromine is confirmed.
soluble in NH4OH.
(iii) A bright yellow precipitate Iodide is present, hence
is formed which is insoluble iodine is confirmed.
NH4OH.

1. Can we use potassium in place of sodium in Lassaigne’s test?
2. Why freshly prepared FeSO4 solution is used to detect nitrogen?
3. Why dil.HCl is added in the test for nitrogen?
4. Why sodium extract is alkaline in nature?
5. What is the oxidation state of the central atom Fe in Fe4[Fe(CN)6]3 ?
6. What is the function of addition of conc.HNO3 and boiling in the detection ofhalogens by
Lassaigne’s test?
7. What is the Prussian blue colour due to in the Lassaigne’s test for nitrogen?
8. Why chlorine water is used to test for bromine and iodine?
9. How can you test the presence of both nitrogen and sulphur by Lassaigne’s test?

PROJECTS
INTRODUCTION
The science and the scientific knowledge has been widely expanded to meet technological
necessities. This gave rise to the change in the system of education and in the methods of instruction.
These days there is a marked change, which lay stress on inquiry rather than traditional class room
teaching methods. Moreover, the development of the technology mandates the learning of practical
skills rather than the study of pure science. This requires an individual approach of a learner and self
inquiry of the things. In this direction, a new dimension in the teaching of science has been added by
including the project-work at the intermediate level. The project work is an individualised
instructional technique. It provides an opportunity to the student to approach to a problem, to plan his/
her work, to search appropriate resources, to carry out his/her plans, and to draw conclusions. This
gives an opportunity to a student to interact with scientific principles and to gain hands on skills. The
project work imparts great awareness about scientific thinking and scientific methods of analysis.
To help the scientific curiosity and to stimulate interest in science and to have a first hand
knowledge about carrying out project work, some investigatory projects have been given which serves
as model projects. Some of the projects involve theoretical work and collection of data from the
books. Other projects involve experimental work, using chemicals and apparatus and are to be carried
out in a laboratory. Apart from the projects given in the book, a student can take up his own project in
consultation with his/her teacher.
Working on project involves the title of project, objectives and importance of project, theory
and background of the project and a brief outline of work on project (procedural process). The projects
are included such that as far as possible, the material (apparatus, instruments, chemicals etc.,) needed
for the project-work is easily available. The project work done by a student is to be recorded in a
Project Record and submitted to the teacher for assessment. Recording the project work should
involve, title of project reflecting objectives, principles used for investigation, apparatus and
chemicals required, procedure, observations and calculations, conclusions and precautions.
PROJECT-1
Title : Study of the methods of purification of water
Objectives
1. To study the level of purity achieved by using different purification methods.
2. To study the advantages and disadvantages of using different purification methods.
3. To know the specific uses of pure water.
Background
Water is essential for all living beings. As such the water should be available in pure form.
Otherwise, the impure water causes many disadvantages like spreading of water borne
First Year 87
diseases, water infections etc., The water is available for us by so many sources like rivers, wells, seas,
rains etc., Depending on the nature of source and degree of contamination, water is purified by the
following methods.
Water purification methods
There are various methods of water purification. Some of them are
1. Storage 2. Coagulation and Sedimentation 3. Filtration 4. Disinfection (using chlorine gas
and sodium hypochlorite and ozone) 5. Boiling 6. Distillation 7. Carbon filtering 8. Reverse osmosis
9. Ion exchange and 10. Electrode ionisation.
Let us discuss the distillation method of purification of water, which gives 99.9% pure water.
Distillation
The process of distillation involves the evaporation and condensation, which helps to purify
water. The key terms are evaporation and condensation. Evaporation is defined as the process through
which a liquid becomes a vapour. Condensation is the process through which a vapour becomes a
liquid, and is the opposite of evaporation. In the case of water, the main mechanisms for evaporation
and condensation are heating and cooling, respectively which is known as distillation.
In this process of distillation, there are different types like steam distillation, fractional
distillation etc., In distillation process, the impure water is taken and it is subjected to evaporation. The
water vapour or steam is collected in a container and is cooled to room temperature (condensation).
The steam which is free from almost all the impurities, upon cooling gives pure water. Distillation
process is helpful to remove impurities like micro biological organisms, organic and inorganic
impurities, heavy metals and radio active substances. The following table gives the comparison of
various water purification methods.
Table P 1.1: Water purification process performance comparison

Type of Carbon Carbon Ceramic Ceramic Reverse Steam
filter with filter with distillation
Microbiological NO PARTIAL YES YES NO YES
Organics YES YES NO YES YES YES
Heavy metals NO NO NO NO PAR- YES
Radio active NO NO NO NO PAR- YES
Inorganics NO NO NO NO PAR- YES
Conclusion: The most inclusive water purification Method is steam distillation

PROJECT- 2
Title : Investigation of the foaming capacity of different washing soaps and the effect of
addition of sodium carbonate on the foaming capacity of a soap.
Objective: To study the foaming capacity of different samples of washing soaps and to study
the effect of addition of sodium carbonate on the foaming capacity of different soaps.
Requirements
Different samples of soaps, distilled water, boiling tubes with corks, measuring cylinder (100
mL), weight box, Na2CO3.
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 0.5 g 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.
Observations
Table P 2.1: Comparison of foaming capacity of different samples of soaps
Height of the boiling tube upto Height of the boiling
Boiling Brand name
which the foam appears/rises tube upto which the foam
tube No. of the soap
(with out Na2CO3) appears/rises (with Na2CO3)
1. A cm cm
2. B cm cm
3. C cm cm
4. D cm cm
Conclusions
1. The greater the height of the boiling tube upto which the foam appears/rises, greater is the
foaming capacity of the soap. As the height of the boiling tube upto which the foam appears/
rises of the sample of the soap of the brand maximum among the samples taken, this sample
has maximum foaming capacity.
2. Calcium and magnesium salts present in water decreases the foaming capacity of soap. But,
when Na2CO3 is added, the Ca and Mg are replaced by sodium, and hence the foaming capac-
ity increases by the addition of Na2CO3.
It is observed that the foaming capacity of all samples of soap increased on addition of Na2CO3.
First Year 89
PROJECT- 3
Title : Study of the acidity of different samples of tea leaves
Objective : To estimate the concentration of acids present in different tea samples and effect
of addition of acids and bases on the colour of tea extract.
Requirements
Beakers, conical flasks, funnel, burner, various samples of tea leaves, 0.02 M NaOH solution,
phenolphthalein
Procedure
Weigh 10 g of the sample of the tea leaves and prepare the extract of each sample separately in
200 mL of distilled water by boiling and then filter.
Take 5 mL of tea extract in a conical flask and dilute it to 20 mL with distilled water. Titrate this
solution against 0.02 M NaOH solution using phenolphthalein indicator. Repeat this process with
different samples. Calculate the concentration of acid present in different tea samples in terms of
molarity. The colour change at the end point is from pink to colourless. If colour of the tea extract
causes any problem, it can be taken in the burette and NaOH solution in the conical flask.
Table P 3.1: Titration of tea extract Vs NaOH solution
Burette readings Volume[1/2mL] of
Sample Volume of tea
NaOH
Initial Final
1. 20 mL X1 mL
2. 20 mL X2 mL
3. 20 mL X3 mL
4. 20 mL X4 mL
5. 20 mL X5 mL
For sample 1
Calculations: Volume of tea extract = V1 Volume of NaOH = V2 = X1mL
Molarity of tea extract = M1 Molarity of NaOH = M2
No. of moles of tea extract = n1 No.of moles of NaOH = n2
V1M1 V2 M 2
We know that 
n1 n2
V2  M 2  n1
Molarity of acid present in tea sample (M1 )  V1  n 2
molL-1
Similarly, calculate the molarity of acid present in extracts of different tea samples and
compare the molarities of acids present in different tea samples.

PROJECT - 4
Title : Study of the rates of evaporation of different liquids
Objective: To study the relationship between the rates of evaporation of different liquids and
their chemical constitution.
Requirements
Weighing bottles, pipettes (10 mL), stop watch, analytical balance and weight box
Procedure
Clean and dry the weighing bottles and mark them as A,B,C,D. Weigh the bottles separately
with stoppers. Now pour 10 mL each of the liquids ethanol, ether, acetone and CCl4 respectively in
different weighing bottles. Weigh each of the bottle with stopper and record their weights (W1). Now
remove the stoppers from all the bottles and keep them at room temperature for 30 minutes now cover
the bottles with stoppers and weigh each of the bottle separately. Record the weight of each of the
bottle (W2) Calculate the loss of mass of each liquid (W1-W2). See that the temperature and surface
area should be the same for evoparation of each liquid. Determine the rate of evaporation of each
liquid in grams per second. Relate the dillerence in the rates or evaporation of liquids with their chemi-
cal constitution and variation in intermolecular/intramolecular interactions. Record your observations
in the table.
Table P 4.1: Rates of evaporation of different liquids
Weighing Liquid taken Initial weight Final weight of Weight of the liquid Rate of
bottle of the bottle + the bottle + evaporated (W -W ) evaporation
liquid (W1) liquid (W2) 1 2 (W1-W2/1800)gs-1
A Ethanol
B Ether
C Acetone
D CC14
Result and conclusion

1. The rates of evaporation of the given liquids is in the order ------
2. The liquid having weaker intermolecular forces has greater rate of evaporation.
PROJECT-5
Title : Study of the effect of acids and alkalies on the tensile strength of fibrers
Objective: To find the effect of acids and alkalies on tensile strength of different fibres like
cotton, wool and silk.
Requirements
Hook, weight hanger, weights, cotton, wool, silk fibres, NaOH solution and HCl
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. Cut out equal thickness and lengths of cotton, wool and silk
threads from given samples. Take a thread and tie its one end to hook and other end to weight hanger.
Start adding weights to the weight hanger gradually until the breaking point is reached. Note the
minimum weight required to break the fibre. Repeat the experiment with different fibres. Record the
observations. These weights are the measure of the tensile strength of the fibre.
First Year 91
The effect of acids and alkalies on the tensile strength of fibres can be determine by dipping
them separately in dil.HCl or in NaOH solution of equal strengths and for equal duration of time. Then
the fibres are removed from the solution, washed with water and dried. Now, determine the tensile
strength of each fibre separately as done earlier. Interpret the observations in terms of chemical
constitution of the material of the fibre.
Conclusions
1. The tensile strength of cotton fibre found to be decreased by acids and unaffected by alkalies.
2. The tensile strength of woolen fibre is found to be unaffected by acids and decreased by alkalies.
3. The tensile strength of nylon fibre is found to be practically unaffected by both acids. and alka-
lies.
PROJECT-6
Title : Analysis of fruit and vegetable juices for their acidity
Objective: To determine the amount of acids present in various fruits and vegetables and also to
detect the presence of iron, carbohydrates, proteins and sugars in them.
Requirements
Test tubes, burner, litmus paper, laboratory reagents, juices of various fruits and vegetables
Theory
Fruits and vegetables are always a part of balanced diet. That means the fruits and vegetables
provide our body the essential nutrients like carbohydrates, proteins, vitamins and minerals. Their
presence in these substances can be indicated by some general observations. For example, freshly cut
apple becomes reddish after some time because iron present in apple gets oxidized to iron oxide.
However, the presence of carbohydrates, proteins. sugars and acids can be tested in the laboratory by
extracting their juices and subjecting them to various tests.
Procedure
(a) Acid content: Take different fruit juices in different containers and dip the pH paper in them.
If pH is less than 7, it is acidic. Determine their acid content by titrating a known quantity of a
fruit juice with 0.01 M KOH solution using phenolphthalein as 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. The acid value of
vegetables and fruits is the number of milligrams of KOH required for neutralising acid present
in one gram of vegetable or fruit.
(b) Test for iron: Take 2 mL of juice and add a drop of conc.nitric acid. Boil the solution. cool and
add 2-3 drops of potassium sulphocyanide solution. Appearance of blood red colouration indi-
cates the presence of iron.
(c) Test for carbohydrates: Take 2 mL of juice and add 1 mL of Fehling's solutions A & B and
boil it. Red precipitate indicates the presence of reducing sugars like maltose, glucose, fruc-
tose and lactose.
(d) Test for starch: Take 2 mL of juice in a test tube and add a few drops of iodine solution. If it
turns blue black in colour, it indicates the presence of starch.
(e) Test for calcium: Take 2 mL of juice in a test tube and add a few drops of ammonium chloride
and ammonium hydroxide solutions. Filter the solution and add 2 mL of ammonium oxalate
solution. White precipitate or milkiness indicates the presence of calcium.

.
CHAPTER-1
SURFACE CHEMISTRY
If the particles of a substance are dispersed in other substance (medium) in such a way that the
dispersed particles are very small in size with diameter ranging between lnm and 100 nm in the
medium, the dispersed substance is said to be in the colloidal state. The colloidal solution is a
heterogeneous.
In a true solution, which is homogeneous, the dispersed particles have diameters between 0.2
and 1.0 nm. If the dispersed particle have diameter 100 nm and above, such solutions are called
suspensions and they settledown on standing.
The substance dispersed in the colloidal state in other substance is called the dispersed phase
and the other substance (medium) is called the dispersion medium.
Substances like egg albumin, starch, gelatin, glue readily pass into colloidal solution on
heating with suitable liquids. These are known as intrinsic colloids and the so obtained colloidal
solution is called lyophilic (solvent loving) sols. If the liquid is water, the intrinsic colloids in water
are called hydrophilic sols. In these sols the colloidal particles are themselves big molecules known as
macro molecules with molecular masses ranging from thousands to millions.
Substances which require special methods to go into colloidal state in the given medium, thus
differ from intrinsic colloids, are called extrinsic colloids and also as lyophobic (solvent hating) sols.
If extrinsic sols in water, they are called hydrophobic sols. A freshly prepared ferric hydroxide,
aluminium hydroxide and arsenic sulphide are some examples for lyophobic sols.
Stability of lyophilic and lyophobic sols
In lyophilic sols dispersed phase particles have greater affinity for the particles of the
dispersion medium. Due to this lyophilic sols are more stable. More the solvation of colloidal par-
ticles, more is the stability of the sols. The stability of the lyophobic sols is due to the charge present
on the colloidal particles. The same type of charges on colloidal particles makes them repelled from
one another and prevent them from coagulation. Starch and arsenious sulphide are negatively charged.
If FeCl3 is added to excess of boiling water, a positively charged hydrated ferric oxide sol is formed. But if
Fecl3, is added to NaOH solution a negatively charged hydrated ferric oxide sol is formed.
Preparation of colloids
Chemical methods, electrical methods and peptisation are some of the methods used to prepare the
colloidal solutions.
Experiment : 1.1
Preparation of Some (a) Lyophilic Sols and (b) Lyophobic Sols
Aim: To prepare some (a) lyophilic sols and (b) lyophobic sols.
Theory
Lyophilic sols are directly prepared by adding and shaking the substances that form dispersed phases
with suitable liquids that form dispersion media. Here, attraction between dispersed particles and dispersion
medium are responsible for the stability of colloidal state. Lyophobic sols are not obtained by simple mixing
and shaking of the substances that form the dispersed phase and the dispersion medium. Special
methods are adopted for the preparation of lyophobic sols.
Sols to be prepared
Lyophilic sols: egg albumin sol, starch sol and gum sol. Lyophobic sols: Ferric hydroxide sol, alu-
minium hydroxide sol and arsenious sulphide sol.
Beakers (250 mL), watch glass, porcelain dish, measuring jar (100 mL), pipette (10 mL), graduated
pipette (20 mL), starch (500 mg), gum (500 mg), egg (1), sodium chloride (5 g), aluminium chloride (2 g), ferric
chloride (2 g) and arsenious oxide (0.2 g).
Procedure
(A) Preparation of lyophilic sols
1. Preparation of starch sol: Take 100 mL of distilled water using measuring jar and transfer it to a
250 mL beaker. Heat the beaker until the distilled water in it boils. Make a paste of starch with 500 mg
of it in water. Transfer this starch paste slowly to boiling water in the beaker with constant stirring.
Continue the stirring and boiling of water for atleast 10 minutes after adding the starch paste. Thus the
starch sol is formed.
Note: The gum sol also is prepared by the same procedure with 500 mg of guminstead.. of 500 mg
of starch.
2. Preparation of egg albumin sol
(i) Take 5 g of sodium chloride in a 250 mL beaker and add to it 100 mL of distilled water using a
measuring jar. Prepare a clear solution by dissolving NaCl in distilled water.
(ii) Break an egg into a porcelain dish. Pipette out the albumin into the above sodium
chloride solution while stirring thoroughly. Egg albumin sol is formed.
(B) Preparation of lyophobic sols
1. Preparation of ferric hydroxide sol
(i) Take 100 mL of distilled water in a 250 mL beaker using 100 mL measuring jar and boil the water.
Add 2 g of ferric chloride powder to this boiling water while stirring well.
(ii) Take another 100 mL of distilled water into another 250 mL beaker and boil it.
(iii)Takel0 mL of ferric chloride solution prepared in step (i) and add it to boiling water prepared
instep (ii) drop by drop with vigorous constant stirring. Keep the water boiling. A brown ferric
hydroxide (Fe(OH)3 sol is formed.
Note: Adopt same procedure to prepare Al(OH)3 sol as given for the preparation of Fe(OH)3 sol. Al(OH)3
sol is white in colour.
2. Preparation of arsenious sulphide sol
(i) Take 100 mL of distilled water with a 100 mL measuring jar and transfer it to a 250 mL glass beaker.
Add 0.2 g of arsenious oxide to it. Heat the beaker with distilled water and arsenious oxide till the
solution boils.
(ii) Cool the beaker and its contents. Filter the solution
(iii) Pass hydrogen sulphide (H2S) gas through the above filtrate till it gives the smell of H2S. Expel
excess H2S by slow heating and filter it. The filtrate is As2, S3, arsenious sulphide sol.
Note
1. Avoid addition of the excess amount of the solute whose sol is to be prepared as the excess of solute
may form precipitate.
2. As As2, O3, is poisonous, handle it with care. Wash the hands immediately after using it.
3. All glass apparatus used for lyophobic sols should be ion-free to prevent coagulation. It must be
washed with distilled water several times.
Experiment : 1.2
Purification of a Sol by Dialysis
Aim: To purify the prepared sol by dialysis.
Principle
Colloidal particles being relatively bigger in size, they get retained by porous membrane like parchment
or cellophane bag, while ionic and other soluble impurities pass through the bag into water in a trough. This
process of purification of a sol is called dialysis. The apparatus in which the dialysis is carried is called a
dialyser.
Parchment / cellophane paper - 1 sheet (30 cm x 30 cm)
Glass trough -1 Colloidal dispersion of any one prepared in expt 1.1.
Wide bore glass tube - 1 (say egg albumin sol)
(if available) Distilled water
Thread Uranyl zinc acetate solution
Test tubes - 2 Silver nitrate solution
Procedure
(i) Take a square sheet (30 cm x 30 cm) of parchment or cellophane paper,
soak it in water and give it a conical shape. Tie the mouth of the bag around
a sleeve of wide bore glass tube by means of a string. Fill the bag with the
sol to be dialysed.
Suspend the bag in the trough containing distilled water. If the glass tube is
not available tie the cone with the thread and suspend it as shown in figure
1.1.
(ii) Change the water in the trough every half an hour till it is free from impurities
of Na+ and Cl-. To test these ions, take the water from trough into two test tubes. Fig. 1.1: Purification of
To one test tube add uranyl zinc acetate solution and to the a sol by dialysis
Second Year 95
other AgNO3 solution. An yellow precipitate with uranyl zinc acetate indicates the presence of Nat and
a white precipitate with AgNO3 solution shows the presence of Cl-. If Na+ and Cl- are not there in trough
water, the egg albumin is pure. Different sols take different timings for the purification.
Note: (i) Water from the trough should not enter into parchment bag. For this, the mouth of the bag
should be above the water surface.
(ii) Water should be changed from the trough from time to time.
Experiment : 1.3
Role of Emulsifying Agents in Stabilizing the Emulsions of Different Oils
Aim : To study the role of emulsifying agents in stabilizing the emulsions of different oils
Principle
The dispersed phase which is in small proportion as well as the dispersion medium which is in
large proportion, if both are liquids, the resulting sol is called an emulsion. When oil is shaken with
relatively more amount of water, a faint milky solution is formed. It is unstable. It is called emulsion
of oil in water. If it is allowed to settle, it gets separated into two layers i.e., oil and water. The mixing
capacity of different oils with water would be different. The mixing of an oil in water depends on the
(i) nature of the oil (ii) type of mixing like shaking (or) swirling
Emulsifying agent
The stability of an emulsion can be increased by adding a substance known as emulsifying agent
to the emulsion. For example, aqueous solution of soap. Soap contains sodium salt of long chain
aliphatic carboxylic acid like oleic acid with non polar hydrocarbon chain and polar carboxylic acid
group. Carboxylate group decreases the inter facial surface tension between oil and water. This makes
oil and water to mix easily to form an emulsion. Hence, soap is an emulsifying agent or emulsifier.
The concentration of soap required for complete emulsification is called optimum concentration. Any
amount less or more than this optimum amount does not cause an effective stabilization. With
optimum concentration of emulsifying agent oil in water emulsion is more stable. It takes more time
for oil in water emulsion to get separated into two layers in the presence of emulsifying agent.
Procedure
(i). Dissolve 1 g of soap or detergent in 10 mL of distilled water in a test tube with vigorous
shaking and heating, if necessary. Label the test tube as 'A'.
(ii) Take four test tubes and label them as B, C, D and E. Put 5 mL of distilled water in each test
tube. Add 10 drops of mustered oil into test tube B, 10 drops of linseed oil to test tube C;
castor oil to test tube D and machine oil to test tube E.
(iii) Shake the test tube B for five minutes vigorously. Keep it in a test tube stand and start a stop
watch simultaneously. Note the time required to get the two layers separated.
(iv). Repeat exactly the same procedure as done in (iii) with the test tube B, with other test tubes
C, D and E and note the time taken for the two layers to get separated.
(v) Now, add two drops of soap or detergent solution from A to each of the test tubes B, C, D and E.
Shake the four test tubes vigorously for five minutes each and allow

them to settle. Note the time taken for two liquids to get separated into two layers. Record your
observations as follows.
Table 1.1: Emulsification of different oils in water by soap or detergent
Test tubes with Name of the oil used Time taken for the separation of two layers
different oils and for emulsification Without soap or With soap or
water detergent detergent
A
B
C
D
E
Precautions
1. Add equal number of drops of soap or detergent solutions to all the test tubes.
2. Shake all the test tubes for identical time spans.
3. Start the stop watch immediately after shaking is stopped and stop it immediately after the two
layers separate.
1. Distinguish among true solution, colloidal solution and suspension.
2. Mention the sols that you come across in your daily life and their importance.
3. Fe(OH)3 / Al(OH)3 sol is positively charged but As2, S3, sol is negatively charged. Why? How is
the charge developed on colloidal particles?
4. Explain coagulation and peptisation. How are they different?
5. How is a colloidal dispersion of sulphur converted into a true solution?
6. Differentiate between a gel and a sol. Which is easier to convert, a lyophilic sol to a gel or a
lyophobic sol to a gel? Why?
7. Mention the applications of colloidal dispersions in medicine, defence and rocket technology.
8. How can the dialysis be made fast?. Give the limitations of that technique?
9. Emulsifying agent in the oil in water type of emulsion other than soap is _______
10. The emulsifier that stabilizes milk is______________
11. The miscible liquids form an emulsion. Yes / No.
12. The reason for different timings for the separation of layers of different layers forming an emul-
sion with water is
13. What are the similarities and dissimilarities among sol, emulsion and gel?
14. A test to distinguish between oil in water and water in oil type emulsion is _________
15. Mention emulsions you observe in daily life. Dettol – water emulsion is stabilized by—

