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Chemistry
Class XI
1582 – Laboratory Manual Chemistry ISBN 978-81-7450-841-6
Class XI
CWC Campus
Opp. Dhankal Bus Stop
Panihati
Kolkata 700 114 Phone : 033-25530454
Publication Team
Head, Publication : Anup Kumar Rajput
Division
Chief Editor : Shveta Uppal
Chief Production : Arun Chitkara
Officer
Published at the Publication Division by the Assistant Editor : Ram Niwas Bhardwaj
Secretary, National Council of Educational Production Assistant : Om Prakash
Research and Training, Sri Aurobindo Marg,
New Delhi 110 016 and Printed at Sagar Cover Layout
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FOREWORD
The National Council of Educational Research and Training (NCERT) is the apex
body concerning all aspects of refinement of School Education. It has recently
developed textual material in Chemistry for Higher Secondary stage which is
based on the National Curriculum Framework (NCF)–2005. NCF recommends
that children’s experience in school education must be linked to the life outside
school so that learning experience is joyful and fills the gap between the experience
at home and in community. It recommends to diffuse the sharp boundaries
between different subjects and discourages rote learning. The recent development
of syllabi and textual material is an attempt to implement this basic idea. The
present laboratory manual will be complementary to the textbook of Chemistry
for Class XI. It is in continuation to the NCERT’s efforts to improve upon
comprehension of concepts and practical skills among students. The purpose of
this manual is not only to convey the approach and philosophy of the practical
course to students and teachers but to provide them appropriate guidance for
carrying out experiments in the laboratory. The manual is supposed to encourage
children to reflect on their own learning and to pursue further activities and
questions. Of course the success of this effort also depends on the initiatives to
be taken by the principals and teachers to encourage children to carry out
experiments in the laboratory and develop their thinking and nurture creativity.
The methods adopted for performing the practicals and their evaluation will
determine how effective this practical book will prove to make the children’s life
at school a happy experience, rather than a source of stress and boredom. The
practical book attempts to provide space to opportunities for contemplation and
wondering, discussion in small groups, and activities requiring hands-on
experience. It is hoped that the material provided in this manual will help students
in carrying out laboratory work effectively and will encourage teachers to
introduce some open-ended experiments at the school level.
HUKUM SINGH
Professor and Head
Department of Education in
Science and Mathematics
vi
LABORATORY MANUAL DEVELOPMENT TEAM
MEMBERS
Anjni Koul, Senior Lecturer, DESM, NCERT, New Delhi
Brahm Parkash, Professor, DESM, NCERT, New Delhi
I. P. Aggarwal, Professor, Regional Institute of Education, NCERT, Bhopal
R. S. Sindhu, Professor, DESM, NCERT, New Delhi
Ruchi Verma, Lecturer, DESM, NCERT, New Delhi
MEMBER-COORDINATOR
Alka Mehrotra, Reader, DESM, NCERT, New Delhi
ACKNOWLEDGEMENTS
The National Council of Educational Research and Training (NCERT)
acknowledges the valuable contributions of the individuals and the
organisations involved in the development of Manual for Chemistry Practicals
for Class XI. The following academics contributed very effectively for the
review of the manuscript of this manual : D. S. Rawat, Reader, Department
of Chemistry, University of Delhi; Haritima Chopra, Reader, Maitreyi College,
New Delhi; K. G. Trikha, Reader (Retired), A.R.S.D. College, New Delhi;
M. S. Frank, Vice Principal, St. Stephen’s College, Delhi; Samta Goel, Reader,
Zakir Hussain College, New Delhi; S. G. Warkar, Lecturer, Delhi College of
Engenering, Delhi; Sunita Bhagat, Reader, A.R.S.D. College, New Delhi;
K. K. Singh, PGT, Kendriya Vidyalaya, Pushp Vihar, New Delhi; Mona Rastogi,
Senior Headmistress, ITL Public School, Dwarka, New Delhi; Nivedita Bose,
PGT, Bluebells School, New Delhi; Nishi Saraswat, PGT, Kendriya Vidyalaya
No.1, Delhi Cantt. We are thankful to them. We also acknowledge the
contribution of Sunita Kumari, JPF. Special thanks are due to Hukum Singh,
Professor and Head, DESM, NCERT for his administrative support.
The Council also acknowledges the support provided by the administrative
staff of DESM; Deepak Kapoor, Incharge, Computer Station; Ishwar Singh,
DTP Operator for refining and drawing some of the illustrations; Ritu Jha and
Hari Darshan Lodhi, DTP Operator; K. T. Chitralekha, Copy Editor. The efforts
of the Publication Department are also highly appreciated.
