Chemistry EM PDF
Chemistry EM PDF
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
c
Board of Intermediate Education
Tadepalli
Price : Rs.
Printed in India
Laser Typeset by M/s StockAssortment, Bapatla.
Printed at M/s
Academic Review Committee
Dr. A. Srinivasulu,
Professor
G. Aruna Sree
JL in Chemistry, MVN & YVN GJC, Agiripalli.
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. 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.
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.
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?
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
(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).
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.
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.
(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.
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.
14 Chemestry Practical Manual
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.
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. 2.13:
(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.
Fig. 2.16: (a) Wash Bottle (Glass) (b) Wash Bottle (Polythene)
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
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.
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
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?
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
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.
Further activity
Carry out the same set of experiments with red cabbage extract instead of universal indicator.
Red cabbage acts as universal indicator.
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.
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.
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)
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.
36 Chemestry Practical Manual
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.
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.
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)
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–
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
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
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.
Questions for discussion
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)
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.
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.
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.
Experiment Observation
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.
First Year 53
Reactions of Nitrite ion (NO2-)
(With Potassium nitrite, KNO2)
Experiment
Experiment Observation
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.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.
First Year 55
Reactions of Sulphite ion (SO32-)
(With Sodium sulphite, Na2SO3)
Experiment Observation
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
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
KI + H2SO4 KHSO4 + HI
2HI+ H2SO4 SO2 + I2 + 2H2O
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)
Experiment Observation
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
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.
Pb(NO3)2 + H2SO4 PbSO4 + 2HNO3
6FeSO4 + 3H2SO4 +2HNO3 3Fe2(SO4)3 + 2NO + 4H2O
FeSO4 + NO + 5 H2O Fe[(NO)(H2O)5]SO4
First Year 61
Reactions of Phosphate ion (PO43-)
Experiment Observation
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.
First Year 63
Test with Sodium carbonate extract
(For confirmation of anions)
Experiment Observation
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.
Pb(NO3)2 + H2SO4 PbSO4 + 2HNO3
6FeSO4 + 3H2SO4 + 2HNO3 3Fe2(SO4)3 + 2NO + 4H2O
FeSO4 + NO + 5H2O Fe[(NO)(H2O)5]SO4
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+)
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.
First Year 67
Reactions of Lead ion (Pb2+)
(With 5% Lead nitrate, Pb(NO3)2 solution containing some acetic acid)
Experiment Observation
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
6. Flame test: Perform flame test and Dull bluish white coloured flame is ob-
observe the colour imparted to the flame. served.
6. Flame test: The characteristic colour Blue or bluish green flame is observed.
imparted to the flame is observed.
First Year 69
Reactions of Aluminium ion(Al3+)
(With 12.5% Al2(SO4)3.18H2O solution containing 2 mL of dil.H2SO4)
Experiment Observation
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.
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.
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
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
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.
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)
Experiment Observation
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.
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.
with solid ammonium chloride and add am-
monium hydroxide and pass H2S gas through
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
7. Borax bead test: The colour of the bead is Heating in non-luminous (oxidising) flame:
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.
74 Chemestry Practical Manual
Reactions of Cobalt ion (Co2+)
(With CoCl2.6H2O solution)
Experiment Observation
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
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.
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
6. Borax bead test: The colour of the bead is Heating in non-luminous (oxidising) flame:
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)
Experiment Observation
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.
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
6. Borax bead test: The colour of the bead is Heating in non-luminous (oxidising) flame:
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.
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)
Experiment Observation
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.
and add dilute sulphuric acid.
5. Flame test: Clean the platinum wire by Brick red coloured flame is observed.
dipping it in conc. HCl taken in a watch
glass and heat the platinum 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. 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.
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.
4. Flame test: Clean the platinum wire by Crimson red coloured flame is observed.
dipping it in conc. HCl taken in a watch
glass and heat the platinum 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. 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 79
Reactions of Magnesium ion (Mg2+)
(With 10% Magnesium sulphate. MgSO4.7H2O Solution)
Experiment Observation
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
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.
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.
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)
80 Chemestry Practical Manual
Reactions of Ammonium ion (NH4+)
(With 3% Ammonium chloride solution (NH4Cl))
Experiment Observation
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
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.
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.
(a) Heating sodium and compound (b) Plunging ignition tube in distilled water
Lassaigne’s
extract
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
Na + Br NaBr
NaBr + AgNO3 AgBr + NaNO3
Pale yellow ppt
(Silver bromide)
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.
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.
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
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.
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.
A Ethanol
B Ether
C Acetone
D CC14
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.
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
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.
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.
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?
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
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 )
Voltmeter
Salt bridge
Zinc Copper
eletrode electrode
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.
Questions for discussion
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?
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
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.
Questions for discussion
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.
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.
Acetone
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
130 Chemestry Practical Manual
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.
Questions for discussion
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?
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.
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
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.
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.
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
3. Solubility in
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.
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.
Experiment Observation Inference
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
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.
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.
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
Experiment Observation Inference
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.
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
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
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___________
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
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
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.
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
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.
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.
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
Experiment Observation Inference
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)
154 Chemestry Practical Manual
Experiment Observation Inference
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).
(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
Experiment Observation Inference
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.
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.
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)
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.
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.
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.
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).
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
Experiment Observation Inference
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.
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.
Salt - II
Aim : To identify and confirm the anion and cation present in the given salt.
Experiment Observation Inference
Preliminary tests
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
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.
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+
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.
and the flame test is per-
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
Experiment Observation Inference
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.
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. 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.
conc.H2SO4 are added and
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.
(ii) To the salt solution NH4OH Pale blue precipitate is formed Copper (Cu2+)is confirmed.
is added. which is soluble in excess of
NH4OH.
Report : The given salt contains.
Anion : Sulphate ion (SO42-)
Cation : Copper ion (Cu2+)
The given salt is copper sulphate (CuSO4)
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?
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?
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?
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?
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.
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.
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?
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.
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.
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.
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
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 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%.
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
2 Carum 100 g
3 Cardamom 100 g
Conclusion
The volume of the essential oil obtained from ----------------- is more among the three
compounds.
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
1. Carboxylic group
(i) Test with neutral FeCl3 2 Marks
(ii) Esterification test 1Mark
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
OR
2. Qualitative tests for Proteins 6 Marks
(a) Biuret Test 2 Marks
(b) Xanthoproteic Test 2 Marks
(c) Ninhydrin Test 2 Marks
Dilute Acids
Bases
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)
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.
188 Chemestry Practical Manual
Some salt solutions / Reagents
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)
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.
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
Some salt solutions / Reagents
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.
.
194 Chemestry Practical Manual