Second Year 97
CHAPTER-2
CHEMICAL KINETICS
Experiment: 2.1
Effects of Concentration and Temperature on the Rates of Reaction - A Practical Study
of the Rate of Reaction Between Sodium Thiosulphate and Hydrochloric Acid.
Aim: To study the effects of concentration and temperature on the rate of the reaction between sodium
thiosulphate and hydrochloric acid.
Theory
As per collision theory that was developed by Max trantz and W.Leuis (1916-18), a chemical
reaction takes place due to the collisions between the hard spherical reactant molecules. The number of
collisions per second per unit volume of the reactants is known as the collision frequency denoted by 'Z'.
The factors which influence the rate of reaction are the collision frequency and also the activation energy
denoted by E2.
For the reaction A + B  products
Rate = ZAB e-Ea/RT
ZAB is the collision frequency of reactants A and B.
Ea = activation energy; T = Temperature in Kelvin scale
R = universal gas constant
Activation energy is the minimum excess of energy than the average energy of reactant
molecules that should be possessed by the reactant molecules to form the intermediate known as
activated complex during this collision. Those collisions which result in the formation of the activated
complex are called fruitiful collisions.
Effect of concentration on the reaction rate: If the concentration of reactant molecules
increases, the number of molecules per unit volume increases and collisions between them per second
automatically increase. Therefore with the increase in the concentration of reactants the rate of the
reaction increases.
Effect of temperature on the reaction rate: If the temperature of the reactant molecule
increases, the kinetic energies of reactant molecules increase. At high temperature, therefore the
collision frequency increases and the reactant molecules possessing energy required to form the
activated complex increase. Hence the rate of the reaction increase with the increase of temperature.
Sodium thiosulphate reacts with hydrochloric acid and forms colloidal sulphur. Due to this the
solution is translucent.
The reaction is S2032- (aq) + 2H+(aq)  H20(1) + S02(q) + S(s)or
Na2S203 (aq) + 2HCl(aq) 2NaCI(aq)+H20(1) +S02(g) +S(s)

The property of the colloidal solution of sulphur to make the reaction system translucent is
used to study the rate of the reaction. Increase of the concentration and increase of the temperature of
the reactants both increase the rate of formation of colloidal sulphur. This is due to increase in the
collision frequency and the increase of kinetic energy of reactant molecules.
Conical flask (100 mL), burette (50 mL), pipette (25 mL), stop watch, thermometer, burette stand,
water bath, 0.1 M sodium thiosulphate solution and 1.0 M hydrochloric acid
Procedure
Part A
Study of the effect of concentration on the rate of the reaction of Na2S2O3 with HCl
1. Take a water trough filled to 1/2 of its volume. It can be used as a constant temperature bath at room
temperature.
2. Wash and rinse the burette. Fill it upto zero mark with 1.0 M HCl solution without any air bubbles
even in the nozzle.
3. Take a 100 mL conical flask. Make a notable mark say 'X' at its bottom outer surface. Add 50 mL
of 0.1 M sodium thiosulphate solution to the conical flask.
Add 4.0 mL of water. Place the conical flask in the water trough at least for 5 minutes to attain constant
temperature as that of the bath.
4. Add 4.0 mL of distilled water and add 1.0 mL of 1.0 M HCl solution to the conical flask from the burette
and start stop watch while 0.5 mL HCl has been added. Swirl the conical flask while adding HCI. Note
that the total volume of the reaction mixture is 55.0 mL.
5. Note the time taken for the mark X' to become invisible for the first time carefully (This may be taken as the
stage of the completion of the reaction). Let the time taken bet1.
6. Repeat the experiment at least 4 more times using 3mL, 2 mL,1 mL and 0.0 mL of distilled water
and 2 mL, 3 mL, 4 mL and 5 mL of 1.0 M HCl in 2nd, 3rd, 4th and 5th experimental parts
respectively to 50 mL of 0.1 M Na2s2o3 solution taken each time in the conical flask so that the total
volume of the reaction mixture is 55.0 mL. Each time, note down the time taken for the disappearance of
the mark 'X' completely for the first time. Let the respective times be t2, t3, t4 and t5 respectively. Record
your observations in table 2.1.
Table 2.1: Effect of concentration of HCl on the rate of reaction between Na2s2o3 and HCI
Volume of 0.1 M Na2S2O2 solution used each time = 50 mL
Concentration of HCl used in the reaction = 1.0 M.
Total volume of solution = 55 mL
Volume of reaction mixture
Sl.No. Na2S2O2 H20 (mL) HCl (mL) Total volume Time taken for mark ‘X’ to
(mL) become invisible (in sec.)
1 50 4 1 55 t1=
2 50 3 2 55 t2=
3 50 2 3 55 t3=
4 50 1 4 55 t4=
5 50 0 5 55 t5=
Second Year 99
Part B
Study of the effect of temperature on the rate of reaction between Na,s,o, and HCI
1. Take 50 mL of 0.1 M Na2s2o2 into a 100 mL conical flask that has been marked "X" with a marker
pencil at the centre of the bottom outer surface. Keep the flask in a thermostat or constant tempera-
ture water bath at 30°C for sufficient (atleast 5 minutes) time to get 30°C temperature. Now add 5
mL of 1.0 M HCl, but start a stop watch after the addition of first 2.5 mL of HCl while swirling the
flask during the addition of 5 mL of 1.0 M HCl.
2. Keep the flask aside and observe carefully when it becomes that 'X' mark is simply invisible for the first
time. Note the time taken for it. Let it be t30.
3. Repeat the experiment each time with 50 mL fresh 0.1 M Na2s2o3 solution thermostating to respective
temperature and adding 5 mL of 1.0 M HCl at 40°C, 50°C, 60°C and 70°C respectively while swirling
the solution. Let the times of complete invisibility of 'X' mark in the respective experiments be t40, t50, t60
and t70.
Record your observations in table 2.2.
Table 2.2: Effects of temperature on the rate of reaction between Na2s2o3 and HCI
Volume of Na2s2o3 solution used each time = 50.0 mL at respective temperatures
Volume of HCl used each time = 5.0 mL at respective temperatures.
Sl.No. Temperature of the reaction Time 't' for mark 'X' to become
mixture (°C) constantly invisible for the first time
1 30 t30
2 40 t40
3 50 t50
4 60 t60
5 70 t70
Plot two graphs, one for the volume of HCl added versus the respective times taken for the 'X'
mark to become invisible (Part-A) and the other for different temperatures versus the times taken for
the 'X' mark to become invisible for the first time (part-B) with variation of time on X-axis and
variation of volume of HCl (part-A) or variation of temperature (part-B) on Y-axis.
Note
1. If thermostat (constant temperature bath) is not available, use water bath for this purpose. Keep
the water in the bath stirring continuously. After reaching the constant temperature, if there is a
possibility of further increase in temperature, take the burner a side. It may be repeated number
of times if necessary.
Stop watch is started after adding half of the reactant to compensate the time error that takes
place during the addition of the reactant.

Experiment : 2.2
Effect of Variation of [I-) on the Rate of Reaction Between Iodide Ions and Hydrogen perox-
ide at Room Temperature
Aim: To study the effect of the variation of iodide ion concentration on the rate of the
reaction between iodide ion and hydrogen peroxide.
Principle
The reaction between 1- and H2O2 takes place in acidic medium as
21- (aq) + H2O2(1) + 2H+(aq)  12(g) + 2H20(1)
Here, H2O2 oxidises I- to I2. The I2 can be reduced as fast as it is formed back into I- with a calculated
quantity of Na2 S2O3. When S2 032- ions are completely oxidised to tetrathionate (S4O62-) in the presence of
starch indicator solution, the I2 liberated by the reaction of H2O2 on I- forms an intense blue complex with
starch. The time required to consume a fixed amount of S2 032- is reproducible. As it is the time that is the basis
for the appearance of colour is noted, the reaction is also called as clock reaction.
Conical flasks (250 mL) : 5 2.5 M H2SO4
Conical flask (500 mL) :1 0.1 M KI solution
Stop watch :1 0.04 Na2 S2O3 solution
Measuring jar (100 mL) : 1 3% H2O2 solution
Trough :1
Procedure
1. Take a 500 mL conical flask. Put in it 25 mL of 3% H,O,, 25 mL of 2.5 MH,SO, 5 mL of freshly
prepared starch solution and 195 mL of distilled water. Stir the contents of the conical flask and
keep the flask in a water bath. Mark the flask as ‘A’.
2. (a) Take four 250 ml conical flasks and mark them as B, C, D and E. Add to the four flasks Na2s2o3
solution (0.04 M), KI solution (0.1M) and distilled water to the flasks B, C and D in proportions as
given below. The flask E is kept for carrying the reaction.
(b) (i) Add to the conical flask 'B' 10 mL Na2S2O3 solution (0.04 M), 10 mL KI solution (0.1 M)
and 80 mLdistilled water. Shake the contents well for thorough mixing and keep it in a water bath.
(ii) Add to the conical flask 'C' 10 mL of 0.04 M Na2S2O3 solution, 20 mL of (0.1 M) KI solution
and 70 mL of distilled water. Shake the contents well and keep the flask in the water bath.
(iii) Add to the conical flask D 10 mL of (0.04 M) Na2S2O3 solution 30 mL of (0.1 M) KI solution
and 60 mL of distilled water. Shake the contents and keep this flask also in the water bath.
(c) (i) Take the conical flask 'E'. Add to it 25 mL of the solution from the flask ‘A’ with a mea-
suring jar. Now add 25 mL of the solution from flask 'B' with constant stirring. Start the stop
watch when about 12 mL of the solution is transferred from B to E. Keep the flask
Second Year 101

E in water bath to maintain its temperature constant. Note the time taken for appearance of
blue colour.
(ii) Carry out the experiment with the solutions of flasks C and D separately using 25 mL of the solution
from them mixing with 25 mL of the solution from A and keeping the flasks containing
these mixtures thermostated and noting the time taken for the appearance of the blue colour in each
case.
3. Repeat the experiment with solution of flasks B, C and D and mixing them with solution of A as mentioned
in (i) and (ii) above. Using the results obtained in 2 (c) (i) and (ii) and 3, the average time required for the
appearance of blue colour in each case is calculated.
4. Draw the table 2.3 and write the observations.
Based on the observations made, find the variation of the rate of the reaction with respect to the change in the
concentration of iodide ions.
Table 2.3: Study of the rate of reaction between I- and H2O2 in acidic medium
SI. Time taken for the appearanc
No. Composition of the reaction mixture of the blue colour Average
First reading Second reading
1. 25 mL of the solution from flask A +
25 mL of the solution from flask B
25 mL of the solution from flask C
25 mL of the solution from flask D
Write the conclusions on the basis of the data of table 2.3.

Note
(i) See that the concentration of Na2 S2 O3 solution is less than that of KI solution.
(ii) Use freshly prepared starch solution and fresh H2O2
(iii) Note the time when the blue colour appears for the first time.
Experiment : 2.3
Rate of Reaction Between Potassium Iodide (KI) and Potassium Peroxodisulphate (Persulphate)
Solutions!..
Aim : To study the rate of the chemical reaction between KI (aq) and K2S2O8 (aq)
Principle
The reaction between KI and K2S208 takes place as S2082- + 21-  2S022- + 12 (slow) If a calculated
quantity of Na2S2O3 and starch indicator solution are added to Kl solution and then if potassium persulphate
is allowed to react with KI solution, the following reaction takes place.
21- +S2,082-  2S042- +I2 - (1)
The liberated I2 does not give blue colour with starch solution because, I, instantaneously reacts with
thiosulphate to form I-.
12 + 2S2 032- 21-+ S4062-- (2)
This reaction continues until the whole of S2032- is consumed. When S2032- is exhausted the solution
immediately gets blue colour due to the unreacted I2.
I2 + starch  I2 - starch -(3)
colourless blue colour
(indicator)
Reaction shown by equation (1) is slow and it is called the main reaction. Reaction shown by equation
(2) is fast and it is called the fast reaction. Reaction (3) is called the indicator reaction.
Time for the appearance of the blue colour depends on
(a) the initial rate of formation of I2 which itself depends on (l-) and (S2O82-)
(b) the amount of thiosulphate present.
For specified concentrations and temperature, the time for the appearance of blue colour has a clock
like accuracy. The combination of the above three reactions is generally called a clock reaction.
Addition of the monitor, S2 032- again discharges the blue colour and when S2 032- is completely
consumed the blue colour reappears. Addition of the monitor is like rewinding of the chemical clock.
The subsequent time intervals will be larger even with the additions of the same quantities of Na2s2o3
because, the concentration of S2082- gradually decrease and the reaction becomes progressively slower.
Thermostat or water bath 0.01 M Pottasium persulphate solution
250 mL measuring jars - 2 0.3 M KI solution
Beakers (100 mL) - 2 0.0005 M Na2s2o3 solution
Pipettes (25 mL) – 2 Freshly prepared starch solution - 10 mL \
Stop watch
500 ml beakers - 2
Procedure
Solution A : Take 250 mL of 0.01 M K2S2O8 solution in a 500 ml beaker. Label it as A.
Solution B: Take another 500 ml beaker and put in it 250 mL of 0.3 M KI solution, 0.0005M
Na2s2o3 + 10 mL of starch solution in 250 mL mixed solution. Label it as B.
Procedure
1. Keep both the beakers containing solution A and solution B in water trough for sufficient time till they get
constant (room) temperature.
2. Take a dry 100 ml beaker and pipette out 25 mL of solution A into it. Take second beaker and put in it 25
mL of solution B. Add solution B to solution A while starting the stop watch after adding about 12 mL of
solution B. Mix the solutions A and B by
Second Year 103
swirling and keep that beaker on a white paper or white glazed tile. Note down the time in the stop-
watch when the blue colour appears for the first time.
Repeat the experiment by preparing the reaction mixtures as follows:
S.No. Solution A Water Solution B
1. 20 mL 5.0 mL 25 mL
2. 15 ml 10.0 mL 25 mL
3. 10 mL 15.0 ml 25 mL
Note down the respective times taken for the formation of blue colour for the first time in each experiment.
Experiment : 2.4
Reaction Between Potassium lodate (KIO3) and Sodium Sulphite (Na2S2O3) using Starch Solution
as Indicator (Clock Reaction)
Principle
This experiment is carried out in the same way as the reaction between Iodide (I-) and persulphate
(S2082-) with starch indicator.
1. I03- + 3S032- I-+3S032-: sulphite is oxidised to sulphate and iodate is reduced to iodide.
2. 5I- + 6H+ + I0-3  3H20 + 3I2: I03- oxidises I- to I2 and it gets reduced to I2.
3. l2 + starch solution (colourless)  I2, starch solution (blue colour)
(in the presence of thiosulphate) (in the absence of thiosulphate)
Procedure
1. Take a 500 mL conical flask. Mark it as A. Transfer 50 mL of 6% KIO3 solution + 50 mL of 2 MH2So4
and 100 mL of distilled water into 'A'. Thermostat it after mixing the solution. Let this be solution A.
2. Take four 250 ml conical flasks. Mark them as B, C, D and E.
S. Flask Solution taken in each flask
No. marked as
1. B 20 mL 6% Na2 SO3 + 5 mL 5 % starch solution + 75 mL distilled water
2. C 15 mL 6% Na2 SO3 + 5 mL 5 % starch solution + 80 mL distilled water
3. D 10 ml 6% Na2 SO3 + 5 mL 5% starch solution + 85 mL distilled water
4. E 5 mL 6% Na2 SO3 + 5 mL starch solution + 90 mL distilled water
Keep all the four flaks in a thermostat
3. Take another conical flask and mark it as F. Take in it 25 mL of the solution from flask A and add 25 mL
of the solution from flask B start stop watch after adding about 12 mL of the solution from B. Keep the
flask F on a white paper or glazed tile. Note the time taken for the appearance of blue colour for the first
time.

Carry out the experiment always taking 25 mL solution from A but 25 mL solution from C, 25 ml
solution from D and 25 mL solution from E separately in three other experiments. Note the respec-
tive times for the appearance of blue colour for the first time.
Repeat the experiment once again.
Record your observations in table 2.4
Table 2.4: Study of the reaction rate between KIO3 and Na2S2O3 in acidic medium
S. Composition of the Time taken for the appearance of Average time
No. reaction mixture the blue colour in seconds. (sec)
1 25 mL from flask A + tB t1B tB+ tB1
25 mL from flask B 2
2. 25 mL from flask A + tC t1C tC+ tC1
25 mL from flask C 2
3. 25 mL from flask A + tD t1D tD+ tD1
25 mL from flask D 2
4. 25 mL from flask A + tE t1E tE+ tE1
25 mL from flask E 2
Write your conclusions on the basis of the data obtained from table 2.4.
Note
1. As Na2S2O3 has a tendency to get oxidized by air in the solution, prepare always fresh solution.
2. Keep (KIO3] > [Na2 So3). If this is not maintained what would happen?
3. Starch solution should be freshly prepared.
1. (a) For the reaction S2O32-(aq) + 2H+(aq)H2O(1) + SO2(g) + S(s)
Give the conditions under which its rate law can be written as, rate of formation of colloidal sulphur =
K[S2 O32-] [H+]2
(b) From the above rate law expression for the formation of colloidal sulphur, if the concentrations of H+
and S2032- are both doubled, how many times the rate of the reaction increase?
2. (a) For a given reaction, its rate may change but its rate constant does not change at given temperature.
How do you comment on this statement?
(b) How does the rate constant of a reaction vary with the temperature?
3. Suggest an experiment with procedure to study the dependence of the rate of formation of colloidal
sulphur on the nature of monobasic acid for the reaction
S2O32- (aq) + 2H+(aq) H2O(1) + SO2(g)+ S(s)
Second Year 105

4. S2032- has the following structure.
Which sulphur (1 or 2) would be precipitated? Can you suggest an experiment to verify it?
S2
O- S1 O-
O
5. (a) Explain order and molecularity of a chemical reaction.
(b) The order of a reaction may be zero or even a fraction in addition to an integer, but, the
molecularity of a reaction is only an integer – Explain.
6. Write the units of (a) rates of reactions of zero, first, second, third and nth order reactions and (b) rate
constants of zero, first, second, third and nth order reactions.
7. Explain the role of I2 and I- in the above experiment.
8. What is the oxidation number of 'S' in S4062- ?
9. Why does I2 give blue colour with starch?
10. Can you suggest any other oxidising agent, other than H2O2 in this experiment?
11. The above reaction is called a clock reaction. Why?
12. In the above experiment (KI) > [Na2 S2 O3]. Why?
13. You would observe an increase in time for appearance of blue colour to the solution in the above
experiment. Why?
14. What would happen for the time for the appearance of blue colour, if the temperature of the
experiment is raised by 10°C?
15. What are the factors that effect the rate of reaction in the present study?
16. For maintaining acidic medium can we use HCl and HNO3? Why?
17. I03- + 3SO32- I- + 3SO42- -1
5I + 103- + 6H+ 3H2O + 3I2 - 2
In (1) and (2) which would be the rate determining step? Give the molecularity of the rate de-
termining step.
18. Can AsO33- be used in place of So32- in the above reaction? Give the reason.
19. [KIO3] should be greater than [Na2SO3]. Why?


CHAPTER-3
THERMOCHEMISTRY
The sum of the various forms of energy associated with a given system is called its internal
energy, denoted by 'U'. As internal energy involves some indeterminable factors, it is not possible to
find the exact internal energy of a system. However, if the system undergoes a change in the state, the
internal energy change (U) of the system can be experimentally determined. At constant volume if
qv calories of heat is supplied to the system, its internal energy increases as qv = U. If the system
loses qv calories heat energy, then its internal energy decreases as qv = U, here U= negative and in
the first case U = positive.
It is more convenient to carry chemical change at constant pressure (atmospheric pressure) than at
constant volume. Heat changes measured for the reactions at constant pressure are called enthalpy changes.
They are denoted by H.
If qp is the heat energy gained or lost by the system at constant pressure
then H = qp
But qp = m cp T, where 'm' is mass of the system, say a solution, Cp = Heat capacity;
T = change in temperature.
But mass = volume x density
m=Vxd
 H = qp = d V Cp T
Measurements of heat changes are carried out by calorimetry process using calorimeters. During
measurement of heat changes, calorimeter, thermometer and stirrer also absorb heat. This amount of heat is
known as calorimeter constant and it is also to be known. In the case of glass apparatus like a beaker, as its
conductivity is very low, only that part (area) which is in contact with the liquid is to be taken into account.
To determine the calorimeter constant, method of mixtures is used. For this the following procedure is
adopted.
To find out the calorimeter constant, a known volume of hot water at given temperature is added to a
known volume of water taken in the calorimeter at room temperature. As per the first law of thermodynamics
the energy is conserved and here the heat energy gained by the calorimeter and cold water in it is equal to the
energy lost by hot water.
Enthalpy change of calorimeter, (H1) + enthalpy change of cold water (H2) = enthalpy change of
hot water (H3)
If tc, th and tm are temperatures of cold, hot and mixture of cold and hot water then
m1 Cp1 (tm – tc) + m2 Cp (tm - tc) + m3 Cp (tm – th ) = 0
Second Year 107

Here m1 is the mass of calorimeter, m2 that of cold water and m3 the mass of hot water. Cp1 and Cp
are heat capacities of calorimeter and water respectively. If the process is carried out in a glass beaker we can
calculate only calorimeter constant W which is equal to m1 Cp1
 W(tm – tc ) + m2 Cp(tm – tc) + m3 Cp((tm – th) = 0
m2 Cp(tm – tc) + m3 Cp(tm – th)
W= (tm – tc)
But mCp = d V Cp
Specific heat capacity or heat capacity per gram is 4.184J.
Hence dVCp = 4.184 JmL-1 K-1
(4.184) [VC(tm – tc) + Vh (tm – th) ]
W= JK-1
(tm – tc)
VC Vh are volumes of cold and hot water respectively.
Experiment : 3.1
Determination of the Enthalpy of Solution of Potassium Nitrate or Copper Sulphate in
Water
Aim: To determine the enthalpy (heat) of solution of potassium nitrate or copper sul phate in water.
Principle
When a solution is prepared by dissolving a solid solute in a liquid solvent, the process is accompa-
nied by the heat liberation or absorption. The enthalpy change when one mole of the solid solute is dissolved
in the large excess of the solvent so that on further addition of the solvent there is no further enthalpy change
is called the enthalpy (heat) of solution.
Suppose that we dissolve a known amount of solute in a known amount of solvent say water, it
involves the heat liberation or absorption. If the dissolution is done in a calorimeter, then, H1 + H2 +
H3 + H4 = 0, where
H1 = Heat gained by calorimeter + stirrer + thermometer
H2 = Enthalpy change of solution i.e., water in the calorimeter
H3 = Enthalpy change of added solution/water in calorimeter
H4 = Enthalpy change of the dissolution
The product of heat capacity of solution and density i.e., d x Cp is taken as 4.184 J mL-1 K-1 for
aqueous solutions which is nearly equal to that of water.
Apparatus and chemical required
Beakers (250 mL)-3, beaker (500 mL), thermometer (110°C), glass rod, cardboard, stirrer,
cotton and potassium nitrate or copper sulphate (2 g)