CONTENTS
F OREWORD iii
PREFACE v
UNIT-1 : Introduction 1
1.1 Do’s and don’ts in a chemistry laboratory 2
1.2 Analytical methods 5
1.3 Basic laboratory equipment and procedures 5
1.4 Handling reagent bottles 10
1.5 Heating devices 11
x
7.1 Systematic analysis of anions 81
7.2 Systematic analysis of cations 93
Group Analysis
(I) Analysis of Group-zero cation 99
(II) Analysis of Group-I cations 101
(III) Analysis of Group-II cations 102
(IV) Analysis of Group-III cations 105
(V) Analysis of Group-IV cations 106
(VI) Analysis of Group-V cations 109
(VII) Analysis of Group-VI cations 111
• Experiment 7.2 : Detection of nitrogen, sulphur and 116
halogens in an organic compound
PROJECTS 122
1. To test the contamination of water by bacteria by 125
checking the sulphide ion concentration and find out
the cause of contamination
2. To study the methods of purification of water 126
3. Testing the hardness, presence of iron, fluoride, 126
chloride etc. in drinking water obtained from different
regions and a study of the cause of presence of these
ions above permissible limits
4. Investigation of the foaming capacity of different 127
washing soaps and the effect of addition of sodium
carbonate on their foaming capacity
5. Study of the acidity of different samples of tea leaves 128
and reasons for the variation in colour of tea
prepared from these leaves
6. Study the rates of evaporation of different liquids 129
7. Study the effect of acids and alkalies on the tensile 130
strength of fibres
8. Study of the acids and mineral contents of vegetables 130
and fruits
APPENDICES 135
xi
UNIT-1
INTRODUCTION
L
ABORATORY work has special importance in the learning of science as scientific
principles develop and grow on the basis of laboratory work. Chemistry is
an experimental science; the concepts learned in the theory classes are
better understood through experimentation. Laboratory work provides an
opportunity to observe many of the chemical phenomena under controlled
laboratory conditions and workout a problem through the method of inquiry. In
other words, it provides you with ample opportunity to become a keen observer
and to draw inferences and explain results.
The training in laboratory work helps to develop skills for handling apparatus
and equipment and carry out experiments. In this way, the experimental work
helps to promote scientific temper and adopt a cooperative attitude. Working in
the laboratory provides a platform for trying novel and creative ideas and giving
them concrete shape.
Before you become familiar with the scientific procedures and experimental
skills and start working in the laboratory, you should be well acquainted with
the chemistry laboratory. You should notice the facilities provided in the
laboratory and on your working table.
You will notice that your table is provided with a water-tap, gas-tap, Bunsen
burner spirit lamp/kerosene lamp, a reagent shelf and a bin for disposing waste
material. You will find that some reagents are kept on the shelf fixed on the table
while some reagents are kept on the shelf fixed on sidewalls. Reagents kept on
the shelf of the table are frequently required while those on the shelf fixed on
walls are less commonly used. Besides the facilities on the table, you will see
that there are exhaust fans fitted on the upper portion of the wall opposite to the
doors and windows and are placed close to the level of the ceiling. This facilitates
the exhaution of harmful fumes and circulation of fresh air in the laboratory.
For this purpose, there are also enough number of windows in the laboratory.
Keep these open while working. A fume cupboard is provided in the laboratory
for performing those experiments in which fumes are produced.
It is strongly advised that you should become fully familiar with your
chemistry laboratory, laboratory practices and procedures, and more importantly
the precautions to be taken while working in the laboratory.
The environment in the chemistry laboratory is somewhat special in the sense
that it can be a place of joy, discovery and learning. It can also become a place of
frustration and danger. Frustration – if you come unprepared and neglect
recording the important data properly, and danger – if you do not follow the
precautions properly in conducting the experiments where potential danger exists.
LABORATORY MANUAL CHEMISTRY
2
INTRODUCTION
3
LABORATORY MANUAL CHEMISTRY
• Do not heat the test tube containing solution with its mouth
towards yourself or your neighbour as the spurting of
content may harm you or your neighbour (Fig 1.1). Do not
heat the test tube continuously in one position. Keep it moving
and shaking while heating so that heating is uniform.
• Clean every piece of apparatus as soon as the work is finished
and keep these at proper place. A dirty seat and apparatus
indicate careless habit and it hinders successful performance
of the experiment.