Procedure
Part - A
Determination of calorimeter constant of the given calorimeter say beaker
1. Take 100 mL of water in a 250 mL beaker marked as A.
Keep this beaker on a wooden block kept in a larger
beaker (500 mL). Pack the empty space between the
small beaker and large beaker with cotton wool. Cover
the big beaker with card board by inserting the
thermometer and stirrer into small beaker through the Stirrer
cardboard, record the temperature of water. Let it be t1°C.
2. Take another 250 mL beaker mark it as B. Put in it Thermometer
exactly 100 mL hot water at constant temperature t2°C. Card board
3. Add hot water from beaker B to beaker A by lifting the
cardboard. Stir the contents and note the temperature of Beaker
the mixed water. Let it be t3°C.
Cotton wool
4. Calculate the calorimeter constant (W) by using the
equation ...
Small wooden
(4.184) [VC (t2 - t1) + Vh (t3 – t2) ] piece
W=
(t3 – t1) Fig. 3.1: Determination of
Here VC = Volume of cold water calorimeter constant
Vh = Volume of hot water

Part - B
Determination of enthalpy of solution
1. Take 100 mL of distilled water in the beaker A, the calorimeter constant of which is known from
part A. Place it on a wooden block taken in a big (500 ml) beaker. Fill the empty space between
the two beakers with cotton wool. Cover the big beaker with a cardboard. Record the temperature
of water in the small beaker. Let it be t1°C.
2. Add a known amount, say 'm', g of finely powdered potassium nitrate or copper sulphate to water,
stir the solution to dissolve the solute completely. Note down the temperature attained by the
solution. Let it be t2°C.
Enthalpy of solution is calculated as given below:
Total mass of the solution = (mass of solvent + mass of solute)
= (100 + m) g
Note that the density of water is taken as 1 g mL
Second Year 109

3. Change in temperature = t2°C-t1°C = t
Enthalpy change of calorimeter = calorimeter constant x t
= W x t
Here W = calorimeter constant
Enthalpy change of solution = [(100+m) t] x 4.184J
Total enthalpy change of the calorimeter + solution = [(w x t) + (100+m)t] x 4.184J
Heat liberated when one gram of solute is dissolved is
[(W x t) + (100+m)t] x 4.184J
m
For 1 mole of solute
1. If the solute is KNO3 the heat of dissolution = molar mass of KNO3 x Heat of
101 [(W x t) + (100+m)t] x 4.184J
dissolution per g. =
m
(Molar mass of KNO3=101 g mol-1)
2. For copper sulphate
(a) For anhydrous CuSo4 the heat of dissolution per mole
159 [(W x t) + (100 + m)t] x 4.184J
= m
(Molar mass of anhydrous CuSO4 = 159 g mol-)
It is experimentally found that the heat of solution of anhydrous Cuso4 is 15.89 kcal (exother-
mic).
(b) For hydrated Cuso4 i.e., CuSO4.5H20, the heat of dissolution per mole
249.5[(W x t) + (100 + m) t] x 4.184J
=
m
The heat of solution found experimentally for CuSo4 5H20 is 2.80 kcal (endothermic) From
(a) and (b) we can calculate the heat of hydration of Cuso4 as equal to + [15.89-(-2.80)] = +
18.69 kcal mol-I (exothermic).
Experiment : 3.2
Enthalpy of Neutralization of Strong Acid (HCI) with a Strong Base (NaOH)
Aim: To determine enthalpy of neutralization of strong acid (HCl) with a strong base (NaOH).
Theory
Neutralisation reaction is the reaction between H+(aq) ions produced by an acid and OH-(aq)ions
produced by a base to form H2O(1) As the reaction involves a bond formation between H+ and OH-, the
neutralization process is always exothermic.
Enthalpy of neutralization is the heat energy liberated when one mole of H+ ions produced by
an acid combine with one mole of OH- ions produced by the base to form one mole of water.
H+(aq) + OH-(ag)  H2O(1) ; neut H = negative
(acid) (base)
Enthalpy of neutralization for strong acid and strong base is constant. It is equal to 57.0 kJ mol-. If
either acid or base or both of them are weak then a part of this energy would be used to ionize that acid, base
or both acid and base which are weak. Therefore, the heat of neutralization in those cases would be less than
57 kJ mol-1.
Beakers (250 mL) - 3 Cotton wool 1 M HCl : 100 mL
Beakers (500 mL) - 1 Small wooden block 1 M NaOH: 100 mL
Thermometer (110°C)-1 Card board piece
Glass rod - 1 Stirrer
Procedure
Part - A: Determination of the calorimeter constant
Follow the same procedure given in the previous experiment.
Part - B: Determination of enthalpy of neutralization
1. Take 100 mL of 1.0 M HCl in the beaker of 250 mL volume (calorimeter) cover it with cardboard.
2. Take 100 mL of 1 M NaOH in another beaker of 250 mL volume.
3. Note down the temperature of both the solutions taken above. It is the same temperature. Let it be
t1°C.
4. Now add 100 mL of 1 M NaOH to 100 mL of IM HCl in the beaker that acts as the calorimeter. Mix
the solutions by stirring and note the final temperature. Let it be t2°C.
Calculation of the enthalpy of neutralization
1. Rise in temperature due to the neutralization reaction is (t2-t1)oC = t°C.
2. Heat evolved during the above neutralization process
Q = (100+100+W) x t°C x 4.184 J
Here 100 and 100 are masses of 1 M HCl and 1 M NaOH solutions. It is assumed that the
density of the solution is 1 g L-1. W is calorimeter constant...
3. The heat evolved 'Q' is only for 100 mL of 1 M acid and 100 mL of 1 M base neutralization. We
have to calculate it per 1 M 1000 mL each of the solutions i.e., the heat of neutralization is
1000xQ
=10Q.As the value in J is big, express it in k(J) mol-1
1000
Second Year 111

Experiment: 3.3
Experimental Determination of the Enthalpy Change for the Reaction Between
Acetone and Chloroform
Aim: To determine experimentally the enthalpy change for the reaction between
acetone and chloroform.
Principle
Chloroform and acetone form a solution like a non-ideal liquid pair system. They show nega-
tive deviation from Raoult's law indicating that the intermolecular forces of attraction between
CH3COCH3 (acetone) and CHC13 (chloroform) molecules are stronger than those between CH3COCH3
and CH3 COCH3 molecules or CHCl3and CHCl3 molecules. This is attributed to the ability of acetone
and chloroform molecules to form hydrogen bonding between them.
H3C CI
C=O-------H-C CI
H3C   CI
Hydrogen Bonding
In the pure acetone or chloroform the intermolecular forces between their molecules are only
vander Waals forces which are weaker than hydrogen bonding. This extra attraction between CH3COCH3
and CHCl3 molecules in the form of hydrogen bonding releases energy in the form of heat. This heat
energy which is liberated depends on the amounts of liquid components mixed. We can determine and
calculate it for 1 mole of chloroform and 1 mole of acetone mixture.
Heat gained by the Enthalpy change enthalpy change enthalpy change of
calorimeter + thermometer + of acetone + of chloroform + hydrogen bonding
+ stirrer (H1) (H2) (H3) (H4)
H4 = (H1+ H2+H3)
Beaker (250 mL), boiling test tube, thermometer (110°C), cotton wool, glass rod, measuring
jar, stirrer, acetone (10 mL) and chloroform (20 mL)
Procedure
Part A : Determination of the calorimeter constant
The same procedure as given in the previous experiments is adopted, but in those experiments
a beaker and 100 mL each of cold water and hot water were used whereas here, we take a boiling test
tube with 8 mL of cold water and 7.5 mL of hot water instead of 100 mL each.
(Note: Here we take total volume of water as 15.5 mL. Why?
For this observe the following discussion
molar mass of that liquid
Volume of one mole of a given liquid =
density of that liquid
If we want 0.1 mole of the liquid, we have to take 1/10 that of the above volume. Suppose that we
want to take 0.1 mole of acetone and 0.1 mole of chloroform for our experiment, let us calculate how many
mL of each liquid is required.
Molar mass of CH3COCH3 = 58 g mol-1 Molar mass of CHCI3 =119.5 g mol-1
Density of acetone = 0.79 g ml-1 Density of chloroform =1.47 g mL-1
Volume of 1 mole of acetone Volume of Imole of CHCI3
58g mol-1 Molar mass of CHCl3 119.5 g mol-1
= = =
0.79g mL-1 Density of CHC13 1.47 g mL-1
= 73.4 mL = 81.4 mL
1 mole of acetone = 73.4 mL 1 mole of chloroform = 81.4 mL
0.1 mole of acetone = 7.34 mL 0.1 mole of chloroform = 8.14 mL
= 7.5 mL (approx.) = 8.0 mL (approx.)
Total volume of CHCI3 and CH3 COCH3 = 7.5+8.0=15.5mL]
Part-B
Enthalpy of interaction of CHCI3, and CH3 COCH3,
1. Take 8.14 mL or 8.0 mL of chloroform in the boiling test tube and insulate it in a beaker with
cotton wool (8.14 mL of chloroform = 0.1 mole of chloroform). Let the mass of chloroform be m1
g. Note the temperature of chloroform. Let it be t1°C.
2. Add 0.1 mole of acetone (7.34 mL) i.e, about 7.5 mL of acetone to chloroform in the boiling test
tube. Let its mass be m2 g. Stir the liquid mixture gently with a stirrer. Note down the temperature of
the mixture of CHCl3 and CH3 COCH3. Let it be t2°C.
3. Let the calorimeter constant be W for the boiling test tube etc. Heat gained by the calorimeter =
W(t2-t1)°C
Take the specific heats of chloroform and acetone from the literature. Let them be q1 and q2
respectively.
Heat gained by chloroform = mass of chloroform x its specific heat (t2-t1)
= (m1 xq1x t)
Heat gained by acetone = mass of acetone x its specific heat x (t2-t1)
= (m2 xq2x t)
Total heat gained by calorimeter, acetone and chloroform
= - [W(t2-t1)+m1q1 (t2-t1)+m2q2(t2-t1)]
The negative sign tells that the process is exothermic.
Precautions
1. Use in all the experiments a thermometer graduated upto 0.1°C atleast.
2. In the determination of the calorimeter constant in all the experiments, note the temperature of
hot water just before mixing it with cold water.
3. Avoid using large amounts of chemicals.
4. Avoid too much stirring as it may produce heat due to friction.
Second Year 113

5. Cotton wool is to create insulation between the outer beaker and inner beaker or boiling test tube.
6. Measure the volumes of solutions like that of HCI, NaOH or liquids like CHCI3 and CH3COCH3
accurately.
7. Note that the total volumes of different liquid mixtures taken in the calorimeter and total volume
of cold and hot water taken in it should be equal.
1. Why should we calculate the heat of neutralization for 1000 mL of 1 M acid and 1000 mL of 1 M
base in the above experiment?
2. Why is the heat of neutralization less with weak acids or weak bases or weak acids and weak
bases?
3. Rise in temperature on H2O(1)  H+(aq) + OH-(aq) favour the equilibrium to shift in the forward
direction. Why?
4. Benzene and acetone form ideal solution but not chloroform and acetone. Why?
5. Ethanol and water show positive deviation from Raoult's law. Why?
6. Mention two liquid pairs that show mixingH negative and positive respectively.
7. Interactions between liquid pairs effects their vapour pressures. Explain.
8. The strength of hydrogen bonds can be explained on the basis of the heat evolved during the
mixing of the component liquids. Explain?


CHAPTER-4
ELECTROCHEMISTRY
4.1 Effect of Concentrations of Electrolytes on the Cell Potential of a Galvanic Cell
A galvanic cell is a device that is used to convert chemical energy into electrical energy. A
galvanic cell is a combination of two half cells. If in one half cell oxidation takes place (losing of
electrons), in the other half cell reduction takes place (gaining of electrons). The overall galvanic cell
reaction is a redox reaction and the chemical energy involved in this reaction is converted to electrical
energy.
In each half cell in the galvanic cell there is generally an electrolyte and an electrode. The two
half cells are connected through electrodes as well as solutions of electrolytes using a salt bridge. The
potential difference between two electrodes of a galvanic cell is called the cell potential. The cell
potential is measured in volts. The cell potential is the difference between the reduction potentials of
the positive electrode (cathode) and the negative electrode (anode).
Ecell = E(+ve electrode or cathode) -E (-ve electrode or anode)
It is not particularly feasible to measure the potential of an individual half cell, but the difference
in the potentials of the two half cells can be measured. This difference in the potentials is the
electromotive force (emf) of the cell.
4.2 Conventions Regarding a Galvanic Cell
1. The potential of standard hydrogen electrode denoted by Pt, H, (g, 1 bar)/ H+(aq, 1M) is
conventionally taken as zero at all the temperatures corresponding to the reaction
H+(aq) + e-  1/2H2
2. Half cell potentials of other half cells are measured with reference to hydrogen electrode. Here a
cell is constructed with standard hydrogen electrode as negative electrode (anode) and the other
electrode as positive electrode (cathode) maintaining standard conditions like the pressure as 1
bar in case of a gas and the concentration of electrolyte solutions as 1M and temperature 25 °C.
The cell potential experimentally determined is taken as the standard electrode potential of the
other half cell, because it is conventionally taken that standard hydrogen electrode half cell has
zero potential.
Then, Eocell = E°(+ve electrode or cathode) - E°(-ve electrode or anode)
Negative electrode is standard hydrogen electrode half cell.
Therefore, Eocell = E°(+ve electrode or cathode)
4.3 Nernst Equation
Nernst derived a relationship between standard electrode potential of a given half cell and the
potential at any concentration other than standard concentration of its electrolyte. This is as follows.
Second Year 115

Mn+ + n e-  M(s)
RT [m(S) ]
E(Mn+/M) = Eo (Mn+/M) - nF ln [Mn ]
aq)
2.303RT
E(Mn+/M) = Eo (Mn+/M) - log Q
nF
[Products]
Q = Reaction quotient ratio = [Reactants]
2.303RT  M ( s ) 
E(Mn+/M) = Eo (Mn+/M) - nF
log  M n + ( a q ) 
[M(s)] is taken as unity ; R= 8.314 JK-1 mol-1 ; T = 298 K; F = 96487 C mol-1

n = number of electrons gained by metal M for reduction
2.303 x 8.314 x 298 1

E = E0  log n+
n x 96487 M (aq) 
0.0591
E = E0 + log Mn+(aq) 
n
The variation of the cell potential of Daniel cell with change in the concentration of an
electrolyte is studied as follows.
4.4 Experiment : 4.1
Study of the Variation in the Cell Potential of Daniel Cell at Room Temperature with
Change in Concentration
Aim: To study the variation in the cell potential of Daniel cell Zn(s)[Zn2+(aq)||Cu2+(aq)|| Cu(s) with
the change in the concentrations of the electrolytes taking different concentrations of Cuso4for
the same concentration of ZnSO4.
Principle
For Daniel cell Zn(s) | Zn2+(aq)(1.0M) ||Cu2+(ag)(x M) | Cu(s)
0.059
Ecu+2/cu = E°Cu2+/cu + log[Cu2+]
2
The variation in the electrode potential of Cu2+/Cu electrode due to the variation of Cu2+ concentra-
tion brings the variation in the overall cell potential
Ecell = Ecu2+/cu – EoZn2+ /Zn
The experiment may be carried out even by varying the concentrations of Zn2+ keeping the concen-
tration of Cu2+ the same.
Zinc plate, copper plate, beakers (50 mL), potentiometer (preferable) (or voltmeter), salt bridge 1.0
M ZnSo4 solution, Cuso4 solution of concentrations of 0.20 M, 0.10 M, 0.05 M, 0.025 M and 0.0125 M.

Procedure
1. Arrange the galvanic cell as shown in the fig.4.1 using 1.0 MZnSo4 and 0.2 M CuSO4 solution. Mea-
sure the potential difference of the cell. Note the polarity of the electrodes to enable a sign to the cell
potential.
2. Remove the salt bridge after measuring the cell potential. Replace the beaker of 0.2 M CuSO4 solution
with the beaker of 0.1 M CuSO4 solution. Keep the salt bridge back and measure the potential differ-
ence.
3. Carry out the experiment with 0.05 M,0.025 M and 0.0125 M CuSO4 solutions also.
4. Calculate log (Cu2+] and Ecu2+cu, for different concentrations of Cu2+ solution used. Note down the
electrode potential values of Cu2+(aq) | Cu(s)electrode for different concentrations of Cu2+ in the table
4.1.
5. Plot a graph for the variation of cell potential with the concentration change taking (Cu2+(aq)] on X-axis
and (Ecu2+/cu) on Y-axis
Table 4.1: Cell potential data
S.No. [Cu2+(aq)] (mol L-) log [Cu2+(aq)] Ecell (volts) Ecu+2/cu (volts)
(experimental value)
1. 0.2 M
2. 10.1 M
3. 0.05 M
4. 0.025 M
5. 0.0125 M
Report : Write the conclusions on the basis of the data obtained.
Voltmeter
Salt bridge
Zinc Copper
eletrode electrode
1.0 M ZnSO4 Cu2+ (aq.)
Fig. 4.1: Set up of Zn(s)/Zn2+(aq.), (1.0 M) || Cu2+ (aq., x M)/Cu(s) cell
Second Year 117
Voltmeter
Precautions
1. Clean Cu and Zn strips and connecting wires with sand paper before use.
2. Keep the salt bridge immediately in distilled water after its use.
1. For the reaction Zn(S) + Cu2+(aq)  Zn2+(aq) + Cu(s) apply Le-chatelier's principle to justify the
results obtained. Get a mathematical rationalisation of the results.
2. Find the slope of the graph. Does the experimental value and theoretical value match together ?
Explain the factors effecting the slope.
3. Device one more experiment to study the effect of concentration of an electrolyte on the cell
potential.
4. Explain the nature of electrolyte solution used in the salt bridge.
5. We cannot measure the electrode potential of a single electrode independently. Why?

CHAPTER- 5
CHROMATOGRAPHY
Chromatography is essentially a separation process for mixture of substances, but this is also
adapted to identify the components of mixtures. Purification of the components is also possible with
this method. Chromatography is a physical process in which the components to be separated are
distributed between two phases, one of which is stationary while the other is a mobile phase.
The stationary phase is usually in the form of a packed column in column chromatography, a thin layer
adhering to a suitable form of backing material such as glass in thin-layer chromatography. In column chroma-
tography, mobile phase flows through the packed column, while in thin layer chromatography, mobile phase
moves by capillary action. In thin layer chromatography, stationary phase may be either a liquid or a solid and
the mobile phase may be a liquid or a gas.
In partition chromatography, stationary phase is thin film of liquid adsorbed on an essentially inert
support. Mobile phase may be a liquid or a gas. Paper chromatography is an example of partition chromatog-
raphy in which liquid present in the pores of paper is stationary phase and some other liquid is mobile phase.
Separation depends upon partition of substance between two phases and the adsorption effects of inert
support (paper) on compounds undergoing chromatographic separation. In chromatography, substance equili-
brates between a mobile and a stationary phase. The more the interaction of substance with the stationary
phase, slower is its movement. Separation of the components of a mixture by using paper chromatography is
given below.
Experiment : 5.1
Separation of Pigments Present in the Extracts of Leaves and Flowers
Aim : Separation of pigments present in the extracts of leaves and flowers by paper chromatography and
determination of Rf value of components. Select the leaves and flowers whose pigments are soluble
in water.
Theory
Paper contains lots of pores. Water molecules which enter into the pores of filter paper act as the
stationary phase. Flowers and leaves are selected in such a way that their pigments are soluble in water. The
moving phase is solvent water. As the moving phase passes through the spot (the reference line) on which the
sample (extract from flower or leaf) has been adsorbed, the solvent dissolves the components more or less
readily; depending upon the solubility and carries them along with it while moving on the support. If the pigments
are not soluble in water, solvents like hexane, toluene, acetone or a mixture of solvents such as methanol-water
can be used as mobile phase. For a given solvent or solvent mixture, at constant temperature, it is possible to
determine the characteristic rate of movement of each substance on the chromoto graphic paper, as the moving phase
moves. This is represented by relative front or
Second Year 119

retardation factor also called Rf value. Rf values of different compounds are different even if the mobile phase
(solvent) is same. Further more, Rf value of a compound may be different in different solvents. Rf values are
calculated by using the following equation.
Distance travelled by the substance from reference line (cm)
Rf =
Distance travelled by the solvent front from reference line (cm)
Since solvent front moves faster than the compounds, the Rf value of a substance will always be less
than one. Rf value has no unit. If the compounds are coloured, then their position on the chromatographic
paper may be easily located. However, if the compounds are colourless, they may be treated with a reagent,
which imparts characteristic colour to them. This reagent is given the name developer. Iodine is the most
commonly used developer in paper chromatography.
Materials required
Whatman's filter paper No.1, glass jar or 100 mL beaker, test tubes, flower extract or extract of
leaves, distilled water, methanol, acetone, chloroform.
Procedure
1. Grind flowers/leaves in a mortar and transfer the paste into a test tube. Add small amounts of
water, methanol or acetone to the crushed material. Shake well. Filter and collect the filtrate in a
test tube.
2. Cut Whatman's filter paper No.1 into a rectangular shape of 4 cm x 16 cm and mark a line 3 cm
from one of the ends of the filter paper with the help of a pencil (Fig.5.1(a)].
3. Using a capillary glass tube, put one spot 'A' with the flower extract. Allow the spot to dry.
4. Using a glass rod and cellotape, hang the filter paper in a jar containing water (or 19 mL petro-
leum ether, boiling range 60-80°C and lmL of chloroform or a mixture of petroleum ether, boiling
range 60-80°C and acetone in the ratio of 9:1), so that the solvent does not touch the reference line
as shown in fig.5.1(b)
5. Carefully observe the filter paper in the jar until the mobile phase (solvent) rises upto 2/3 of the
length of the paper (Fig. 5.1(c)].
6. Take the filter paper out, mark the solvent front, outline the spots with the help of a pencil and
allow the paper to dry.
7. Measure the distance of the solvent front and the centre of different spots with respect to the
reference line as shown in fig.5.1(d).
8. Find out the number of pigments present in the extract of flowers/leaves.
9. Calculate the Rf values of different spots as explained earlier.
10. Record your observations in a table.

Fig. 5.1: .
(a) Marked paper (b) Dipping the filter (c) Elution of components (d) Developed chromatogram
paper in the solvent in the extract
Table 5.1: Separation of pigments of flowers/ leaves
S.No. Name of the Colour of the Distance of Distance of the Rf value
flower/leaf spot the spot from solvent front
extract reference line from reference
(in cm) line (in cm)
1
2
3
Result : Rf values of components of flower / leaf are ——————

Precautions
1. Dip the filter paper in the solvent in such a way that the spot of the mixture should not touch the
solvent directly.
2. Do not allow the extract spots to spread. Use capillary glass tube to put the spot on the paper.
Experiment : 5.2
Separation of Ions Pb2+ and Cd2+ in a Mixture of Compounds Using Chromatographic
Technique
Aim : Separation of ions Pb2+ and Cd2+ in a mixture of compounds using chromatographic
technique.
Theory
Principle for the separation of cations is same as given in experiment 5.1. The two cations to
be separated are colourless, therefore, a developer is needed. In the present case, ammonium
Second Year 121
sulphide (NH4)2S, can be used to locate the position of these ions on chromatographic paper. (Ammonium
sulphide is prepared by passing H2S gas through 10% liquor ammonia solution in water for 45 minutes).
Materials required
Whatman's filter paper No.1, glass jar, test tubes, 1-2% solution of Pb(NO3)2 and Cd(NO3)2
ethanol, 6.0 M HNO3,
Procedure
1. Cut the Whatman's filter paper No.1 in a rectangular size of 4 cm x 16 cm and mark a line 3 cm from one
of the ends of the filter paper.
2. Using a capillary glass tube put a spot of the mixture on the marked reference line.
3. Using a glass rod and cellotape, hang the filter paper in a jar containing a mixture of ethanol, 6.0 M HNO3
and distilled water in the ratio of 8:1:1
4. Keep the jar undisturbed till the mobile phase (solvent) rises upto two thirds of the length of the paper.
5. Take the filter paper out from the jar and mark the solvent front.
6. Spray ammonium sulphide solution on the chromatographic paper to see yellow and black coloured
spots. Mark the position of the spots with a pencil and allow the filter paper to dry.
7. Measure the distance of the solvent front and the different spots of the cations with respect to the
reference line. Record the observations in a table. Calculate the Rf values for each cation (Pb2+
and Cd2+).
Table 5.2: Separation of Pb2+ and Cd2+ ions by paper chromatography
S.No. Name of the Colour of the Distance of Distance of the Rf value

flower/leaf spot the spot from solvent front
extract reference line from reference
(in cm) line (in cm)
1
2
Precautions
1. Dip the filter paper in the solvent in such a way that the spot of the mixture should not touch the solvent
directly.
2. Do not allow the extract spots to spread. Use capillary glass tube to put the spot on the paper.
1. How is adsorption phenomenon applied in the separation of components in a mixture by
chromatography?
2. What is the criteria of a developer?
3. What is a chromatogram?
4. What is meant by the term Rf value?
5. Name different chromatographic techniques.

CHAPTER- 6
PREPARATION OF
INORGANIC COMPOUNDS
Experiment : 6.1
Preparation of Ferrous Ammonium Sulphate (Mohr's Salt)
Aim: To prepare ferrous ammonium sulphate (Mohr's salt), a double salt.
Theory
When a mixture containing equimolar proportions of ferrous sulphate and ammonium
sulphate is crystallized from its solution, ferrous ammonium sulphate (Mohr's salt), a double salt is
formed. The reaction for the formation of ferrous ammonium sulphate (Mohr's salt) is given as
FeSO4 + (NH4)2 SO4 + 6H2O  FeSO4 (NH4)2 SO4. 6H2O
Ferrous ammonium sulphate
Fe2+ ions undergo hydrolysis. Therefore, while preparing aqueous solution of ferrous sulphate
in water, a few mL of dilute sulphuric acid is added to prevent the hydrolysis of the salt.
Beaker (250 mL), china dish, funnel, funnel stand, glass rod, wash bottle, tripod stand and wire
gauze.
Ferrous sulphate, ammonium sulphate, dilute sulphuric acid and ethyl alcohol
Procedure
(i) Take a 250 ml beaker. Put in it 5 g of ferrous sulphate, 2.5 g of ammonium sulphate, 0.5 mL of
dilute sulphuric acid and 15 mL of distilled water. Dissolve the salts by heating and stirring the
contents and filter the hot solution to remove undissolved impurities.
(ii) Transfer the filtrate to a china dish and heat the solution for sometime to concentrate to the
crystallisation point and allow the solution to cool to the room temperature slowly.
(iii) On cooling, light green crystals of ferrous ammonium sulphate separate out.
(iv) Decant off the mother liquor quickly and wash the crystals by shaking with very small amounts
of 1:1 cold water and alcohol mixture to remove any sulphuric acid sticking to the mother
liquor.
(v) Dry the crystals between the folds of a filter paper and record the yield.
Result
Yield of ferrous ammonium sulphate (Mohr's salt) is___________g.
Second Year 123

Precautions
(a) Cool the solution slowly to get good crystals. Avoid rapid cooling.
(b) Do not disturb the solution while it is being cooled.
(c) Do not heat the solution for long time while preparing crystals of ferrous ammonium sulphate, as
it may oxidise ferrous ions to ferric ions.
Experiment : 6.2
Preparation of Potash Alum
Aim: To prepare potash alum (K2SO4.Al2(SO4)3.24H2O).
Theory
When a mixture containing equimolar proportions of potassium sulphate and aluminium sul-
phate (hydrated) is crystallised from its solution, potash alum, a double salt is formed. The reaction for
the formation of potash alum is given as
K2SO4 + Al2 (SO4)3 18 H2O + 6H2O  K2SO4 A12 (SO4)3.24H2O
Potash alum
A13+ ions undergo hydrolysis. Therefore, while preparing aqueous solution of aluminium sul-
phate in water, a few drops of dilute sulphuric acid is added to water to prevent-the hydrolysis of the
salt.
Beaker (250 mL), china dish, funnel, funnel stand, glass rod, wash bottle, tripod stand and wire
gauze.
Potassium sulphate, aluminium sulphate, dilute sulphuric acid and ethyl alcohol
Procedure
(i) Take a 250 mL beaker. Put in it 6.5 g of aluminium sulphate, add 0.5 mL of dilute sulphuric acid
and 10 mL of distilled water. Dissolve 2.5 g of potassium sulphate in the solution by heating and
stirring the contents.
(ii) Transfer the mixture to a china dish and heat the solution for sometime to concentrate to the
crystallization point and allow the solution to cool to the room temperature slowly.
(iii) On cooling, the crystals of potash alum separate out.
(iv) Decant off the mother liquor quickly and wash the crystals by shaking with very small amounts
of 1:1 cold water and alcohol mixture to remove any sulphuric acid sticking to the mother liquor.
(v) Dry the crystals between the folds of a filter paper and record the yield.
Result
Yield of potash alum is ___________ g.
Precautions
(a) Cool the solution slowly to get good crystals. Avoid rapid cooling.
(b) Do not disturb the solution while it is being cooled.

Experiment : 6.3
Preparation of Potassium Trioxalatoferrate(III)
Aim: To prepare potassium trioxalatoferrate(III) (K3[Fe(C2O4)3]).
Theory
When hydrated ferric chloride is dissolved in aqueous solution of oxalic acid containing potas-
sium hydroxide, the complex potassium trioxalatoferrate(III) (K3[Fe(C2O4)3]) is formed. The reaction
takes place as follows.
FeCl3 + 6KOH + 3 H2C2O4  K3 (Fe (C2O4)3] + 3KCI + 6H2O
Beaker (250 mL), china dish, funnel, funnel stand, glass rod, wash bottle, water bath, tripod
stand and wire gauze.
Hydrated ferric chloride, oxalic acid, potassium hydroxide and ethyl alcohol
Procedure
(i) Prepare a solution of 3.0 g.of oxalic acid in 12.5 mL of hot water contained in a clean 50 ml
beaker.
(ii) To the above solution, add 3.8 g of potassium hydroxide gradually with stirring so that it dis-
solves completely.
(iii) Add 2.5 g of ferric chloride to the above solution with constant stirring till it is completely
dissolved.
(iv) Filter the solution and concentrate the green filtrate by heating in a porcelain dish over a water
bath and cool the mixture slowly.
(v) Filter the crystals so formed, wash with 1:1 mixture of cold water and alcohol and dry them by
pressing between the folds of a filter paper.
Result
Yield of potassium trioxalatoferrate (III) is________g.
Precautions
1. Do not concentrate the solution too much.
2. Weigh the desired quantities of different substances accurately.
3. Maintain the temperature of hot water around 40°C.
4. Add potassium hydroxide to oxalic acid solution in small lots.
5. The concentrated solution is allowed to cool slowly.
1. What is meant by equimolar proportions? Why do we take equimolar quantities of reacting
compounds in the preparation of ferrous ammonium sulphate?
2. In the preparation of ferrous ammonium sulphate, can we use concentrated sulphuric acid in-
stead of dilute sulphuric acid?
3. What is the difference between a double salt and a complex compound? Explain with examples.
Second Year 125

4. Why dilute sulphuric acid is added to the solution during the preparation of ferrous ammonium
sulphate?
5. What are the ions present in the aqueous solution of Mohr's salt?
6. Is potash alum a complex compound or a double salt?
7. In the preparation of potash alum, can we use concentrated sulphuric acid instead of dilute sulphuric
acid?
8. What is the nature of aqueous aluminium sulphate solution?
9. Why dilute sulphuric acid is added to the solution during the preparation of potash alum?
10. What are the ions present in the aqueous solution of potash alum?
11. Mention two uses of potash alum.
12. What is the oxidation state of Iron in K3 [Fe(C2O4)3] ?
13. What is the coordination number of Fe in K3[Fe(C2O4)3] ?
14. Does K3[Fe(C2O4)3] give tests for Fe3+ ions? If not, why?
15. What is the magnetic nature of K3[Fe(C2O4)3]?


CHAPTER- 7
PREPARATION OF
ORGANIC COMPOUNDS
Experiment : 7.1
Preparation of Acetanilide
Aim: To prepare acetanilide by the N-acetylation of aniline with acetic anhydride in the presence of
glacial acetic acid.
Theory
Acetanilide can be prepared by the acetylation of aniline with acetic anhydride.
Aniline Acetic anhydride Acetanilide Acetic acid
Apparatus
Beaker (250 mL), round bottomed flask (100 mL), funnel, air condenser, sand bath, stand, clamp
and pumice stone
Chemicals
Aniline (5 mL), acetic anhydride (5 mL), glacial acetic acid (5 mL)
Procedure
Take 5 mL of aniline in a round bottomed flask and add acetylating mixture containing 5 mL of
acetic anhydride and 5 mL of glacial acetic acid. Now, fit the air condenser to the mouth of the round
bottomed flask after adding a few pumice stones and reflux the mixture gently for 10-15 minutes on a
sand bath. Then cool the reaction mixture and pour these contents into a beaker containing 150-200
mL of ice cold water with stirring. Acetanilide would separate out as a white precipitate which could
be filtered and washed with cold water. Recrystallise a small amount of sample from hot water con-
taining a few drops of methanol or ethanol.
Report the yield of the compound.
Result
Yield of the sample of acetanilide is________g
Precautions
1. Handle acetic anhydride carefully as it may cause irritation to the eyes.
Second Year 127
2. Wash the solid 2-3 times with cold water till the filtrate is neutral to litmus.
3. Aniline is a toxic substance and may burn the skin. So it is to be carefully handled.
Preparation of Acetanilide (Alternate Method)
(Acetanilide is also prepared from aniline and acetyl chloride in the pyridine)
Aim: To prepare acetanilide.
Theory
Acetanilide can be prepared by the acetylation of aniline with acetyl chloride in the presence of
pyridine.
CH3 COCI
Pyridine
NH2 NHCOCH3
Aniline Acetanilide
Apparatus
Beaker (100 mL), water bath and funnel
Chemicals
Aniline (5 mL), acetyl chloride (5 mL) and pyridine (5 mL)
Procedure:
Take 5 mL of aniline and 5 mL of pyridine and mix them thoroughly. To this mixture add 5 mL of
acetyl chloride (1.0 mL at a time) in a beaker. If the beaker becomes very hot, cool it under tap water.
Then heat the mixture for five minutes in a boiling water bath. Cool the beaker and add about 10 mL
of ice cold water to the contents of the beaker with constant stirring. Acetanilide separates as white
precipitate, which can be filtered, washed and dried in the folds of filter paper.
Report the yield of the compound
Result
Yield of the sample of acetanilide is__________g
Precautions
1. If aniline is coloured, distill it before carrying out the experiment.
2. Use dry apparatus.
3. Do not inhale the vapours of acetyl chloride while adding.
4. Handle pyridine with extreme care.

Experiment : 7.2
Preparation of Dibenzalacetone
Aim: To prepare dibenzalacetone.
Theory : Dibenzalacetone is obtained when two moles of benzaldehyde condenses with one mole of acetone
in the presence of aqueous sodium hydroxide. This preparation is an example of Claisen-Schmidt reaction.
α -hydrogen atoms of aliphatic aldehydes and ketones are acidic in nature. Therefore in the presence of dilute
alkali aliphatic aldehyde or ketone condenses with an aromatic aldehyde to give α , β - unsaturated aldehyde
or ketone. The equation for the above reaction is given as
Acetone
Benzaldehyde Benzaldehyde Dibenzalacetone

Apparatus
Conical flask (250 mL), beaker (250 mL), funnel, filter papers and test tube
Chemicals : Benzaldehyde: 3.2 mL, 10% NaOH solution: 5.0 mL, acetone: 2.2 mL, rectified spirit: 25 mL
Procedure
1. Take 3.2 ml of benzaldehyde, 2.2 mL of acetone and 25 mL of rectified spirit (methylated
spirit) into a conical flask. Cork the flask and shake till a clear solution is obtained.
2. Take 5 mL of 10% NaOH solution in a test tube and add this to the above conical flask drop by
drop with shaking of the flask. During the addition of sodium hydroxide solution maintain the
temperature of the reaction mixture between 20-25°C by occasional cooling by placing the
flask in water bath.
3. Cork the flask again and shake vigorously for about 10 minutes releasing the pressure from
time to time.
4. Allow the flask to stand for 20 minutes at room temperature and then cool in the ice water for
a few minutes.
5. Filter the pale yellow solid thus obtained and wash with cold water to remove excess of alkali.
6. Dry it and recrystallise its small amount from ethanol or ethyl acetate.
7. Report the yield of the compound.
Result
Yield of the sample of dibenzalacetone is____________g
Precautions
1. Maintain the temperature around 20°C while shaking the reaction mixture.
2. Always use fresh solution of benzaldehyde.
Second Year 129

Experiment : 7.3
Preparation of Phenyl-azo-  -naphthol
Aim : To prepare phenyl-azo-  - naphthol (azo dye).

Theory
Aniline is an aromatic primary amine. It forms diazonium salt (Benzene diazonium chloride)
when treated with nitrous acid (HNO2) at 0-5°C. This process is called diazotization. Nitrous acid is
normally obtained instantly by the reaction between sodium nitrite and hydrochloric acid. The diazo-
nium salt is coupled with an alkaline solution of  -naphthol to form orange red azo dye which is phenyl-azo-
 -naphthol.
Benzene
Aniline diazonium chloride
Benzene
diazonium chloride  -naphthol
Phenyl-azo-  -naphthol
(orange red azo dye)
Apparatus
Beaker (250 mL), conical flask (100 mL), glass rod, thermometer, funnel and filter papers
Chemicals
Aniline (2 mL), conc. HC1 (6.5 mL), sodium nitrite (1.6 g),  -naphthol (3.2 g), sodium hydroxide
(2.0 g), glacial acetic acid (12 mL), ice and distilled water (as per need)
Procedure
Take 6.5 mL of conc. HCl in a beaker and dilute it with 6.5 mL of water and dissolve 2 mL of aniline
in it. Cool this mixture by placing the beaker in ice bath at 0-5°C. To this add the solution of sodium nitrite
prepared by dissolving 1.6 g of it in 8 mL of water and cooling the solution to less than 5°C. Dissolve 3.2 g of
 -naphthol in 18 mL of 10% sodium hydroxide solution. Add about 25 g of crushed ice to it. Stir  -
naphthol solution well and add chilled diazonium chloride solution very slowly to it with constant stirring. An
orange red dye of phenyl-azo-  - naphthol is formed. Keep the mixture in the bath for 30 minutes with
occasional shaking. Filter the crystals obtained and wash them well with cold water. Recrystallise about one
fourth of the crude product from glacial acetic acid. Dry the sample between the folds of filter paper.
Report the yield of the compound
Result : Yield of the sample of phenyl-azo- ß- naphthol is___________g
Note: Azo-dye synthesis is so nearly quantitative, that one should use amounts of the reactants closely
agreeing with stoichiometric equation and any excess of reactants may cause decomposition of
unused material and tar may appear.
Precautions
1. Maintain the temperature in the range of 0-5°C during diazotization.
2. Always add diazonium chloride solution to alkaline  - naphthol for dye formation.
3. Dry the recrystallised sample perfectly for determination of melting point.
1. Why is acetic anhydride preferred over acetyl chloride for acetylation reaction?
2. Is it necessary to recrystallise the compound obtained from the reaction? Explain why?
3. How is an organic compound recrystallised?
4. Which of the following compounds on diazotization followed by coupling with  - naphthol will form an
azodye?
(i) p-toulidine (ii) benzylamine (iii) N-methyl amine
5. Why is diazonium chloride usually soluble in water?
6. Why is aniline soluble in HCl and insoluble in H2O?
7. Why is aniline weaker base than ammonia?
8. In contrast to aromatic primary amines, aliphatic primary amines do not form stable diazonium salts.
Why?

Second Year 131

CHAPTER- 8
TESTS FOR FUNCTIONAL GROUPS IN
ORGANIC COMPOUNDS
Compounds containing only carbon and hydrogen are called hydrocarbons. The other organic
compounds are derived from hydrocarbons by replacement of one or more hydrogen atoms by other
groups such as -OH, -CHO, -COOH, =C=O, -NH2 etc. These are called functional groups. The
properties of the compounds largely depend on the functional groups. Different compounds having
same functional group have similar properties and are classified as same family. The compounds
having different functional groups have different properties and belong to different families of the
compounds. Qualitative analysis of organic compounds helps to . identify and characterize unknown
organic compound.
Some of the common functional groups are
Functional group Formula Class of compounds Example
1. Carboxylic group -COOH Carboxylic acids Acetic acid
(CH3 COOH)
2. Aldehydic group -CHO Aldehydes Acetaldehyde
(CH3CHO)
3. Ketonic group >C=0 Ketones Acetone (CH3)2 C=O
4. Alchoholic group R-OH Alcohols Ethyl alcohol (C2H5OH)
5. Phenolic group Ar-OH Phenols Phenol (C6H5OH)
6. Amino group -NH2 Amines Aniline (C6H5 NH2)
We study the systematic analysis of identification of functional group present in a given organic
compound. For this, we carry out the identification tests in the following order caboxylic (--- COOH),
aldehydic (--- CHO), ketonic (>C=O), alcoholic (R--- OH), phenolic (Ar--- OH) and amino (--- NH2)
functional groups.
Aim : To identify the functional groups present in an organic compound.
1. Physical State a. Solid May be aromatic acid.
b. Liquid May be alcohols, aldehydes,
ketones, aliphatic acids.
c. Liquid with pungent smell May be amine or phenol.
2. Ignition test
Take a small quantity of a. Burns with non-luminous May be aliphatic compound.
the given organic compound and non-sooty flame.
on a nickel spatula and b. Burns with luminous and May be aromatic compound.
burn it in the Bunsen flame. sooty flame.
3. Solubility in
a. Ether Soluble in ether. May be non - polar compound.
b. Cold water Soluble in cold water. May be polar organic com-

pounds like lower alcohols, car-
boxylic acids, aldehydes and ke-
tones.
c. NaOH solution Soluble in NaOH solution May be Cardboxylic (-COOH)

phenolic (Ar-OH) group.
d. NaHCO, solution Soluble in NaHCO3, solution May be carboxylic (-COOH)

with effervescence. group.
e. Dil. HCl Soluble in dil.HCI. May be amino (-NH2) group

4. Identification of
functional groups
(a) Test for carboxylic
group (-COOH)
Neutral ferric chloride test: Buff colour precipiteate is Carboxylic (-COOH) group may
Dissolve 0.1 g or 1 mL of the obtained. be present.
compound in water and add
2 drops of neutral ferric
chloride solution.
Confirmation test for

carboxylicgroup (-COOH)
Esterification
Take about 0.1 g or 1 mL of the com- Fruity smell is observed. The given compound contains
pound in a test tube and add 1 mL etha- carboxylic (-COOH) group.
nol and 2-3 drops of concentrated
sulphuric acid. Heat the reaction mix-
ture for 10-15 minutes in a hot water
bath at about 50°C. Pour the reaction
mixture in a beaker containing aque-
ous Na 2 ,CO 3 solution to
neutralize excess acid.
(b) Tests for aldehydic
(-CHO) and ketonic
(>C=O) functional groups
Second Year 133

2,4 - DNP test
Take 2-3 drops of the compound An orange red precipitate is May be carbonyl compound (Al-
in a test tube and add few drops of formed. dehydic (-CHO) or ketonic
an alcoholic solution of 2,4 (>C=O) functional group may be
dinitrophenyl hydrazine (2,4 present).
DNP) solution. Shake the mixture
and allow it to stand for 5 minutes.
Confirmation test for alidehydic

(-CHO) and ketonic (>C=O)
functional groups
Schiff’s test:
Take 2-3 drops of the given com- a. Pink colour is observed. (a). Aldehydic funtional group
pound and dissolve it in alcohol (-CHO) is confirmed.
and then add few drops of Schiff’s b. Pink colour is not ob- (b). Ketonic (>C=O) functional
reagent. served. group is confirmed.
(c) Identification test for alcohlic

group (R-OH)
Esterification
Take 2 mL of given organic com- Sweet smell or fruity smell Indicates the presence of alco-
pound in a clean dry test tube and is observed. holic group (R-OH).
add 1 ml of glacial acetic acid and
2-3 drops of concentrated
sulphuric acid. Heat the mixture
for 10-15 minutes in a hot water
bath at about 50Oc. Pour the reac-
tion mixture in a beaker contain-
ing aqueous sodicum carbonate
solution to remove excess of acid.
Confirmation test for alcoholic

group (R-OH)
Iodoform Test
Take 1 mL of the compound in a Yellow crystals of iodoform Confirms the presence of alco-
test tube and add 1 mL of 1% separate out. holic (R-OH) group.
iodine solution. Then add dilute
NaOH solution dropwise until the
brown colour is discharged. Warm
gently on a water bath.