4
INTRODUCTION
• If you will follow the Do’s and Don’ts outlined above, your
experience of learning basic scientific techniques will surely
be full of joy.
In the following pages you will be introduced to basic
laboratory equipments, procedures and techniques required for
working in a chemistry laboratory. Let us begin with the
introduction to type of analytical methods used in chemistry.
5
LABORATORY MANUAL CHEMISTRY
6
INTRODUCTION
7
LABORATORY MANUAL CHEMISTRY
Test Tubes
Test tubes of different volumes are available but usually for this
level of chemistry practical work, test tubes of 125 mm (length) ×
15 mm (diameter), 150 mm (length) × 15 mm (diameter) and 150
mm (length) × 25 mm (diameter) are used. Test tubes are available
with or without rim around the mouth. Test tubes of smaller width
are used for carrying out reactions, which do not require heating
or when heating is required for a short period. Only one third of
the test tube should be filled while carrying out a reaction.
The test tube of bigger diameter is called boiling tube. It is used
when large volume of solution is required to be heated. Test tube
holder is used to hold a test tube while heating a mixture or
solution in it. Test tube stand should be used to keep test tubes
containing solutions in the upright position (Fig.1.4).
Flasks
Mostly round bottom and conical flasks (also called Erlenmeyer
flask) are used in chemistry laboratory. These are available in
various capacities ranging from 5 mL-2000 mL. Choice of the
size and type depends upon the amount of solution to be
handled and the type of reaction to be carried out. Generally,
for heating or refluxing a reaction mixture contained in a round
bottom flask, direct flame / sand bath / water bath, is used.
Conical flasks are employed for carrying out certain reactions
at room temperature or lower temperatures. These are specially
used for carrying out volumetric titrations.
8
INTRODUCTION
Beakers
Beakers of various capacities ranging from 5 mL to 2000 mL are
available and are employed for the purpose of preparing
solutions, for carrying out precipitation reactions and for
evaporation of solvents etc.
Separating Funnels
These are used for separating immiscible liquids. Separating
funnels of various sizes and shapes are available (Fig. 1.5).
(a) (b)
Fig. 1.6 : (a) Air condenser
(b) Water condensers
9
LABORATORY MANUAL CHEMISTRY
10
INTRODUCTION
11
LABORATORY MANUAL CHEMISTRY
BUNSEN BURNER
1. The Base
Heavy metallic base is connected to a side tube called gas tube.
Gas from the source enters the burner through the gas tube and
passes through a small hole called Nipple or Nozzle and enters
into the burner tube under increased pressure and can be burnt
at the upper end of the burner tube.
If the air vent is closed and the gas is ignited, the flame will be
large and luminous (smoky and yellow in colour). The light emitted
by the flame is due to the radiations given off by the hot carbon
particles of partially burnt fuel. The temperature of the flame in
this situation is low. If adjustment of sleeve on vent is such that
gas mixed with air is fed into the flame, the flame becomes less
12
INTRODUCTION
luminous and finally turns blue. When the flow of air is correctly
adjusted, the temperature of the flame becomes quite high. This
is called non-luminous flame. Various zones of flame are shown
below in Fig. 1.13.
Three distinctly visible parts of the Bunsen flame are described
below:
13
LABORATORY MANUAL CHEMISTRY
14
INTRODUCTION
The tube becomes very hot and it may produce burns on touching.
This may melt attached rubber tube also. If it happens, put off the
burner and cool it under the tap and light it again by keeping the
air vent partially opened.
SPIRIT LAMP
If Bunsen burner is not available in the laboratory then spirit
lamp can be used for heating. It is a devise in which one end of a
wick of cotton thread is dipped in a spirit container and the other
end of the wick protrudes out of the nozzle at upper end of the
container (Fig. 1.14). Spirit rises upto the upper end of the wick
due to the capillary action and can be burnt. The flame is non
luminous hence can be used for all heating purposes in the
laboratory. To put off the lamp, burning wick is covered with the
cover. Never try to put off the lighted burner by blowing at
the flame. Fig. 1.14 : The spirit lamp
15
UNIT-2
BASIC LABORATORY
TECHNIQUES
T
HE laboratory apparatus for carrying out reactions, in general, is made up
of glass. It is because glass is resistant to the action of most of the
chemicals. Generally, two types of glass are used for making apparatus
for laboratory work. These are soda-lime glass and borosilicate glass.
Soda-lime glass, which is made by heating soda, limestone and silica, softens
readily at about 300-400°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 700-800°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.