(d) Identification test for phe-
nolic group(Ar-OH)
Neutral ferric chloride test
Take 2 mL of aqueous or alcoholic A violet colouration is The compound may contain phe-
solution of given organic com- produced. nolic group (Ar-OH).
pound and add few drops of neu-
tral ferric chloride solution
dropwise.
Confirmation test for phenolic

group (Ar-OH)
(Libermann Test)
Presence of phenolic group (Ar-
Place 2-3 crystals of sodium ni- A deep blue or a deep green
trate in a clean dry test tube and colouration is developed in OH) is confirmed.
add 0.5 g of given organic com- two minutes.
pound. Heat gently for half a
minute and allow it to cool. Then
add about 1mL of concentrated
sulphuric acid and shake the test
tube to mix the contents.
(e) Identification test for

aminogroup (-NH2)
Diazotization Test
Dissolve 5 drops of given organic A brilliant red dye is formed. Amino group (-NH2) may be
compound in 1 mL of HCI and present in the compound.
cool in ice. To this ice cold solu-
tion, add 1mL of 2.5% cold aque-
ous solution of NaNO2. In another
test tube dissolve 0.2g of.  -naph-
thol in dilute sodium hydroxide
solution. Add the solution pre-
pared in the first step to cold  -
naphthol solution slowly with shak-
ing.
Confirmation test for amino

group (-NH2)
Carbylamine test Foul smell or offensive odour This confirms the presence of
Take 2-3 mL of the compound in is observed. primary amino group (-NH2) in
a test tube. Then add 2-3 mL of the compound.
chloroform and equal amount of
alcoholic KOH solution. Heat the
contents gently.
Second Year 135
Note : As the solubility test is crucial for the identification of the functional group in a given organic
compound it may carried out in the following order :
If the given organic compound is
1. Soluble in ether, water, NaHCO3, (effervescence) and NaOH and insoluble in dil.HCl the compound
may be acidic, contain carboxylic (-COOH) group. Then, carry out the identification and confirmation
tests for carboxylic (-COOH) group. This ends your experiment. No need to proceed further.
2. Soluble in ether, water, insoluble in NaHCO3, (even if soluble, no effervescence), soluble in NaOH and
dil.HCl, the compound may be neutral and may contain aldehydic -CHO) or ketonic (>C=0) or alco-
holic (-OH) functional group.
(a) Carry out the identification test first for aldehydic and ketonic groups (carbonyl group) with
2,4 DNP. If orange coloured solution is formed, carry out the confirmation test with Schiff's
reagent and confirm either aldehydic (-CHO) or ketonic (>C=O) functional group. This ends
your experiment. No need to proceed further.
(b) If orange coloured solution is not formed with 2,4 DNP, it indicates the absence of carbonyl
group. Then, carry out the identification and confirmation tests for alcoholic (-OH) group.
This ends your experiment. No need to proceed further.
3. Soluble in ether, insoluble in water, insoluble in NaHCO3 (no effervescence), soluble in NaOH
and insoluble in dil.HCI, the compound may be weakly acidic and may contain phenolic (Ar-
OH) functional group. Then, carry out the identification and confirmation tests for phenolic (Ar-
OH) group. This ends your experiment. No need to proceed further.
4. Soluble in ether, insoluble in water, insoluble in NaHCO3(no effervescence), insoluble in NaOH
and soluble in dil.HC1, the compound may be basic and may contain amino (-NH2) group. Then,
carry out the identification and confirmation test for amino (-NH2) group.
Solubility Test Flow Chart Organic
Compound
Soluble Water Insoluble

test solution with pH paper
5% NaOH
Soluble 5% NaHCO3
Soluble/ insoluble/
5% NaHCO3 insoluble bubbles no bubbles
5% HCI carboxylic acid phenol
insoluble
solubel / insoluble/ soluble
bubbles no bubbles
amine conc.H2SO4
Soluble/colour insoluble/
carboxylic acid low mol, mass change no colour change
alcohol, aldehyde, alkene, alcohol, alkane, alkyl halide
ketone, amine aldehyde, ketone

Specimen record of identification of functional group in organic compound
(Example-1)
Aim : To identify and confim the functional group present in a given organic compound.
1. Physical state of the compound Liquid May be alcohol, aldehyde,
ketone, aliphatic acid.
2. Ignition test
A small quantity of the given Non-luminous and non-sooty May be aliphatic compound.
organic compound is taken on a flame is observed.
nickel spatula and burnt in the
Bunsen flame.
3. Solubility in
a. Ether Soluble in ether. May be non-polar compound.
b. Cold water Soluble in cold water. May be polar organic compound

like lower alcohol or carboxylic
acid or aldehyde or ketone.
c. NaOH solution Soluble in NaOH solution. Carboxylic (-COOH) or phe-

nolic (Ar-OH) group may be
present.
d. NaHCO3 solution Soluble in NaHCO3 solution Carboxylic (-COOH) group may

with effervescence. be present.
e. Dil.HCI Soluble in dil.HCI but not in May be Amino (-NH2) group and
water or basic solution. it may be aromatic amine.
As the compound produced
effervescence with NaHCO 3
solution, it may contain carboxy-
lic (-COOH) group.
4. Test for carboxylic group (-

COOH)
Neutral ferric chloride test

Carboxylic (-COOH) group may
0.1 g or mL of the compound is Buff colour precipitate is
be present.
dissolved in water and 2 drops obtained.
of neutral ferric chloride solution
is added.
Second Year 137

Confirmation test for carboxy-
lic group (-COOH)
Esterification
about 0.1 g or 1 mL of the com- Fruity smell is observed. Presence of carboxylic group
pound is taken in a test tube and (-COOH) is confirmed.
1 mL ethanol and 2-3 drops of
concentrated sulphuric acid are
added. The reaction mixture is
heated for 10-15 minutes in a hot
water bath at about 50Oc. The
reaction mixture is poured in a
beaker containing aqueous
Na2CO3 solution to neutralise
excess of acid.
Report : The given organic compound contains carboxylic (-COOH) functional group.
Specimen record of identification of functional group in organic compound
(Example-2)
Aim : To identify and confim the functional group present in a given organic compound.
1. Physical state of the compound Liquid with pungent smell. May be phenol or amine.
2. Ignition test
A small quantity of the given Luminous and sooty flame May be aromatic compound.
organic compound is taken on a observed.
nickel spatula and burnt in the
Bunsen flame.
3. Solubility in
a. Ether Soluble in ether. May be non-polar compound.
b. Cold water Insoluble in cold water. May be phenol or amine.
c. NaOH solution Insoluble in NaOH solution. Carboxylic (-COOH) and phe-

nolic (Ar-OH) group are obsent.
d. NaHCO3 solution Insoluble in NaHCO3 and Carboxylic (-COOH) group is

effervescence are not absent.
produced.

e. Dil. HCI Soluble in dil.HC1. Amino (-NH2) group may be
present.
As the compound is soluble in
dil.HCI, it contains amino (-NH2)
functional group.
4.Test for amino (-NH2) group
Diazotization Test
5 drops of given organic
compound is dissolved in 1 mL of A brilliant red dye is formed. Amino group (-NH2) may be
HC1 and cooled in ice. To this ice present in the compound.
cold solution, 1 mL of 2.5% cold
aqueous solution of NaNO 2 is
added. In another test tube 0.2 g of
 -naphthol is dissloved in
dilute sodium hydroxide solution. The
solution prepared in the first step is
added to cold  -naphthol solution
slowly with shaking.
Confirmation test for amino

(-NH2) group
Carbylamine test
2-3 mL of the compound is taken Foul smell or offensive odour The presence of primary amino
in a test tube. Then 2-3 mL of chlo- is observed. group (-NH2) in the compound
roform and equal amount of alco- is confimed.
holic KOH solution are added. The
contents are heated gently.
Report : The given organic compound contains amino (-NH2) functional group.
Precautions
1. All the tests are to be performed at room temperature
2. Always use freshly prepared neutral and very dilute solution of ferric chloride wherever
applicable.
3. Phenol is toxic and corrosive in nature and should be handled with care.
4. Do not heat the reaction mixture directly on a flame.
5. When doing sodium bicarbonate test, it should be added slowly so that effervescence is
visible clearly.
Second Year 139

6. Do not expose yourself to the vapours while performing carbylamine test because isocyanide is
highly poisonous. Destroy it immediately by adding concentrated hydrochloric acid and flush it
into the sink.
7. During diazotisation test maintain the temperature of the reaction mixture below 5°C as diazonium chlo-
ride is unstable at high temperature.
8. Always add diazonium chloride solution into the alkaline solution of  -naphthol and not vice-versa.
Preparations of reagents
1. Neutral ferric chloride solution: It is prepared by adding dilute sodium hydroxide solution to ferric
chloride solution drop by drop till a small but permanent brown precipitate appears. The solution is
filtered and the clear filtrate is used for the test.
2. Iodine solution: Dissolve 2 g of solid potassium iodide in about 40 mL water, add lg of solid iodine,
shake well and dilute to 100 mL.
3. 2,4- dinitrophenylhydrazine: Dissolve 1g of 2,4- Dinitrophenylhydrazine in 50 mL methanol to which
2 mL of concentrated sulphuric acid is added. Filter if necessary.
4. Schiff's reagent: Dissolve 0.1 g p-rosanaline hydrochloride in 100 mL water and pass sulphur dioxide
gas until its red colour is discharged. Filter and the filtrate is Schiff's reagent.
1. What is a functional group?
2. Why does phenol decolourize bromine water?
3. How do you distinguish between phenol and benzoic acid?
4. Name two tests which distinguish aldehydes from ketones.
5. What is esterification test ?
6. Why is alcohol dried before carrying out sodium metal test? \
7. What is Tollen's reagent?
8. What is the application of carbyl amine test?
9. Why is the solution of iodine prepared in potassium iodide and not in water?
10. How can methanol and ethanol be distinguished from each other chemically?
11. How do you distinguish between alcohol and phenol?
12. What is Schiff 's reagent?
13. How is nitrous acid prepared?
14. Name the reagent used to detect carbonyl group in a compound?


CHAPTER- 9
CHARACTERISTIC TESTS FOR
CARBOHYDRATES AND PROTEINS
9.1 Carbohydrates
Carbohydrates are optically active polyhydroxy aldehydes or polyhydroxy ketones or their de-
rivatives. They have the general formula CX(H2O)Y. They are classified into monosaccharides,
disaccharides, oligosaccharides and polysaccharides.
Monosaccharides
They are reducing sugars. They can reduce Tollen's reagent and Fehling's solution.
Ex: Glucose, fructose etc.
Oligosaccharides
They yield 2-10 monosaccharides on hydrolysis. They are non-reducing sugars.
Ex : Sucrose, maltose etc.
Polysaccharides
They contain more than 10 monosaccharide units. Their general formula is (C6H10O5)n
Ex: Starch, cellulose etc.
The carbohydrates perform two important functions.
a) They act as bio-fuels to provide energy for the functioning of living organisms.
b) They act as constituents of cell membrane.
9.2 Qualitative Tests for Carbohydrates

1. Conc. H2SO4 test : Take small Charring takes place, burnt Indicates the presence of
quantity of given compound then sugar smell is observed. carbohydrate.
add few drops of conc. H2SO4
and heat.
2. Molisch test : Take 1-2 mL of

aqueous solution of carbohy- A deep violet ring is formed Indicates the presence of
drate and add few drops of 10% at the junction of the two liq- carbohydrate.
alcoholic solution of alpha-naph- uids.
thol. Add conc. H2SO4 slowly
along the sides of the test tube.
Second Year 141

3. Benedict’s test : Take mL of Brick red precipitate is Presence of reducing sugar is
aqueous solution of carbohy- observed due to formation indicated.
drate in a test tube and add 1-2 Cu O
2
mL of Bendict’s reagent. Keep
the test tube in a boilling water
bath.
4. Tollen’s test : Take 1-2 mL of A shining silver mirror is Presence of reducing sugar is
aqueous solution of carbohy- observed. indicated.
drate in a test tube and add 2-3
mL of tollen’s reagent. Keep the
test tube in a boilling water bath
for about 10 minutes.
9.3 Proteins
Proteins are high molecular mass, long chain polymers composed of  -aminoacids. The linkage
between two amino acids is called peptide linkage. The product formed by the combination of two  -amino
acids is called dipeptide and with three amino acids is a tripeptide. A polypeptide contains large number of
 -amino acid molecules. A polypeptide having molecular mass greater than 10,000 is called protein. Pro-
teins are constituents of cells and hence are present in all living bodies. Some of the proteins act as enzymes
and catalyse the biochemical reactions. Most of the hormones which control various metabolic processes are
basically proteins. Some proteins act as antibodies and protect the body from the effect of invading sub-
stances.
9.4 Qualitative Tests for Proteins
1. Biuret test : Take about 2 mL of given
sample solution in a test tube and add about Bluish violet colouration is Indicates the presence
2 mL 10% NaOH solution to it. Then, add observed of protein.
4-5 drops of 2% CuSO4 solution to it.
2. Ninhydrin test : Take 2-3 mL of aqueous Blue coloration is observed. Protein is present.
solution of given sample in a test tube and
add 3-4 drops of Ninhydrin solution to it.
Then heat the solution.
3. Xanthoprotic test : Take about 2 mL of

given sample in a test tube and add few Yellow precipitate is Protein is present.
drops of conc. HNO 3. Then heat the observed.
solution.
Cool the yellow precipitate in a test tube

and add a few drops of 10 M sodium An orange colour appears. Protein is present.
hydroxide solution.

Note
1. Preparation of Ninhydrin solution: It is prepared by dissolving 0.1 g of Ninhydrin in about 100
mL of distilled water. This solution is unstable and can be kept only for 2 days.
2. As a source of protein, egg albumin or any of the pulses can be selected.
1. How do you distinguish between sucrose and glucose?
2. Why does fructose reduce Fehling's solution and Tollen's reagent though it has ketonic group.
3. What is silver mirror?
4. How are proteins affected by heat?
5. What is Molisch's reagent?
6. What are the final products of hydrolysis of proteins?
7. What is a peptide linkage?
8. What is the name given to the reaction between protein and concentrated HNO3?
9. Why do we get red precipitate in Fehling's test?

Second Year 143

CHAPTER- 10
QUANTITATIVE ESTIMATION
(REDOX REACTIONS)
Experiment : 10.1
Determination of the Strength of Potassium Permanganate
Aim: Determination of the strength of potassium permanganate (KMnO4) solution using
0.05 M standard oxalic acid solution.
Principle
Potassium permanganate in its aqueous solution and in acid medium is a strong oxidizing agent.
Note that it can also act as oxidizing agent even in basic medium, but in quantitative analysis we use
it mostly in acidic medium.
MnO4- + 8H+ +5e- Mn2+ + 4H20
For maintaining acidic medium dilute sulphuric acid has to be used not nitric acid as it itself is an
oxidizing agent and not even hydrochloric acid as it reacts with KMnO, as follows.
2KMnO4 + 16 HC1  2KCI + 2MnCl2 + 5C12 + 8H20
Oxalic acid, a reducing agent can be titrated against Kmno4 solution. The overall redox reaction may be
shown as follows.
Molecular equations
(a) 2KMnO4+3H2SO4  K2SO4 +2 MnSO4+3H2O+5(O) (reduction half reaction)
70-80OC
(b) [H2C2O4 + (O)  2CO2 + H2O] x5 (oxidation half reaction)
The overall reaction of (a)+(b) is
2KMnO4 + 3H2SO4 + 5 H2C204  K2SO4 + 2MnSO4 + 8H20 + 10CO2
If we write ionic reaction, it is as follows
(a) [Mno-4 + 8H+ + 5e- Mn2++4H20] x 2 (reduction half reaction)
(b) [C2O42-  2CO2 + 2e-] x 5 (oxidation half reaction)
Overall reaction [ (a) + (b)] is 2MnO4 + 5C2O42- +16H+  2Mn2++10CO2+8H20
Here MnO4- is reduced to Mn2+ and C2O42- is oxidized to CO2.
In the titration involving permanganate, the permanganate itself acts as self indicator. As far as
oxalic acid is present in the solution it reduces the added coloured MnO4- to colourless Mn2+. Once the
oxalic acid is completely consumed, the extra added drop of MnO-4, retains the

colour of MnO-4 which imparts pale pink colour to the solution. As the reaction between oxalic acid
(or oxalate if Na2C2O4 is used) and KMnO4 is very slow at room temperature, the reaction is carried
out at about 70°C in the presence of dilute H2SO4. The reaction between MnO4-1 and C2O42- is an
autocatalysis process. The Mn2+ so formed acts as catalyst. The reaction therefore is very slow in the
beginning. Therefore in the beginning of the titration KMnO4 solution from the burette is added drop
wise slowly to get sufficient number of Mn2+ which acts as catalyst.
Burette (50 mL) Potassium permanganate solution
Pipette (20 mL) (approximately 0.02 M)
Conical flask (100 mL or 250 mL) Oxalic acid solution (0.05 M)
Funnel Dilute H2SO4 (2 M)
Burette stand
Weighing bottle
White glazed tile
Bunsen burner
Wire gauge
Analytical balance with weight box and fractional weight box with rider and forceps.
Procedure
PART 1
Preparation of 0.05 M oxalic acid or sodium oxalate solution by weighing
Molar mass of oxalic acid is (COOH)2.2H20 is 126 g mol-1 and that of sodium oxalate
(COONa)2 is 134 g mol-1
Suppose that we have to prepare 250 mL of 0.05 M oxalic acid solution, then
250
the amount of oxalic acid to be weighed is (w) = 0.05   126 = 1.575 g
1000
If the solute is Na2C2O4 the amount to be weighed is
250
W = 0.05   134 = 1.675 g
1000
Prepare the above solution as per the procedure given already.
PART 2
Titration of oxalic acid solution against potassium permanganate solution
(a) Fill the burette upto zero mark without any air bubbles even in the nozzle after washing and
rinsing it with the given approximately 0.02 M KMnO4 solution.
(b) Take 20 mL of 0.05 M oxalic acid or sodium oxalate solution with clean washed and rinsed pipette and put
it in a clean 100 mL or 250 mL conical flask. Add to this solution about 1/2 test tube full of dilute H2 SO4
given. Heat the oxalic acid solution to about 60-80°C (until you get first bubbles that come before the
liquid starts boiling). Titrate the hot solution against KMnO4 solution using a white glazed tile below the
Second Year 145

conical flask. After reaching the equivalence point if one drop excess of permanganate solution
is added the solution attains permanent light pink colour.
(c). Repeat the experiment to have atleast two consecutive / concurrent burette readings are obtained
(i.e., atleast two successive readings constant).
(d). Record the readings in the table.
Table 10.1: Titration of oxalic acid solution against KMnO4 solution
Sl.No. Volume of oxalic acid Burette readings Volume of KMnO4 run
solution (V1 mL) Initial (V1 mL) Final (Vf mL) down (Vf-Vi)=V2 mL
1. 20.0
2. 20.0
3. 20.0
4. 20.0
Calculations
The strength of KMnO4 solution in terms of molarity may be calculated as follows.
Molarity of oxalic acid solution = M1 = 0.05 M
Volume of oxalic acid solution = V1 = 20.0 mL
(Do not take the volume of H2SO4 added into consideration)
Number of moles of oxalic acid = n1=5
(this is also the number of electrons gained by MnO-4 per formula unit in the stoichiometric
equation.)
Volume of KMnO4 solution run down = V2 = (Vf-Vi) = from experiment
Number of moles of KMnO4 = n2 = 2 (this is number of electrons lost by oxalic acid per formula
unit in the stoichiometric equation).
Molarity of KMnO, solution = M2 = ?
M1V1 M 2 V2 MV n
= ;M 2 = 1 1  2
n1 n2 n1 v2
M2 the molarity of KMnO4 solution may be calculated
Amount of KMnO, per litre of solution = M2 × molar mass of KMnO4
= M2 mol L-1 x 158 g mol-1
= M2 × 158 g L-1
If the strength of KMnO4 is to be calculated per 250 mL of the solution then it is given by
M2158 g L-1 × 250 mL
=g
1000
Result : Molarity of KMnO4 solution is___________
Amount of KMnO4 present in one litre of the solution is___________

Experiment : 10.2
Estimation of Potassium Permanganate
Aim: To find the strength of potassium permanganate (KMnO4) solution by titrating it against standard fer-
rous ammonium sulphate (Mohr's salt, FeSO4(NH4)2SO4.6H2O) solution.
Principle
Ferrous ammonium sulphate is a reducing agent through Fe2+ in the titration against KMnO4, solution.
Fe changes to Fe3+ and Mno-4 changes to Mn2+ during the redox chemical change. The reaction takes place
2+
at higher even at room temperature. Therefore, no heating is required.

Chemical equation for the reaction
Molecular reaction
2 FeSO4 (NH4)2SO4 6H2O  2FeSO4 + 2(NH4)2 SO4 + 12 H2O
[2FeSO4 + H2SO4+(O) Fe2(SO4)3 + H2O] 5 (oxidation half reaction)
2KMnO4 + 3H2SO4 K2SO4 + 2MnSO4 + 3H2O + 5(O) (reduction half reaction)
Overall molecular redox reaction
10 FeSO4 + 2KMnO4 + 8H28O4 —5Fe2(SO4)3 + 2MnSO4 + K2SO4, + 8H20
Ionic reaction
MnO4- + 8H+ + 5e-  Mn2+ + 4H20 (reduction half reaction)
[Fe2+  + Fe3+ + e-] × 5 (oxidation half reaction)
MnO4 + 5Fe + 8H Mn + 5Fe + 4H2O (overall redox reaction)
2+ + 2+ 3+

Same as given under oxalic acid versus KMnO4 but instead of oxalic acid, ferrous ammonium sulphate
solution is to be taken.
Procedure
PART 1
Preparation of 250 ml of ferrous ammonium sulphate hexahydrate (Mohr's salt FeSO4 (NH4)2SO4,
6H2O) of 0.1 M concentration. Amount of the Mohr's salt required is (molar mass 392 g mol-1)
250mL
W = M × vol. of solutionx molar mass = 0.1mol L-1× ×392 g mol-1
1000mL L
= 9.8 g
PART 2
(a) Wash and rinse the burette and fill it with the given (approximately 0.02 M) KMnO4 solution
without air bubbles in the solution including nozzle upto the mark. Note the burette reading (V1
mL).
(b) Take 20 mL of ferrous ammonium sulphate solution with a washed and rinsed pipette and put it
in a clean, washed (don't rinse) conical flask. Add to it 1/2 test tube full of the given 2 M dilute H2 SO4
Second Year 147

(c) Titrate the acidified ferrous ammonium sulphate solution (b) against the permanganate solution
(a) until the solution in the conical flask attains permanent light pink colour. Note down the
volume of KMnO4 solution rundown (Vf mL).
(d) Repeat the experiment to get two concument burette readings of i.e., two successive constant burette
readings.
(e) Record the readings in the table.
Table 10.2: Titration of KMnO4 solution against standard Mohr's salt solution
Sl.No. Volume of ferrous Burette readings Volume of KMnO4 run
ammonium sulphate solution run down in
solution used in each Initial (V1 mL) Final (Vf mL) each experiment
titration (V1mL) V2 = (Vf - Vi) mL
1. 20.0
2. 20.0
3. 20.0
4. 20.0
Calculations
Molarity of ferrous ammonium sulphate solution (M1) = 0.1 M
Number of moles of Feso, in the stoichiometric equation (n1) = 10
Volume of Feso4 solution in acidic medium (V1) = 20.0 mL
Volume of KMnO4 solution run down (V2) = (Vf-Vi) mL = (From the Table)
Number of moles of KMnO4 in the stoichiometric equation (n2) =2
Molarity of KMnO4 solution (M2) = ?
M1V1 M 2 V2 MV n
= ;M 2 = 1 1  2
n1 n2 n1 v2
Amount of KMnO4 per litre of solution = M2× molar mass of KMnO4

Result: The amount of KMnO4 present per litre of solution = M2×158gmol-1 = gL-1
10.3 Precautions During Titrimetic Analysis
PART 1
Weighing
1. The pans of the balance should be clean and the balance should be properly adjusted for equal
oscillations of the pointer on both sides of the ivory plate on its release. The side doors should
only be opened and closed during weighing.
2. Substances should be weighed with the weights including fractional weights with forceps.
Substances should not be spilled on the pans of the balance.
3. For colourless solution the lower meniscus should coincide with the marking. The solution should
be thoroughly mixed to have uniform concentration.
PART 2
1. Always wash and rinse the burette and pipette with the respective solution, which are to be taken
in them in the beginning but never rinse the conical flask. Why it should not be rinsed?
2. All readings should be taken without parallax error.
3. For colourless transparent the lower meniscus must coincide with the marking but for coloured
non transparent solutions the upper meniscus must coincide with the marking.
4. See that no air gaps are present in the solution of burette.
5. Don't blow the last drop of the solution in the pipette from its nozzle.