In the following pages you will learn about some of the techniques of handling
glass tubes and glass rods without injuring yourself. Also, you will learn the
techniques of using laboratory apparatus and equipments.
Material Required
Procedure
(i) Place the glass tube or the glass rod on the table and press it with your left
hand.
BASIC LABORATORY TECHNIQUES
(ii) Keep the lower end of a triangular file with its sharp edge
perpendicular to the tube to be marked and pull it towards
you to make a single deep scratch on the glass tube or the
glass rod at a desired length (Fig. 2.1 a).
(iii) Keep thumbs of your hands on both sides, very close and
opposite to the scratch as shown in Fig. 2.1 b and break the
glass tube or rod by applying pressure from your thumbs
in a direction away from you (Fig. 2.1 c). Break the tube/
rod by holding it with a cloth so that hands are not harmed.
(iv) If the glass tube does not break, make a deeper scratch at
the point marked earlier and make a fresh attempt.
(v) Trim any jagged edge by striking with a wire gauge (Fig. 2.2 a).
(vi) Heat the freshly cut edge of the tube gently in the flame to
make the edges round and smooth (Fig. 2.2 b). This is called
fire polishing. For fire polishing, first continuously warm the
cut end in the Bunsen flame and then rotate it back and
forth until the edge is rounded. Too much heating may distort
the rounded edge (Fig. 2.2 c).
17
LABORATORY MANUAL CHEMISTRY
Precautions
(a) Make a single deep scratch at the desired length with one stroke of the file.
(b) To avoid injury, carry out the filing and breaking of the glass tube/rod away
from the face as far as possible and hold the glass tube / rod with the help of a
piece of cloth to avoid injury to hands.
Discussion Questions
Material Required
Procedure
(i) Cut a tube of desired length with the help of a triangular file
as described in section 2.1.
(ii) Place the tube in the hottest zone of Bunsen burner flame
and heat that portion from where it is to be bent (Fig. 2.3 a).
(iii) While heating the tube in the flame keep it rotating slowly until
the portion, which is to be bent, becomes red hot and soft and
starts bending under its own weight. (Fig. 2.3 b).
18
BASIC LABORATORY TECHNIQUES
(iv) Remove the tube from the flame and bend it slowly at a
desired angle by pressing it against a glazed tile to ensure
the coplanarity of the bend (Fig. 2.3 c). Slow process of
bending prevents flattening of glass tube (Fig. 2.4).
(v) Cool it by placing on a glazed tile (Fig. 2.3 c).
(vi) Bend the tubes at different angles as shown in Fig. 2.5.
Precautions
(a) Avoid heating the glass tube only on one side, rather rotate it while heating.
(b) Select a glass tube of appropriate length (nearly 30 cm long) to keep your hands
safe from heat.
(c) To avoid flattening of the glass tube while bending, carry out the process slowly.
Discussion Questions
Material Required
19
LABORATORY MANUAL CHEMISTRY
Procedure
(i) Select a glass tube of appropriate diameter for drawing a jet.
(ii) Cut the glass tube of desired length with the help of a
triangular file.
(iii) Heat the tube in the hottest portion of the Bunsen burner
flame by holding it at both the ends.
(iv) Rotate the tube slowly until the portion, which is kept in the
flame, becomes red hot and soft.
(v) Remove the tube from the flame and pull the ends apart
slowly and smoothly until it becomes narrow in the middle
and then stretches into a fine jet as shown in Fig. 2.6 b.
(vi) Cut the tube in the middle (Fig 2.6 c) and make the jet
uniform and smooth by rubbing it with sand paper and by
fire polishing.
(b)
(a)
(c)
Fig. 2.6 : (a) Heating the tube to draw a jet (b) Before cutting (c) After cutting
Precaution
While drawing a jet, pull apart the two ends of the red-hot tube slowly so that it
becomes thin uniformly.
Discussion Questions
Material Required
20
BASIC LABORATORY TECHNIQUES
Procedure
(i) Mark the rubber cork on both its sides at the place where a
hole is to be drilled (Fig. 2.7 a).
(ii) Choose a borer of diameter slightly smaller in size than
that diameter of the tube to be inserted in the hole (Fig. 2.7 b).
(iii) Place the rubber cork on the table with its smaller end in the
upward direction as shown in Fig. 2.7 c.
(iv) Hold the cork in position with the left hand and put a suitable
borer, lubricated by dipping in water or glycerine, at the
place where the hole is to be drilled (Fig. 2.7 c). By lubricating
the borer with water or glycerine a smooth hole is drilled.