Second Year 149

CHAPTER-11
QUALITATIVE INORGANIC ANALYSIS
In qualitative analysis, a given compound is tested for the nature of the constituents of the
compound. In the present context. We analyse a simple salt for the cation and anion present in it. A
simple salt is a salt containing generally one cation and one anion only. On the other hand a mixture of
salts contains more than one cation and one anion. So to carry out the analysis for identification of cation and
anion present in a given simple salt, a systematic procedure is to be adopted. Thus, the analysis is called
systematic qualitative analysis.
The systematic qualitative analysis of a simple salt (inorganic salt) involves physical examina-
tion of the salt, anion analysis and cation analysis. Thus, the simple salt analysis involves the follow-
ing steps.
1. Preliminary tests: Observation of the physical characteristics like colour, odour and physical
state of the salt, dry heating test (action of heat) followed by flame colour test, charcoal cavity
test/cobalt nitrate test and borax bead test come under preliminary test. These preliminary tests
give an insight into the anion and cation present in the given simple salt.
2. Analysis of anion: An inorganic salt is formed by neutralization of an acid and a base. Thus, the
part of the salt contributed by acid is referred to as acid radical or anion, which generally carry
negative charge. For analysis of anion, carry out test with dilute hydrochloric acid (dil.HCl) or
dilute sulphuric acid (dil.H2SO4) for carbonates and acetates followed by test with conc. sulphuric
acid (conc.H2SO4) for halides and nitrate and finally test with barium chloride solution (BaCl2)
for sulphate. This is followed by wet tests for confirmation of the anion (Refer to wet tests for
confirmation of anions with sodium carbonate extract is discussed in chapter-7 of first year
practicals).
3. Analysis of cation: An inorganic salt is formed by neutralization of an acid and a base. Thus, the
part of the salt contributed by base is referred to as basic radical or cation, which generally
carries positive charge. For analysis of cation, the preliminary examination gives an indication
of the cation present in the salt and wet tests are to be carried out in solution group wise for
identification and confirmation of the cation. The preliminary examination of the given salt like
colour, action of heat (dry heating test) and flame colour test gives us an indication of the cation
present in the given salt. The confirmation tests for cation are to be carried out using the original
solution of the salt. So the first step in the analysis of cation is to prepare the original solution.
Preparation of original solution

Depending upon the solubility of the salt, the original solution is prepared using suitable sol-
vent in which it is soluble. The following solvents are tried one after the other in systematic order. If
the salt does not dissolve in a particular solvent even on heating, try the next solvent in the order.
However, we have at Intermediate level water soluble salts only.
(i) Distilled water (cold and hot)
(ii) Dilute HCl (cold and hot)
(iii) Conc.HCl (cold and hot)
Take a small quantity of salt in a boiling tube and add suitable solvent. Shake well till the salt
dissolves completely to form a clear and transparent solution. This is called original solution and is
used for performing confirmatory tests.
For the systematic identification, the cations are classified into the following groups. Each
group of cation has suitable reagent(s) called group reagent. The cations present in respective groups,
group reagents and the details of precipitates formed in each group due to the reactions between
cations and the group reagents is given in a table called Group Separation Table.
Group Separation Table for cations
Group Colour of the Precipitate

Cations Group reagent
Precipitate
Group I Pb2+ Dil.HCl White PbCl2
Group II Pb2+ Black PbS

Dil.HCl + H2S
Cu2+ Black CuS
Al3+ White Al(OH)3
Group III Fe2+ NH4Cl+NH4OH Light green Fe(OH)2
Fe3+ Brown Fe(OH)3
Zn2+ White Zns
Group IV Mn2+ Flesh colour MnS
NH4Cl+NH4OH + H2S
Co2+ Black CoS
Ni2+ Black NiS
Ba2+ White BaCO3

Ca2+ NH4Cl+NH4OH + (NH4)2CO3 White CaCO3
Group V
Sr2+ White SrCO3
Group VI Mg2+ No specific group reagent ----- -----
Generally NH4+ tests have to be performed ater confirming that no cations from group I to V
are present. But, we use several times NH4+ compounds as reagents which may interfere at the end
and give positive tests for NH4+ though it is not NH4+ salt. To avoid this, it may be advised to perform
tests of NH4+ before starting the group separation.
Second Year 151

Systematic qualitative analysis of simple salt
(i) Preliminary tests
1. Colour: Observe the colour (i) Blue (or bluish green May be cupric (Cu2+) salt.
of the salt. (ii) Light green May be ferrous (Fe2+) salt.
(iii) Light pink (buff colour) May be manganese (Mn2+)
(iv) Greenish May be nickel (Ni2+) salt
(v) Pink May be cobalt (Co+2) salts
(vi) White or colourless Absence of Cu2+, Fe2+, Mn2+,
Ni2+, Co2+ cobalt salts.
2. Physical state: Observe the (i) Crystalline

-
physical state of the salt. (ii) Amorphous (Soft to touch)
3. Action of heat (Dry heat- (i) White sublimate is formed.

ing test) : Take a pinch of (ii) Colourless gas with the May be ammonium (NH4+) salt.
solid salt in a dry test tube smell of ammonia is May be ammonium (NH4+) salt.
and heat it strongly. evolved.
(iii) Reddish brown vapours
are evolved. May be nitrate (NO3-) salt.
(iv) Crackling sound is ob
served. May be lead (Pb2+) salt.
(v) Water drops are formed
along the inner walls of May be hydrated salt.
the test tube (loss of water
of crystalliztion)
(vi) Yellow when hot and
white when cold. May be zinc (Zn2+) salt.
(vii) Characteristic vinegar
like smell. May be acetate (CH3COO-) salt.
(viii) Blue salt becomes white
(colour - less) on heating. May be hydrated copper (Cu2+)
salt.
4. Flame test: Take small (i) Blue (or) Bluish green flame
amount of solid salt into a (ii) Brick red flame May be copper (Cu2+) salt.
watch glass and add a few (iii) Grassy green flame May be calcium (Ca2+) salt.
drops of conc.HCl to it and (iv) Crimson red flame May be barium (Ba2+) salt.
prepare a paste. Introduce (v) Green flashes May be strontium (Sr2+) salt.
this paste into the blue flame May be zinc (Zn2+) salt.
with platinum loop wire.
Observe the characterstic
(ii) Analysis of anion
1. Test with dil.HCl: Take a (i) Colourless and odourless Carbonate (CO32-) ion may be
small quantity of the salt in a gas of carbondioxide is present.
test tube and add dil.HCl. evolved with brisk
effervescence which puts
out the burning splinter and
turns lime water milky.
(ii) Colourless vapours of Acetate (CH3COO-) ion may be
acetic acid with vinegar present.
smell are evolved which
turns blue litmus red.
(iii) No characteristic reaction CO32- and CH3COO- ions are
(No gas is evolved) absent.
Confirmatory tests for car- A white precipitate of barium Carbonate (CO 3 2- ) ion is
bonate ion (CO32-): carbonate is formed. confirmed.
Take a small quantity of the salt
solution (or water extract of the
salt) in a test tube and add
barium chloride (BaCl 2 )
solution.
Solubility of the above ppt. is The precipitate is soluble in Carbonate (CO 3 2- ) ion is
tested in dil.HCl. dil.HCl confirmed.
Confirmatory tests for acetate

ion (CH 3COO-):
(i) Take a small quantity of the Deep red colour solution is Acetate (CH 3 COO -) ion is
salt solution (or water ex- formed. confirmed.
tract of the salt) in a test
tube and add neutral ferric
chloride (FeCl3) solution.
Boil the above solution in Reddish brown precipitate is Acetate (CH 3 COO -) ion is
water bath. formed. confirmed.
(ii) Esterification: Take a Pleasant fruity odour of the Acetate (CH 3 COO -) ion is
small quantity of the salt in ester, ethyl acetate is observed. confirmed.
a test tube and add ethyl
alcohol and conc.H2SO4. Heat
the contents and pour into a
beaker containing water.
Second Year 153
2. Test with conc.H 2SO 4 : (i) Colourless gas with pungent Chloride (Cl - ) ion may be
Take a small quantity of the smell (HCl) is evolved present.
salt in a test tube and add which fumes in moist air
conc.H2SO4. and produces white dense
fumes when a glas rod
dipped in ammonium hy-
droxide is placed at the
mouth of the test tube.
(ii) Reddish brown vapours Bromide (Br -) ion may be
with pungent smell (Br2) present.
are evolved which turns
starch paper yellow.
(iii) Violet vapours of I2 are Iodide (I-) ion may be present.
evolved which turns starch
paper blue.
(iv) No characteristic reaction Halides (Cl-, Br- and I-) are ab-
(No gas is evolved). sent.
Confirmatory tests for chlo-
ride ion (Cl):
(i) Test with MnO 2 and
conc.conc.H2SO4 :
Take a small quantity of the Greenish yellow gas of chlorine Chloride (Cl-) ion is confirmed.
salt in a test tube add man- with pungent smell is evolved
ganese dioxide(MnO2) and which turns moist starch-iodide
conc.H2SO4 and heat. paper blue.
(ii) Take salt solution acidify A white curdy precipitate of sil- Chloride (Cl-) ion is confirmed.
with di.HNO3 and add silver ver chloride is formed which is
nitrate (AgNO3) solution. soluble in ammonium hydrox-
ide (NH4OH)
Confirmatory tests for
bromide ion (Br-):
(i) Test with MnO 2 and
conc.H2SO4:
Take a small quantity of the
salt in test tube add manga- Reddish brown vapours of bro- Bromide (Br-) ion is confirmed.
nese dioxide (MnO2) and mine (Br2) with pungent smell
conc.H2SO4 and heat. are evolved which turns starch
(ii) Take salt solution acidify paper yellow.
with dil.HNO3 and add sil- Pale yellow precipitate of silver Bromide (Br-) ion is confirmed.
bromide is formed which is par-
ver nitrate (AgNO3) solution.
tially soluble in ammonium hy-
droxide (NH4OH)
Confirmatory tests for iodide
ions (I-) :
(i) Test with MnO2 and
conc.H2SO4 :
Take a small quantity of the Deep violet vapours of iodine Iodide (I-) ion is confirmed.
salt in a test tube add man- are evolved which turns starch
ganese dioxide (MnO2) and paper blue.
conc.H2SO4 and heat.
(ii)Take salt solution, acidify An yellow precipitate of silver Iodide (I-) ion is confirmed.
with dil.HNO3 and add sil- iodide is formed which is in-
ver nitrate (AgNO3) soluble in ammonium hydrox-
ide (NH4OH).
3. (i) Test with conc.H2SO 4

(hot condition) : Take small Reddish brown vapours of NO2 Nitrate (NO 3 -) ion may be
quantity of the salt in a test tube are evolved. present.
and add conc.H2SO4 and heat.
(ii) Test with copper turnings (i) Deep reddish brown vapours Nitrate (NO 3 -) ion may be
and conc.H2SO4 : Take a small of NO2 are evolved and the so- present.
quantity of the salt in a test tube lution turns pale blue.
and add a few copper turnings and
add conc.H 2 SO 4 and heat (ii) No characteristic reaction Nitrate (NO3-) ion is absent
strongly. (No reddish brown gas is
evolved).
Confirmatory test for nitrate
ion (NO-3) : (Brown ring test):
Take the salt solution in a test A dark brown ring is formed at Nitrate (NO3-) ion is confirmed.
tube and add freshly prepared the junction of the two layers.
ferrous sulphate solution in ex- (acid and solution layers).
cess. To this conc.sulphuric acid
(conc.H2SO4) is added slowly
along the sides of the test tube
keeping the test tube in an in-
clined position.
4. Test for sulphate ion (SO42-) White crystalline precipitate of Sulphate (SO42-) ion is present.
To the salt solution add barium barium sulphate (BaSO 4) is
chloride (BaCl2) solution. formed.
The solubility of the precipitate
is tested in conc.HCl The precipitate is insoluble in Sulphate (SO42-) ion is present.
conc.HCl
Second Year 155
(iii) Analysis of cation
Analysis of ammonium ion (i) Colurless gas with Ammonium ion (NH 4 + ) is
(NH4+) characteritic ammonia present.
Take a small quantity of salt in smell is evolved, which
a test tube, add sodium hydrox- gives white dense fumes
ide (NaOH) solution and heat. when a glass rod dipped in
conc.HCl is brought near
the mouth of the test tube.
(ii) Ammonia gas is not Ammonium ion (NH4+) is
evolved. absent.
Confirmatory test for

ammonium ion (NH4+)
To the salt solution add Reddish brown precipitate is Ammonium ion (NH4+) is con-
Nessler’s reagent (alternatively formed. firmed.
pass the above gas into
Nessler’s reagent).
Preparation of original
solution
The salt is dissolved in a suit- Clear and transparent solution Name it as original solution.
able solvent (distilled water or is formed.
dil.HCl).
Analysis of Group-I
To the original solution (i) White precipitate is formed. Group-I is present (Pb 2+ is
(O.S) add dil.HCl present).
(O.S. + dil.HCl) (ii) No white precipitate is Group-I is absent.
formed.
Confirmatory tests for lead

ion (Pb2+)
Dissolve the above precipitate
in hot water and divide it into
two parts.
1. To one part add potassium Yellow precipitate formed Pb2+ is confirmed.

chromate (K2CrO4) solution. which dissolves in NaOH
solution.

2. To the second part add Yellow precipitate is formed Pb2+ is confirmed.
potassium iodide (KI) solution. which dissolved in hot water
and on cooling the solution,
golden spangles are formed.
Analysis of Group-II
To the original solution add (i) Black precipitate is formed. Group-II is present (Cu 2+ is
dil.HCl and pass H2S gas. present)
(O.S + dil.HCl +H2S) (ii) No black precipitate is Group-II is absent.

formed.
Confirmatory tests for copper

ion (Cu2+)
1. To the original solution A chocolate brown coloured Cu2+ is confirmed.
add potassium ferrocya precipitate is formed.
nide K4[Fe(CN)6]
solution.
2. To the original solution A pale blue precipitate is Cu2+ is confirmed.
add NH4OH. formed which is soluble in
excess of NH4OH.
Analysis of Group-II
To the original solution add (i) White gelatinous precipitate Group-III is present (Al 3 is
solid NH 4Cl and excess of is formed. present)
NH4OH (ii) Light green (dirty green) Group-III is present (Fe2+ is
(O.S. + NH4Cl + NH4OH). precipitate is formed. present)
(iii) No precipitate is formed. Group-III is absent
Confirmatory tests for alu-

minium ion (Al3+)
1. To the original solution White gelatinous precipitate is Al3+ is confirmed.
add NaOH solution. formed which is soluble in ex-
2. To the original solution cess of NaOH.
add NH4OH. White gelatinous precipitate is Al3+ is confirmed.
formed.
Confirmatory tests for fer-
rous ion(Fe2+)
1. To the original solution Dirty green precipitate is Fe2+ is confirmed.

add NH4OH. formed which is soluble indilute
acid.
Second Year 157
2. To the original solution add A white precipitate is formed Fe2+ is confirmed.
potassium ferrocyanide which turns light blue due to
K4(Fe(CN)6) solution. aerial oxidation.
Analysis of Group-IV
To the original solution add (i) White precipitate is formed. Group-IV is present (Zn2+ is
solid NH4Cl and excess of present)
NH4OH and pass H2S gas (ii) Flesh coloured (buff Mn2+ is present.
(O.S. + NH4Cl + NH4OH + coloured) precipitate is
H2S). formed.
(iii) Black precipitate is formed. Ni2+ is present.
(iv) No precipitate is formed. Group-IV is absent.

Confirmatory tests for zinc
ion (Zn2+)
1. To the original solution add
NaOH solution. White precipitate is formed Zn2+ is confirmed.
which is soluble in excess of
2. To the original solution add NaOH solution.
potassium ferrocyanide A bluish white precipitate is Zn2+ is confirmed.
K4[Fe(CN)6] solution. formed.
Confirmatory tests for man-

ganese ion (Mn+2)
1. To the original solution add White precipitate is formed which
NaOH solution. turns brown on exposure to air Mn2+ is confirmed.
and the precipitate is insoluble
in excess of NaOH solution.
2. To the original solution add White precipitate is formed which

NH4OH. is soluble in excess of NH4OH. Mn2+ is confirmed.
Confirmatory tests for nickel

(Ni2+) A bright red rose coloured pre-
1. To the original solution add cipitate is formed.
ammonium hydroxide and a Ni2+ is confirmed.
few drops of dimethyl
glyoxime (CH3CNOH)2 so-
lution.
2. To the original solution add A black precipitate is formed. Ni2+ is confirmed.
sodium hydroxide solution in
excess and bromine water.
Analysis of Group-V
To the original solution add (i) White precipitate is formed. Group-V is present (Ba2+ or Ca2+
solid NH 4Cl excess of or Sr2+ is present).
NH 4 OH and (NH 4 ) 2 CO 3
solution.
(O.S. + NH4Cl + NH4OH + (ii) No white precipitate is formed Group-V is absent.

(NH4)2CO3) which is soluble in conc.HCl

barium ion (Ba2+)
1. to the original solution add Yellow precipitate is formed which Ba2+ is confirmed.
potassium chromate is soluble in conc.HCl.
(K2CrO4) solution.
2. To the original solution add White precipitate is formed which Ba2+ is confirmed.
ammonium oxalate is soluble in acetic acid.
((NH4)2C2O4) solution.
3. Flame test: Take a platinum A grassy green colour flame is ob- Ba2+ is confirmed.
wire and dip it in conc.HCl. served.
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 group-V precipitate or
original salt in conc.HCl.
Heat it in the flame.
Confirmatory tests for cal-

cium ion (Ca+2)
1. To the original solution add No precipitate is formed. Yellow Ca2+ is confirmed.
potassium chromate coloured solution is obtained.
(K2CrO4) solution.
2. To the original solution add White precipitate is formed which Ca2+ is confirmed.
ammonium oxalate is insoluble in acetic acid.
((NH4)2C2O4).
3. Flame test: Perform the A brick red colour flame is ob- Ca2+ is confirmed.
flame test as given for Ba2+ served.
Second Year 159

Confirmatory test for
strontium ion (Sr2+)
1. To the original solution add
ammonium sulphate White precipitate is formed. Sr2+ is confirmed.
((NH 4) 2SO 4) solution and
warm. Scratch the inner sides
of the test tube with a glass
rod.
A crimson red colour flame is Sr is confirmed.
2+
2. Flame test: Perform the
flame test as given for Ba2+. observed.
Analysis of Group-VI
To the original solution add White crystalline precipitate is Group-VI is present (Mg2+ is
solid NH4Cl excess and NH4OH formed which is soluble in present)
and disodium hydrogen phos- dilute mineral acids and acetic
phate solution (Na2HPO4) and acid.
scratch the inner sides of the test
tube with a glass rod (O.S. +
NH4Cl + NH4OH + Na2HPO4).
Confirmatory test for magne-

sium ion (Mg2+)
1. To the original solution add White precipitate is formed Mg2+ is confirmed.
NaOH solution. which is soluble in NH4Cl so-
lution.
2. To the original solution add White precipitate is formed. Mg2+ is confirmed.

Note: In the systematic qualitative analysis of a simple salt for identification of anion and
cation the following points are to be noted.
1. The given simple salt contains one anion and one cation only.
2. Perform the preliminary tests for the salt like colour, physical state, action of heat (dry heating
test) and flame test. Record your observations and inferences in the table.
3. After the preliminary tests, carry out the analysis of anion in the following order.
(i) Test with dil.HCl: If the salt gives any gas with dil.HCl the salt may contain either carbonate or
acetate. Depending upon the nature of the gas (effervescence smell etc.,) perform the confirmatory
tests for that particular anion. With this the analysis of anion is over and proceed for the analysis of
cation. No need of performing tests with con.H2SO4 and BaCl2 for other anions.

(ii) Test with conc.H2SO4: If no gas is evolved with dil.HCl (absence of CO32- and CH3COO-), then
perform test with conc.H2SO4 (in cold and hot conditions). If any gas/vapours are evolved, the
salt may contain Cl- or Br- or I- or NO3- Depending upon the nature of gas/vapours (colour, smell
etc.,) perform the confirmatory tests for that particular anion. With this, the analysis of anion is over
and proceed for the analysis of cation. No need of performing tests with BaCl2 for other anions.
(iii) Test with Baci2: If no gas is evolved with dil.HCI (absence of CO32- and CH3COO-) and with
conc.H2SO4 (absence of C1-, Br-, 1-, NO3-), then perform test with Bacl2 A white precipitate
indicates the presence of sulphate ion (SO42-) and perform the confirmatory test for SO42- and
proceed for analysis of cation.
Record your observations and inferences in the table.
(iv) In the analysis of cation, in the beginning perform tests for ammonium ion (NH4+). If ammonia
smell is evolved on adding NaOH solution to the salt carry out confirmatory test for NH4+.
This completes the analysis of cation. Do not proceed further for groups I to VI as the salt
contains only one cation, which is confirmed as NH4+
(v) If ammonia smell is not observed in the test for NH4+ proceed to Group-I. If precipitate is
formed (presence of group-I), do confirmatory tests for Group-I cations. This ends the analy-
sis of cation. No need of proceeding to Groups-II to VI.
(vi) Adopt similar procedure for analysis of cation in other groups also.
So, if a precipitate is formed in a particular group, perform confirmatory tests for the cation of that
particular group only and with this the analysis of cation is over. Do not proceed further to next
groups.
Record your observations and inferences in the table in a systematic order and report the
result. Thus the analysis of simple salt is over.
(iv) Model Analysis of Simple Salts
Salt - I
Aim : To identify and confirm the anion and cation present in the given salt.

Preliminary tests
1. Colour of salt. White Absence of Cu2+ , Fe2+, Mn2+,

Ni2+, Co2+ salts.
2. Physical state Crystalline ---
3. Action of heat (Dry heating Colourless gas with the smell of May be ammonium (NH4+) salt.
test): A pinch of salt is taken in ammonia is evolved.
a dry test tube and heated
strongly.
4. Flame test: A paste of the salt No Characteristic colour im- Cu2+ , Ba2+, Ca2+ and Sr2+ are
with conc.HCl is prepared and parted to the flame. absent.
the flame test is performed.
Second Year 161
Analysis is anion
5. A pinch of salt is taken in a Colourless and odourless gas is Co32- is present.
test tube and dil.HCl is added evolved with brisk effervescence.
(Salt + dil.HCl). which puts out the burning splin-
ter.
6. The above gas is passed into Lime water turns milky. Co32- is present.
a test tube containing lime
water.
Confirmatory test for CO32-

7. To the salt solution BaCl2 White precipitate is formed. Co32- is present.
solution is added.
8. The solubility of the precipi- The precipitate is soluble in Co32- is present.

tate is tested in dil.HCl. dil.HCl
Analysis of cation
Test for ammonium ion
(NH4+)
9. To a pinch of the salt NaOH Colourless gas with ammonia NH4+ is present.
solution is added and heated. smell is evolved.
A glass rod dipped in conc.HCl Dense white fumes are evolved. NH4+ is present.
is brought near the mouth of
the tube.
10. Confirmatory test for

ammonium ion (NH4+)
To the salt solution Nessler’s Reddish brown precipitate is NH4+ is present.
reagent is added. formed.
Report : The given salt contains
Anion : Carbonate ion (Co32-)
Cation : Ammonium ion (NH4+)
The given salt is ammonium carbonate (NH4)2CO3.
Salt - II
Preliminary tests
1. Colour of the salt White Cu2+ , Fe2+ , Mn2+ , Ni2+ , Co2+

salts are absent.
2. Physical state Crystalline
3. Action of heat (Dry heating Water drops are formed along May be hydrated salt.
test): A pinch of salt is taken the inner walls of the test tube
in a dry test tube and heated (loss of water of crystallization)
strongly.
4. Flame test: A paste of the salt Light apple (grassy) green May be barium salt (Ba2+)
is prepared with conc.HCl colour flame is observed.
and the flame test is per-
formed.
Analysis of anion
5. A pinch of salt is taken in a Colourless gas with vinegar Acetate (CH COO -) ion is
test tube and dil.HCl is smell is evolved which turns present.
3
added (Salt + dil.HCl). moist blue litmus paper red.

Acetate ion (CH3COO)-:
6. To a small quantity of the salt Deep red coloured solution is Acetate (CH3COO-) ion is
solution (or water extract of formed.
the salt) in a test tube neu- confirmed.
tral ferric chloride (FeCl3)
solution is added.
7. The above deep red coloured

solution is boiled with wa- Brown precipitate is formed. Acetate (CH3COO-) ion is
ter. confirmed.
8. Esterification: To the salt a

few drops of ethyl alcohol Pleasant fruity odour is Acetate (CH COO-) ion is
and conc.H2SO4 is added and observed. 3
confirmed.
heated. The contents are
poured into a beaker contain-
ing water.
Analysis of cation
9. Test for ammonium ion Ammonia gas is not evolved. NH4+ is absent
(NH4+): To a pinch of the salt
NaOH solution is added and
heated.
10. Original solution is prepared Clear and transparent solution Labelled it as original solution.
by dissolving the salt in ex- is formed.
cess of distilled water.
11. Analysis of Group-II

To the original solution dil.HCl No precipitate is formed. Group-I is absent.
is added.
Second Year 163

12. Analysis of Group-II No precipitate is formed. Group-II is absent.
To the original solution dil.HCl
is added H 2S gas is passed
13. Analysis of Group-III

To the original solution solid No precipitate is formed. Group-III is absent.
NH4Cl and excess of NH4OH
are added.
14. Analysis of Group-IV

To the original solution solid No precipitate is formed. Group-IV is absent.
are added and H2S gas is passed
15. Analysis of Group-V

To the original solution solid White precipitate is formed. Group-V is present (Ba2+ or Sr2+
NH4Cl, excess of NH4OH and or Ca+2 is present)
(NH4)2CO3 solution are added.
16. Confirmatory tests for

Barium ion (Ba2+)
i) To the original solution po- Yellow precipitate is formed Barium ion (Ba2+) is confirmed.
tassium chromate solution which is soluble in conc.HCl.
(K2CrO4) is added.
ii) To the original solution am- White precipitate is formed Barium ion (Ba2+) is confirmed.
monium oxalate solution Which is soluble in acetic acid.
((NH4)2C2O4) is added.
iii) Flame test: Take a platinum Light apple (grassy) green Barium ion (Ba ) is confirmed.
2+
wire and dip it in conc.HCl flame is observed.

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 group-v precipitate or
original salt in conc.HCl.
Heat it in the flame.
Report : The given salt contains.

Anion : Acetate ion (CH3COO-)
Cation : Barium ion (Ba2+)
The given salt is barium acetate (CH3COO)2Ba
Salt - III
Preliminary tests
1. Colour of the salt White Absence of Cu2+, Fe2+, Mn2+,
Ni2+, Co2+ salts
3. Action of heat (Dry heating Water drops are formed along May be hydrated salt.
test): A pinch of salt is taken the inner walls of the test tube
in a dry test tube and heated (loss of water of crystallization)
strongly.
4. Flame test: A paste of the salt No charateristic colour im- Cu2+, Ba2+, Ca2+, and Sr2+ salts
with conc.HCl is prepared parted to the flame. are absent.
formed.
Analysis of anion
5. A pinch of salt is taken in a No gas is evolved. CO32- and CH3COO- are absent
test tube and dil.HCl is added
(Salt + dil.HCl).
6. A pinch of salt is taken in a test Colourless gas with pungent Chloride ion(Cl - ) may be
tube and conc.H2SO4 is added smell is evolved and dense present.
(Salt + conc.H2SO4). white fumes are evolved when
a glass rod dipped in con.HCl
is brought near the mouth of the
test tube.
7. Confirmatory tests for chlo-
ride ion (Cl-) Chloride ion(Cl-) is confirmed.
(i) To a pinch of salt manganese Greenish yellow gas with pungent
dioxide (MnO 2) and smell is evolved.
conc.H2SO4 are added and
heated.
Chloride ion(Cl-) is confirmed.
(ii) To the salt solution ( or wa- White precipitate is formed
ter extract of the salt) silver which is soluble in NH4OH.
nitrate solution (AgNO3) is
added.
Analysis of cation
8. Test for ammonium ion
(NH4+) NH4+ ion is absent.
To a pinch of the salt NaOH Ammonia gas is not evolved.
solution is added and heated.
Second Year 165
9. Original solution is prepared Clear and transparent solution Labelled it as original solution.
by dissolving the salt in excess is formed.
of distilled water.
10. Analysis of Group-I

To the original solution dil.HCl No precipitate is formed. Group-I is absent.
is added.
To the original solution dil.HCl No precipitate is formed. Group-II is absent.
is added and H2S gas is passed
12. Analysis of Group-III

To the original solution solid No precipitate is formed. Group-III is absent.
are added.
13. Analysis of Group-IV

To the original solution solid No precipitate is formed. Group-IV is absent.
are added and H2S gas is passed
14. Analysis of Group-V

To the original solution solid No precipitate is formed. Group-V is absent.
NH4Cl, excess of NH4OH and
(NH4)2CO3 solution are added.
15. Analysis of Group-VI

To the original solution solid White crystalline precipitate is Group-VI is present Mg2+ is
NH4Cl, excess of NH4OH and formed which is soluble in present.
disodium hydrogen phosphate acetic acid and dil.HCl.
(Na2HPO4) solution are added.
Warmed and the inner sides of
the test tube are scratched with
a glass rod.
16. Confirmatory test for Mg2+

To the original solution sodium White precipitate is formed. Mg2+ is confirmed.
carbonate solution is added.

Anion : Chloride ion (Cl-)
Cation : Magnesium ion (Mg2+)
The given salt is Magnesium chloride (MgCl2)
Salt - IV
Preliminary tests Absence of Cu2+, Fe2+, Mn2+,
1. Colour of the salt White Ni2+, Co2+ salts
3. Action of heat (Dry heating Colourless gas with the smell of May be ammonium (NH +) salt.
4
test): A pinch of salt is taken ammonia is evolved.
in a dry test tube and heated
strongly.
4. Flame test: A paste of the salt No characteristic colour im- Cu2+, Ba2+, Ca2+, and Sr2+ salts
with conc.HCl is prepared and parted to the flame. are absent.
the flame test is performed.
Analysis of anion
5. A pinch of salt is taken in a No gas is evolved. CO32- and CH3COO- are absent
(Salt + dil.HCl).
6. A pinch of salt is taken in a Reddish brown vapours with Bromide ion(Br ) may be
-
test tube and conc.H2SO4 is pungent smell (Br 2

) are present.
added (Salt + conc.H2SO4). evolved.

Bromide ion (Br-)
(i) To a pinch of salt manganese Reddish brown vapours with Bromide ion(Br-) is confirmed.
dioxide (MnO 2) and pungent smell (Br2) are evolved
conc.H 2SO 4 are added and which turns starch paper yellow.
heated.
(ii) To the salt solution silver Pale yellow precipitate is Bromide ion(Br-) is confirmed.
nitrate solution (AgNO3) is formed which is partially
added. soluble in NH4OH.
Analysis of cation
(NH4+)
To a pinch of the salt NaOH Colourless gas with ammonia NH4+ is present.
solution is added and heated. smell is evolved.
9. A glass rod dipped in Dense white fumes are formed. NH4 is present.
+
conc.HCl is brought near the

mouth of the test tube.
10. Confirmatory test for Reddish brown precipitate is NH + is present.
Ammonium ion(NH4+): formed. 4
To the salt solution Nessler’s
reagent is added.
Report : The given salt contains Anion : Bromide ion (Br-)
Cation : Ammonium ion (NH4 ) +
The given salt is Ammonium bromide (NH4Br-).
Second Year 167

Salt - V
Preliminary tests
1. Colour of the salt White Absence of Cu2+, Fe2+, Mn2+,

Ni2+, Co2+ salts
3. Action of heat (Dry heating Reddish brown vapours are

May be Nitrate (NO3-) salt.
test): A pinch of salt is taken evolved and cracking sound is
in a dry test tube and heated observed.
strongly.
No characteristic colour im- Cu2+, Ba2+, Ca2+, and Sr2+ salts
4. Flame test: A paste of the salt parted to the flame.
are absent.
with conc.HCl is prepared
and the flame test is
performed.
Analysis of anion No gas is evolved. CO32- and CH3COO- are absent

5. A pinch of salt is taken in a
(Salt + dil.HCl).
No gas is evolved. Halides (Cl- , Br- and I- ) are ab-
6. To a pinch of the salt
sent.
conc.H2SO4 is added.
Deep reddish brown vapours Nitrate ion (NO 3 -) may be
7. To a pinch of the salt a few are evolved and the solution in
present.
copper turnings and the test tube becomes blue.
heated strongly.
8. Confirmatory test for

Nitrate ion (NO3-) Brown A dark brown ring is formed at
Nitrate ion (NO3-) is confirmed.
ring test: Prepared the the junction of the two layers
sodium carbonate extract of (acid and solution layers).
the salt and is acidified with
dil.H 2 SO 4 and freshly
prepared ferrous sulphate
solution is added in excess.
To this conc.sulphuric acid
(conc.H2SO4) is added slowly
along the sides of the test tube
keeping the test tube in an
inclined position.
Experiment
Observation Inference
Inference
Analysis of cation
(NH4+): To a pinch of the salt No ammonia gas is evolved. NH4+ is absent.
NaOH solution is added and
heated.
10. Preparation of original

solution: Original solution is Clear and transparent solution Labelled it as original solution.
prepared by dissolving the is formed.
salt in excess of distilled
water.
11. Analysis of Group-1

To the original solution White precipitate is formed. Group-I is present (Pb 2+ is
dil.HCl is added (O.S. + present)
dil.HCl)

lead ion (Pb2+)
(i) To the original solution Yellow precipitate is formed Pb2+ is confirmed.
potassium chromate solution which is soluble in NaOH
(K2CrO4) is added. solution.
(ii) To the original solution Yellow precipitate is formed Pb2+ is confirmed.

potassium iodide solution which dissolves in hot water
(KI) is added. and on cooling golden spangles
are formed.

Anion : Nitrate ion (NO3-)
Cation : Lead ion (Pb+2)
The given salt is lead nitrate (Pb(NO3)2)
Second Year 169

Salt - VI
Preliminary tests
1. Colour of the salt Bluish green May be copper (Cu2+) salt.
2. Physical state Crystalline ---
3. Action of heat (Dry heating

test): A pinch of salt is taken Water drops are formed along May be hydrated copper salt.
in a dry test tube and heated the inner walls of the test tube
strongly. and the blue coloured salt be-
comes colourless ( or white).
4. Flame test: A paste of the salt Bluish green flame is observed. May be copper (Cu2+) salt.
with conc.HCl is prepared
formed.
Analysis of anion
5. A pinch of salt is taken in a No gas is evolved. CO32- and CH3COO- are absent.
(Salt + dil.HCl).
6. To a pinch of the salt No gas is evolved. Halides (Cl- , Br- , and I- ) are
conc.H2SO4 is added. absent.
7. To a pinch of the salt a few No reddish brown gas is Nitrate ion (NO -) is absent.
3
copper turnings and evolved.
heated strongly.
8. To the salt solution barium White crystalline precipitate is Sulphate ion (SO 2-) is present.
4
chloride solution (BaCl2) is formed which is insoluble in
added. conc.HCl.
9. Confirmatory test for Sul-

phate ion (SO42-) :
The sodium carbonate extract White crystalline precipitate is Sulphate ion (SO 2-) is con-
(or water extract) of the salt is formed which is insoluble in firmed.
4
prepared and it is acidified conc.HCl

with dil.HCl and barium
chloride solution (BaCl2) is
added.
Analysis of cation
(NH4+): To a pinch of the No ammonia gas is evolved. NH4+ is absent.
salt NaOH solution is added
and heated.
11. Preparation of original

solution: Original solution Clear and transparent solution Labelled it as original solution.
is prepared by dissolving the is formed.
salt in excess of distilled
water.
12. Analysis of Group-1

To the original solution No precipitate is formed. Group-I is present.
dil.HCl is added (O.S. +
dil.HCl)

To the original solution Black precipitate is formed. Group-II is present (Cu 2+ is
dil.HCl is added and H2S present).
gas is passed through the
solution (O.S. + dil.HCl +
H2S).

Cu2+
(i) To the salt solution potas- Chocolate brown precipitate is Copper (Cu2+)is confirmed.
sium ferrocyanide solution formed.
(K4[Fe(CN)6]) is added.
(ii) To the salt solution NH4OH Pale blue precipitate is formed Copper (Cu2+)is confirmed.
is added. which is soluble in excess of
NH4OH.
Anion : Sulphate ion (SO42-)
Cation : Copper ion (Cu2+)
The given salt is copper sulphate (CuSO4)
Second Year 171

Question for discussion
1. What is qualitative inorganic analysis?
2. What is the difference between qualitative analysis and quantitative analysis?
3. Why do inorganic salts ionise when dissolved in water?
4. Name the colours of Fe(II), Fe(III), Cu(II), Co(II), Mn(II) and Ni(II) salts.
5. Anions and cations are called acidic and basic radicals respectively Why?
6. Why do salts containing cations like Ca2+, Ba2+, Sr2+ and Cu2+ impart colour to the flame
while Mg2+ does not impart any colour to the flame?
7. Why lime water turns milky when CO2 gas is passed into it? Give equation.
8. Both CO2 and SO2 turns lime water milky. How can you distinguish between the two?
9. Explain the chemistry of flame test.
10. Why do we use conc.HCl to prepare paste of the salt for flame test?
11. SO2 gas turns potassium dichromate paper green. Which compound is reduced in the
reaction? Mention the oxidation states.
12. Both NO2 and Br2 are reddish brown in colour. How can you distinguish between the
two?
13. What is the white precipitate formed when AgNO3 solution is added to the chloride salt?
14. What colour is imparted to the flame in the flame test for barium ion?
15. What is the composition of brown ring formed in the ring test?
16. Why AgNO3 solution is stored in dark coloured bottles?
17. Why NH4+ is tested at the begining before proceeding to the groups?
18. What are the dense white fumes formed when ammonia gas is exposed to HCI?
19. When KI solution is added to Pb2+, yellow precipitate is formed and it is soluble in hot
water. But on cooling, the precipitate reappears. Why?

20. Can we use conc.HCl in the analysis of Groups I and II instead of dil.HCl?
21. How do you detect the presence of NH4+ in the salt?
22. What are the anions that are detected with dil.HCl?
23. Group-III cations are precipitate as hydroxides. Then, why is it necessary to add solid NH4Cl
along with NH4OH?
24. Name a cation which is not obtained from a metal.
25. What is the action of dil.HCl on a salt containing acetate ion?
26. What is the compound formed in the esterification of sodium acetate with ethyl alcohol?
Give its IUPAC name.
27. Give the equation for the reaction of neutral FeCl3 with CH3COONa followed by boiling
with water.
28. Why Fecl3 is neutralized before it is used?
29. What is name of the precipitate formed when solution of carbonate salt is treated with
Bacl2 solution?
30. What are the dense fumes evolved when HCl gas is exposed to a glass rod dipped in
ammonia solution.
31. Why the sodium carbonate extract of the salt is to be neutralized with a suitable acid
before it is tested for anions?
32. What is the precipitate formed when the solution of SO42- is treated with Baci2 solution?
Give equation.
33. How do you detect ammonia gas?
34. What is the white precipitate formed when solution of Pb2+ is treated with dil.HCI?
35. Copper is precipitated as sulphide with H2S. Why is it necessary to add dil.HCI?
36. In cation analysis instead of NH4OH, can we use NaOH? If not why?
37. Give the colour of precipitates of Group-IV cations.
38. Why the original solution is not prepared in conc.HNO3 or conc.H2SO4?
Second Year 173

39. Why is it essential to add NH4OH before passing H,S gas in group-IV?
40. Why the white crystalline precipitate in group-VI is not formed immediately?
41. In what way the preliminary examination helps in the analysis of a salt?
42. What is lime water?
43. Can we use ammonium sulphate instead of ammonium chloride in the precipitation of group-
III cations?
44. Name the group reagents and cations present in different groups.


PROJECT - I
Title
study of presence of oxalate ions in guava fruit at different stages of ripening
Objective
The objective of the project is to find the variation of the content of oxalate ions in guava fruit
during different stages of its ripening.
Background
Guava is a light green or dark green coloured fruit which is juicy and sweet. It is widely
cultivated in India. Guava fruit is a rich source of minerals and vitamin C. It is also rich source of
oxalate. The oxalate content of guava fruit varies during different stages of its ripening. During its
different stages of ripening it acquires green or pale green colour (unripe), yellowish white (partially
ripe) and yellow colour (fully ripe).
Requirements
Guava fruits (at different stages of ripening), beakers, conical flask, measuring flask, mortal
and pestle, funnel, burette, weight - box, pipette, filter paper, dilute H2SO4, 0.001N KMnO4
Theory
Oxalate ions are extracted from guava fruit pulp by boiling it with dilute H2SO4 and volumetri-
cally estimated by titrating with standard KMnO4 solution.
Procedure
Take different samples of guava fruits (green, pale green, yellowish white and yellow coloured
from unripe, partially ripe to fully ripe variety). Take 100 g of one of the samples and crush it into pulp
in mortar and add 100 mL of distilled water. Boil it for 10-15 minutes and filter. Take 20 mL of the
filtrate into a conical flask and add 20 mL of dilute H2SO4. Heat the contents to about 60°C and titrate
it with 0.001 N KMnO4 solution. Repeat the experiment with different samples of guava fruit.
Record your observations in the table.
Observations
Weight of guava fruit taken each time = 100.0 g
Volume of guava extract taken each time (V1)= 20.0 mL
Normality of KMnO4 solution (N2) = 0.001 N
Table P 1.1: Titration of different samples of guava fruit extract (oxalate ions) with KMnO4
Burette readings Concordant volume of
Variety of guava fruit
0.001 N KMnO4
extract Initial Final solution (V2)
Green (unripe) X1 mL
Pale green (unripe) X2 mL
Yellowish white X3 mL
(partially ripe)
Yellowish (fully ripe) X4 mL
Second Year 175

Calculations
According to the rule of normally N1V1 = N2V2
Guava extract KMnO4
For unripe sample of guava fruit (Green)
N 2V2
Normally of oxalate (C2O42-), N1 = V1
0.001 X 1
N1 
20
Strength of oxalate ions = N1  eq.mass of C2O42-
= N1  44 g lit-1
Similarly calculate strength of oxalate ions in other samples of guava fruit.
PROJECT - 2
Title
Study of quantity of casein present in different samples of milk
Objective
To compare the quality of different samples of milk by finding out the quantity of casein
present in them.
Background
Milk contains proteins, carbohydrates, fats, minerals, vitamins and water. Among proteins
present in milk, casein is the major constituent. The casein content is different for different samples of
milk like cow milk, buffalo milk, goat milk and sheep milk. Casein is present as calcium caseinate in
milk and exist in the form of micelles.
Requirements
Different samples of milk (cow milk, buffalo milk, goat milk and sheep milk), beakers
(500 mL), burner, glass rod, funnel, weight -box, filter paper, dil.HCI
Procedure
Take 200 mL of different samples of milk in different 500 mL beakers. Heat to about 50-60°C
temperature. Add a few drops of dil.HCl to it slowly by constant stirring with a glass rod for 5-10 minutes.
Casein coagulates to form an amorphous substance. Filter and wash the precipitate several times with tap
water. Remove the fat content by dissolving in a suitable organic liquid. Allow the precipitate to dry. Take the
weight of the precipitate in previously weighed watch glass. Repeat the same process for different samples of
milk. Record your observations.

Observations
Table P 2.1: Determination of percentage of casein present in
different samples of milk
Volume of the milk taken in each case (V) = 200 mL
Milk sample Weight of Percentage of casein
 w  w×100
 =
 v  200
1. Cow milk
2. Buffalo milk
3. Goat milk
4. Sheep milk
Conclusion : Different samples of milk contains different percentages of casein.
PROJECT - 3
Title
Preparation of soyabean milk and its comparison with natural milk with respect to curd forma-
tion, effect of temperature etc.,
Objective
To prepare soyabean milk and compare it with natural milk with respect to curd formation,
effect of temperature, taste etc.,
Background
Natural milk is a complete balanced diet, which contains proteins, carbohydrates, vitamins,
minerals, fats and water and fresh milk is sweet to taste. The formation of curd from milk is due to the
conversion of lactose present in milk to lactic acid and in this acidic condition, the casein present in
milk forms precipitate, which is called curd. Soyabean milk is prepared from soyabeans and contains
proteins, carbohydrates, vitamins, minerals and fats.
Requirements
Beakers, mortar and pestle, measuring cylinder, glass rod, tripod stand, thermometer, muslin
cloth, burner, soyabeans, buffalo milk, fresh curd and distilled water.
Procedure
Prepare soyabean milk by soaking 150 gm of soyabean seeds in warm water and keeping them
overnight in water. Make a paste of seeds by crushing and finely grinding them with a pestle and
mortar. Add 250 mL of water to the paste and filter it through muslin cloth and discard the undissolved
portion. The filtrate so obtained is soyabean milk. Compare soyabean milk with natural milk with
respect to its taste, colour, smell, effect of temperature, curd formation, etc.. Comparison of effect of
temperature and curd formation may be carried out as follows.
Take 50 mL each of natural milk (buffalo milk) and soyabean milk in three separate beakers and heat
the beakers to 30°C, 40°C and 50°C respectively. Add 1/4 spoonfull of curd to each of the beakers and
leave the beakers undisturbed for 8 hours. Curd is formed.
Second Year 177

Observations
Table P 3.1: Comparision of effect of temperature and curd formation between
natural milk and soyabean milk.
Type of milk Beaker No. Temperature Quality of curd Taste of curd

Natural milk 1 30OC
2 40OC
3 50OC
Soya bean milk 1 30OC
2 40OC
3 50OC
Conclusion
For natural milk and soyabean milk the best temperatures for the formation of good quality
and tasty curd respectively are ------OC and ------OC
PROJECT - 4
Title
Study the effect of potassium metabisulphite as food preservative under various conditions
(temperature, concentration, time etc.,)
Objective
To study the effect of concentration of potassium metabisulphite (preservative), temperature
and time on preservation of food.
Background
Potassium metabisulphite (KHSO3) is a good food preservative. It is used for preservation of colourless
food materials like fruit juices, apples and squashes etc., KHSO3 reacts with the acid content of the fruit juice
and liberates SO, gas which destroys the harmful micro-organisms present in food material and thus prevents
the food material from spoilage.
H+(aq) + HSO3- (aq)  H2O(l) + SO2(g)

Requirements
Boiling tubes, knife, glass rod, amla fruit, spices, salt, mustard oil, potassium metabisulphite.
Procedure
Collect amla fruits and wash them with water. Cut the amla fruits into small pieces and dry in
the sunlight for a few hours. Add the spices and the salt to the amla pieces. Pour 25 g of amla pieces
into each of the six boiling tubes denoted as A,B,C,D,E and F.
Weigh 500 mg of potassium metabisulphite and dissolve it in 20 mL of distilled water.
Keep the boiling tube A without mixing preservative and oil. In boiling tube B and C add 1 mL
of the preservative solution and 2 mL of oil and mix the mixture with the glass rod. Keep the
boiling tube B at the room temperature (25-35°C) and the boiling tube C at a temperature of
40O. In boiling tubes D, E and F add 2 mL, 4 mL and 8 mL of the preservative solution respectively and 2 mL
of mustard oil. Keep these boiling tubes at the room temperature. Prepare again the fresh mixture in boiling
tubes D, E and F and keep them at 40OC temperature. Keep all these boiling tubes for 3 to 5 days. Note the
growth of fungi, if any, in these tubes.
Record your observation and draw conclusion.
Observation
Table P 4.1: Growth of micro-organisms in food stuffs with temperature and time
Weight Amount of Amount of Tempereature Growth of micro

Sample organisms after
of amla Preservative mustard
pieces solution oil added
added 30OC 40OC 3 days 4 days 5 days
A 25g - -
B 25g 1.0 mL 2.0 mL
C 25g 1.0 mL 2.0 mL
D 25g 2.0 mL 2.0 mL
E 25g 4.0 mL 2.0 mL
F 25g 8.0 mL 2.0 mL
Conclusion
The growth of micro-organisms occurs earliest in the sample kept at room temperature and with out
preservative added.
PROJECT - 5
Title
A comparative study of the rate of fermentation of (a ) Wheat flour, (b) Gram flour, (c) Potato
juice, (d) Carrot juice, (e) Orange juice, (f) Apple juice and (g) Sugar-cane juice.
Objective
To determine the rate of fermentation of different substance and study the effect of concentra-
tion, time and temperature on the rate of fermentation of these substances.
Back ground
1. Wheat flour, gram flour, potato juice contains starch. These food materials are crushed to
powder and diluted with water to get starch solution. The germination of barley produces the enzyme
diastase which converts starch into maltose.
Diastase
2 (C6H10O5)n + n H2O  n C12H22O111
Starch Maltose
Second Year 179

2. Carrot Juice, orange juice, apple juice and sugar-cane juice contains sugars like sucrose,
glucose and fructose, which on fermentation with yeast gives ethanol. The enzyme invertase
convert sucrose into glucose and fructose. The enzyme zymase in turn convert glucose into
ethanol.
Invertase
C12H22O11  C6H12O6 + C6H12O6
Sucrose Glucose Fructose
zymase
C6H12O6  2 C2H5OH + 2CO2 
Glucose Ethanol
Requirements
Conical flask (100 mL), gas delivery tube, glass rod, thread, balloon, wheat flour, gram flour,
potato juice, carrot juice, orange juice, apple juice and sugar-cane juice.
Procedure
Take a conical flask (100 mL) fitted with a delivery tube. Remove the delivery tube and add 10
g of wheat flour and about 80 mL of the distilled water into the flask. Stir the contents of the flask with
a glass rod and add 2 g of yeast. Stir the contents again. Fit the delivery tube into the mouth of the
flask. Tie a balloon with the help of a thread to the upper end of the delivery tube. As the fermentation
proceeds, carbon dioxide gas is evolved and the balloon inflates. The extent to which the baloon
inflates in the given time is the measure of the rate of fermentation. Repeat the experiment with other
materials such as gram flour, potato juice, carrot juice, orange juice, apple juice and sugar-cane juice.
Effect of concentration of yeast

Take one of the above substances (say wheat flour) and carry out the experiment as explained
above, but adding 1 g 2 g and 3 g of yeast and note the extent of inflation of balloon in a fixed interval
of time. Note the observations and draw conclusions.
Effect of time
Carry out the reaction using the same substance for different intervals of time and observe the
extent of inflation of balloon and draw your conclusion.
Effect of temperature
Carry out the reaction using the same substances for a fixed interval of time but at three differ-
ent temperatures (25°C, 30°C, and 35°C). Note the extent of fermentation by observing the inflation
of balloon in these reactions and draw conclusions.
Conclusions
1. As the concentration of yeast increases, the rate of fermentation also increases till an optimum
is reached.
2. While the rate of fermentation declines with time at a constant temperature, it does not com
pletely stop. However, the longer the fermentation time, the higher the degree of fermentation.
3. The higher the temperature, more is the yeast activity and therefore the rate of fermentation
increases. Within the given range of temperatures in which yeast is operative, every one degree
rise in temperature increases the rate of yeast fermentation by 3-5%.

Rate of CO2 production
(mL h-1)
Concentration of yeast (g L-)
Fig. P 5.1: Effect of concentration of yeast on the rate of fermentation
PROJECT -6
Title
Extraction of essential oils present in saunf (aniseed), ajwain (carum) and illaichi
(cardamom).
Objective
To extract essential oils from aniseed, carum, and cardamom by using petroleum ether as a
solvent.
Background
The aromas of plants are due to volatile oils present in them. These volatile oils are called
'essential oils' as they are derived from the essence of plants and these are used in perfumes and in
some food flavouring agents. The essential oils contain complex mixtures of esters, alcohols, phenols,
aldehydes, ketones and hydrocarbons. The essential oils are mostly concentrated in the seeds or the
flowers of the plants. Let us learn how to extract the essential oils from aniseeds, carum, and carda-
mom. Essential oils are extracted by the process of steam distillation.
Requirements
Conical flask (250 mL), rubber cork, funnel, filter paper, boiling tube, aniseed, carum, carda-
mom, petroleum jelly
Procedure
Take 100 g of crushed aniseed in a conical flask and add 100 mL of petroleum ether (of
boiling range 60-80° in it. Close the mouth of the flask with a rubber cork and shake it for sometime.
Keep the flask for a day. Filter the solution and collect in a distillation flask. Distill off the petroleum
ether at 60°C - 80°C. Petroleum ether is a highly inflammable liquid. Do not bring any flame near to
it. Use heating mantle for heating the flask. Do not heat it directly on flame. Transfer the liquid (oil)
which is left in the flask to a boiling tube and close the mouth
Second Year 181
of the boiling tube with a rubber cork. Note the colour, odour and volume of the essential oil so
collected.
Similarly, extract essential oils from carum and cardamom.
Observations
Table P 6.1: Comparison of volumes of essential oils extracted
Name of Volume of the Colour of the

S.No essential oil Odour of the
the Weight taken essential oil
obtained essential oil
compound
1 Aniseed 100 g
2 Carum 100 g
3 Cardamom 100 g
Conclusion
The volume of the essential oil obtained from ----------------- is more among the three
compounds.

BOARD OF INTERMEDIATE EDUCATION, A.P., HYDERABAD
CHEMISTRY (Practicals)
Model Question Paper with Scheme of valuation
(With effect from IPE March-2014)
Time: 3hrs Max. Marks
I. Qualitative Analysis 10 Mar
1. Physical state, Colour.Flame test and Action of heat 1/2 X4-2 Ma

2. Carbonates
(a) Action of dil.HCI 1M
(b) Testing gas with burning splinter / limewater 1M
(c) Action of BaCl2 solution 1M
(d) Solubility of the above ppt.in dil.HCI 1M
3. Acetates
(b) Test with neutral FeCl3 solution IM
(c) Boiling the above solution with water 1M
(d) Esterification test 1M
4. Halldes
(b) Action of conc. H2SO4 1M
(e) Action of MnO2 and conc. H,SO, 1M
(d) Action of Silver Nitrate solution 1M
5. Nitrates
(a) Action of dil.HCI 1Mark
(b) Action of cone. H2SO4 1Mark
(c) Action of Copper turnings and conc. H2SO4 and heat 1Mark
(d) Brownring test 1Mark
Second Year 183

6. Sulphates
(a) Action of dil.HCI 1Mark
(b) Action of conc. H2SO4 1Mark
(c) Action of BaCl, solution 1Mark
(d) Solubility of the above ppt.in conc.HCI 1Mark
7. Identification of Cation
(a) Systematic identification of cation in the correct group 2Marks
(b) Confirmation Test for cation 1Mark
8. Correct Salt Report 1Mark
Note:1. Minimum twelve salts must be given for a batch of 20 students

2. Only water soluble salts are to be given
II. Titrimetric Analysis (Volumetric Analysis) 8 Marks
1. Procedure in the first 10 mts. with equation 1+1 Marks
2. For an error upto 1% 4 Marks
3. For an error between 1% and 2% 3 Marks
4. For an error above 29% 2 Marks
5. For indicating the formula 1Mark
6. For Calculation 1 Mark
Note: Minimum two concentrations are to be given for a batch of 20 students
III (a) Identification of Functional group in the given organic compound with the
following tests 6 Marks
1. Physical state (i) Solid 1/2 Mark
(ii) Liquid
2. Ignition Test (i) Sooty flame- Aromatic 1/2 Mark
(ii) Non-sooty flame-Aliphatic
3. Solubility (i) In ether 2Marks
(ii) In water
(iii) In NaHCO3

(iv) In NaOH
(v) In dil.HCI
4. Identification and Confirmation Tests for Functional Groups 3Marks
1. Carboxylic group
(i) Test with neutral FeCl3 2 Marks
(ii) Esterification test 1Mark
2. Aldehydic and Ketonic groups

(i) Test with 2,4 DNP 2 Marks
(ii) Test with Schiff's reagent 1 Marks
3. Alcoholic group
(i) Esterification test 2 Marks
(ii) Iodoform test 1 Mark
4. Phenolic group
(i) Test with neutral FeCI3 2 Marks
(ii) Libermanin test 1 Marks
5. Amino group
(i) Test with NaNO2, dil.HCl and α -Napthol
(Azo dye test) 2Marks
(ii) Carbyl amine test 1 Mark
OR
III (b) Preparation of Colloidal solutions (sols) 6 Marks
(i) Preparation of one lyophilic sol 3 Marks
(ii) Preparation of one lyophobic sol 3 Marks
OR
III (c) Chromatography 6 Marks
(i) Preparation of Chromatographic paper 2 Marks
Second Year 185

(ii) Elution 2 Marks
(iii) Calculation of R1 value 2 Marks
OR
III (d) 1. Qualitative tests for Carbohydrates 6 Marks
(a) Test with conc.H2SO4 2 Marks
(b) Mollisch's Test 2 Marks
(c) Benedict's Test 2 Marks
OR
2. Qualitative tests for Proteins 6 Marks
(a) Biuret Test 2 Marks
(b) Xanthoproteic Test 2 Marks
(c) Ninhydrin Test 2 Marks
IV. Viva Voce 2 Marks

V. Project Work 2 Marks
VI. Record 2 Marks
--------------
Total 30 Marks

APENDIXII
COMMON REAGENTS USED IN CHEMISTRY LABORATORY

Concentrated Acides
Acid Specific gravity Approximate strength

1. Glacial acetic acid (CH3COOH) 1.05 17 M
2. Hydrochloric acid (HCl) 1.18 12 M
3. Nitric acid (HNO3) 1.41 16 M
4. Sulphuric acid (H2SO4) 1.84 18 M
Note: While diluting a concentrated acid, add acid to water. Never add water to a concentrated
acid.
Dilute Acids
Acid Preparation Approximate Strength

1. Acetic acid Dilute 285 mL of conc. CH3COOH to 1 5M
(Dil. CH3COOH) litre with distilled water.
2. Hydrochloric acid Dilute 430 mL of conc. HCl to 1 litre 5M
(Dil. HCl) with distilled water.
3. Nitric acid Dilute 310 mL of conc. HNO3 to 1 litre 5M
(Dil. HNO3) with distilled water.
4. Sulphuric acid Dilute 140 mL of conc. H2SO4 slowly 5M
(Dil. H2SO4) and with constant stirring into 500
mL of distilled water and dilute to 1 litre
Bases
Base Preparation Approximate Strength

1. Ammonia Solution Sp. gr, 0.88 ; 28% NH3 15 M
(Conc. NH4OH)
2. Ammonia solution Dilute 335 mL of conc. NH4OH 5M
(Dil. NH4OH) to 1 litre with distilled water.
3. Lime water Shake lime with distilled water and allow 0.02 M
Ca(OH)2 to stand for some time; filter off the liquid.
The clear solution is lime water
4. Sodium hydroxide Dissolve 200 g of caustic soda in 5M
solution (NaOH) distilled water and dilute to 1 litre
Second Year 187

Some salt solutions / Reagents
(M.W = molecular weight)
Reagents with Preparation Approximate

Molecular Weight Strength
Ammonium acetate
CH3COONH4 Dissolve 231 g of salt in the distilled water and make the volume 3M
(M.W: 77) one litre
Ammonium carbonate Dissolve 160 g of salt in a mixture of 140 ml. of cone Ammonia
(NH4)2CO3 (M W: 96) solution and 860 mL of distilled water 4M
Ammonium chloride
Dissolve 270 g of salt in the distilled water and make the volume
NH4Cl (M.W 53:5) 5M
one litre
Ammonium oxalate Dissolve 35 g of salt in the distilled water and make the volume
(NH4)2C2O4 one litre.
0.5 M
(M.W : 142)
Ammonium sulphate Dissolve 132 g of salt in the distilled water and make the volume
(NH4)2SO4 one litre.
2M
[M.W : 132)
Ammonium molybdate Dissolve 45 of salt in a mixture of 40 mL of conc. ammonia

(NH4)6Mo7O4H2O solution and 60 ml of water, and 120 g of ammonia nitrate and
dilute with water to prepare one litre solution.
Ammonium thiocyanate
NH4CNS (M.W: 76) Dissolve 38 g. of salt in water to get one litre of solution.
0.5 M
YellowAmmonium Saturate 150 mL of concentrated ammonia solution with H2S

sulphide (NH4)Sx keeping the solution cold add 1 g of flowers of sulphur and 250
mL. of cone ammonia solution, shake until the sulphur has 6M
dissolved and dilute to 1 litre.
Bartum chloride
BaCl22H2O (M.W: 244) Disolve 61 g of salt in the distilled water to prepare one litre
solution. 0.25 M
Calcium chloride
CaCl2 .6H2O Dissolve 55 g of hydrated salt in the distilled water and make
(M.W: 219) the volume of one litre solution by diluting with water. 0.25 M
Potassium ferrocyanide
K4[Fe(CN)6 .3H2O Dissolve 55 g of in the water and make the volume of one litre
0.125 M
(M.W : 422) solution by diluting with water.

Potassium iodide Dissolve 83 g of salt in the water and make the volume of one 0.5 M
KI (M.W: 166) litre solution by diluting with water.
Potassium
Dissolve 3.2 g. of salt in the water and make the volume of one
permanganate KMnO4 0.02 M
litre solution by diluting with water.
(M.W: 158)
Potassium thiocyanate Dissolve 49 g. of salt in the water and make the volume of one 0.5 M
KCNS (M.W: 97) litre solution by diluting with water.
Cobalt nitrate Dissolve 44 g of salt in the water and make the volume of one
Co(NO3)2 . 6H2O litre solution by diluting with water. 0.15 M
(M.W 291)
Copper sulphate Dissolve 125 g of salt in the water containing 3 mL of cone.

CuSO4 5H2O H2SO4 and make the volume of one litre solution by diluting 0.5 M
(M.W: 249.5) with water.
Ferric chloride Dissolve 135 g of hydrated salt to distilled water containing 20 0.5 M
FeCl3,.6H2O mL of cone. HCI and make the volume of one litre solution by
(M.W: 270) diluting with water.
Lead acetate Dissolve 95 g of salt in the water containing 15 ml of acetic acid

(CH3COO)2Pb.3H2O and dilute to one litre. 0.25 M
(M. W: 379)
Mercuric chloride Dissolve 27 g of salt in 1 litre of distilled water.

HgCl2 0.1 M
(M.W: 272)
Silver Nitrate Dissolve 10.8g of silver in minimum conc. HNO3 and dilute to 0.1 M
AgNO3 one litre with distilled water or dissolve 17.0 g of silver nitrate in
(M.W:170) distilled water and dilute to one litre
Sodium acetate Dissolve 408 g of salt in distilled water and make the volume of 3M
CH3COONa. 3H2O one litre solution by diluting with water.
(MW: 136)
Disodium hydrogen Dissolve 120 g of salt in water and make the volume of one litre 0.3 M
phosphate solution by diluting with water.
Na2HPO4 .12H2O
(M.W: 358)
Second Year 189

Stannous Chloride Dissolve 56 g of salt in 100 ml of conc. HCI and dilute to one 0.25 M
SnCl2.2H2O litre Keep a few pieces of tin in the bottle to prevent oxidation.
(M.W: 226)
Bromine water Prepare saturated solution by shaking 11 mL of liquid bromine 1.5 M
Br2 (M.W : 160) with water. Add more bromine, if necessary, to ensure a slight
excess.
Chlorine water Prepare saturated solution by passing chlorine as in distilled 00.5 M
Cl2 (M.W: 71) water.
Iodine solution Dissolve 12.7 g of iodine in a solution of 20 g of pure KI in 30

I2 (M.W: 254) mL of water and dilute to one litre with water
Dimethyl glyoxime Dissolve 1 g of the substance in 100 mL of distilled rectified

reagent spirit.
Sodium cobaltinitrate, Dissolve 17 g of the salt in 250 mL of water.

Na3[Co(NO2)6]
Sodium Nitroprusside, Dissolve a crystal in 5 ml of water.
Na3[Co(NO2)6]
Nessler's reagent Dissolved 10 g of KI in 10 mL of ammonia free water. Add
Alkaline solution of saturate HgCl, solution (60 g per litre in small quantities at a
K2[HgI4] time, with shaking until a slight permanent precipate forms. Then
add 80 mL of 9 N NaOH solution and dilute to 200 mL. Allow
to stand overnight and decant off the clear liquid
Reagents Preparation Approximate

Strength
Phenolphthalein Dissolve 1 g of phenolphthalein 100 mL of cohol. 1%
Methyl orange Dissolve 1 g of methyl orange in one litre water. 0.1%
Methuyl red Dissolve 1 g of solid in one litre of hot water or dissolve in 600
mL of alcohol and dilute with 400 mL of water. 0.1%

Starch solution Make a paste of 1 g of starch with cold waters. Pour this drop
by drop into about 100 mL boiling water and continue to boil 1%
for few minutes. Allow to stand until cool. Decant off clear
solution. If 100 g of salicylic acid is added to 100 mL of starch
solution then it keeps well for a long time.
Litmus solution (blue) Dissolve 10 g of solid dye in a litre of water. 1%
Second Year 191

Preparation of solutions for titrimetric analysis (Volumetric analysis)
Compound with Strength (mol L-) Amount (weight or volume to be
molecular weight dissolved for 1 litre of solution
Sodium hydroxide 0.05 M 2 g in one litre

(NaOH) (Mol. Wt. 40)


Oxalic acid (hydrated) 0.05 M 6.3 g in one litre

(H2C2O4. 2H2O, Mol. Wt. 126)
Oxa,ic acid (hydrated) 0.1 M 12.6 g in one litre

(H2C2O4. 2H2O, Mol. Wt. 123)
Hydrochloric acid (HCl) 0.1 M 8.5 mL of concentrated acid

(Mol. Wt. 36.5) (12 M) in one litre
Hydrochloric acid (HCl) 0.05 M 4.2 mL of concentrated acid

(Mol. Wt. 36.5) (12 M) in one litre
Sulphuric acid (H2SO4) 0.1 M 6 mL of concentrated acid

(Mol. Wt. 98) (18 M) in one litre
Sulphuric acid (H2SO4) 0.05 M 3 mL of concentrated acid

(Mol. Wt. 98) (18 M) in one litre
Sodium Carbonate (Na2CO3) 0.05 M 5.3 g in one litre

(Mol. Wt. 106)
Sodium Carbonate (Na2CO3) 0.1 M 10.6 g in one litre

(Mol. Wt. 106)
Potassium Permanganate 0.02 M 3.16 g in one litre

(KMnO4) (Mol. Wt. 158)
Ferrous ammonium 0.1 M 39.2 g in one litre

sulphate (Mohr’s salt)
(FeSO4(NH4)SO4.6H2O
(Mol. Wt. 392)

Second Year 193
.

Chemistry EM PDF

Uploaded by

Document Information

Original Title

Copyright

Available Formats

Share this document

Share or Embed Document

Sharing Options

Did you find this document useful?

Is this content inappropriate?

Copyright:

Available Formats

Chemistry EM PDF

Uploaded by

Copyright:

Available Formats

Intermediate Practical Manual

Andhra Pradesh State Board of Intermediate Education

Printing, Publishing and Districution rights

First Edition : 2013

All rights whatsoever in this book are stictly reserved and no

Syed Omer Jaleel, IAS

Smt. M. Radha Reddy, Member

Sri M. Somi Reddy - Member

Educational Research & Telugu Akademi

Sri M. Somi Reddy, M.A., B.Ed.

Dr. S.A.T. Rajyalakshmi, M.Sc., B.Ed., M.A., Ph.D.

Sri K. Chandra Sekhar Rao,

Educational Research &

Dr. D. Gopal Reddy,

Sri M. Ravi Sankar Naik,

Dr. M. Ramana Reddy,

Sri J.V. Ramana Gupta

Practical Manual Scrutiny Committee Members

Layout & Drawings

The importance of Laboratory Practicals in the teaching of science subjects cannot be

1.1 Do’s in a Chemistry Laboratory

2 Chemestry Practical Manual

4 Chemestry Practical Manual

1.5 Emergency First-Aid in chemistry Laboratory

6 Chemestry Practical Manual

Burner Air holes

Air adjusting disc Air adjusting disc

Oxidising zone Non - luminous outer zone

Air hole opened

Fig. 2.2 Different zones in Bunsen flame

8 Chemestry Practical Manual

2.2 Cutting a Glass Tube and a Glass Rod

2.3 Bending a Glass Tube

Fig. 2.5: Drawing a glass jet

Place marked for boring

Fig. 2.6: (a) Marked cork (b) Boring process

Filter papr Folded once Folded twice opened

Fig. 2.9: Process of filtration

2.9 Measuring Volume of Liquid

Fig. 2.11: Burette Fig. 2.12: Filling the burette

16 Chemestry Practical Manual

(a) (b) (c) (d)

Using conical flask

2.10 Wash Bottle

18 Chemestry Practical Manual

Questions for discussion

20 Chemestry Practical Manual

MELTING, BOILING POINT OF COMPOUNDS &

Fig.3.1: Determination of melting point of an organic solid

Table 3.1: Melting points of some organic substances

22 Chemestry Practical Manual

Table 3.2: Boiling points of some organic liquids

Purification of chemical substances by crystallisation

26 Chemestry Practical Manual

H2O(1)  H+(aq) +OH-(aq)

Table 4.1: pH values of different solutions

S.No. Name of the solution Colour with universal pH value Inference

Fig. 4.1: Universal indicator as test papers

Determination of pH of Some Fruit Juices

Table 4.2: Determination of pH of different fruit juices

Table 4.3 : pH change on dilution

30 Chemestry Practical Manual

Table 4.4: pH change during the neutralisation of 25 ml 0f