(v) Now hold and push the borer vertically in the downward
direction, and drill the hole by rotating the borer and
simultaneously apply the pressure gently.
(v) For making two holes in the same cork, keep appropriate
distance between the holes and use borers of proper size.
Fig. 2.7 : (a) Marked cork (b) Choosing the borer (c) Boring process
Precautions
(a) Make a mark on both sides of the cork and select borer of proper size.
(b) To obtain a smooth hole, drill half the hole from one side and another half from
the other side of the cork.
Discussion Questions
21
LABORATORY MANUAL CHEMISTRY
Note : (i) Never heat the apparatus with thick walls because it may
break. Borosilicate glass apparatus is usually used for
heating substances.
Fig. 2.9 : Heating solution in (ii) The apparatus, which is used for measuring volume, should
a beaker also not be heated because heating may distort it and
graduations may become invalid.
2.7 FILTRATION
22
BASIC LABORATORY TECHNIQUES
Material Required
• Funnel : One
• Beaker : Two
• Funnel stand : One
• Glass rod : One
• Filter paper : As per need
Procedure
(i) Fold the filter paper to fit in the funnel as shown in Fig. 2.10.
For this, fold the circular filter paper in half, tear off a small
piece of paper from the corner and once again fold it.
(ii) Open the folded filter paper into a cone by keeping three
folds on one side and one on the other such that the torn off
corner is outside. Fit the cone into the funnel. Take care that
filter paper cone fits in one cm below the rim of the funnel.
Fig. 2.10 : Folding the filter paper and placing it in the funnel
23
LABORATORY MANUAL CHEMISTRY
Precautions
(a) The stem of the funnel should touch the side of the beaker in which filtrate is
collected so that falling drops do not cause splashing.
(b) Filter paper cone should not be filled more than two-thirds. If level of the liquid
being filtered rises above the cone, then some unfiltered solution may pass into
the beaker kept below the funnel to collect the filtrate.
Note : (i) For quick filtration, a fluted filter paper may be used with advantage. The ordinary paper is folded into
6 or 16 folds instead of 4 and the folds are then turned alternately inwards and outwards. On opening
the paper we get a cone of fluted filter paper with series of ridges meeting at the apex. Filtration is
rapid due to the large surface available for filtration (Fig. 2.12).
Fig. 2.12 : Folding the filter paper to get a fluted filter paper cone
(ii) For separating the solid from the liquid, filtration should be done in two stages. First, almost whole
of the liquid should be poured out carefully down a stirring rod (Fig. 2.11). When only a few millilitres
of the mixture remain in the beaker, it should be poured into the funnel after swirling the beaker
gently. The sides of the beaker are then rinsed with a stream of water and the content is again
poured into the funnel. Rinsing is repeated till the beaker and the stirring rod is clean. It is better to
pour down a solid liquid mixture along a glass rod (Fig. 2.11). However, care should be taken that
paper is not punched by the stirring rod.
24
BASIC LABORATORY TECHNIQUES
IMPROVISATION
If you do not have a Buchner funnel or if you have very small amount of substance to be
filtered, try following improvised apparatus for suction filtration. Take a glass rod and check
that it passes through the stem of the funnel freely. Flatten one end of the glass rod by
heating it in a bunsen burner flame and then pressing it against the glazed tile. The flat
portion of the rod will now fit into the upper part of the stem of the funnel.
Cut the length of the rod to a small size so that it forms a button with a small stem. Fit the
button in the funnel as shown in the figure below.
Cut a small circular piece of filter paper of the size such that it covers the flat button and
just touched the sides of the funnel. Moisten the filter paper and use this improvised funnel
in place of a Buchner funnel. Try using shirt button in place of this button.
(a) (b)
Fig. 2.14 : (a) Water forming curved surface in the glass apparatus
(b) Noting the reading
25
LABORATORY MANUAL CHEMISTRY
26
BASIC LABORATORY TECHNIQUES
After rinsing, the solution is filled in the burette with the help
of a funnel above zero mark. Stopcock is then opened wide and
the solution is allowed to run through the nozzle till there are no
air bubbles in it (Fig. 2.18).
27
LABORATORY MANUAL CHEMISTRY
28
BASIC LABORATORY TECHNIQUES
29
LABORATORY MANUAL CHEMISTRY
30
BASIC LABORATORY TECHNIQUES
(a) (b)
31
LABORATORY MANUAL CHEMISTRY
(d)
Fig. 2.25 : (a) Weight box (b) Fractional weights (c) Rider and (d) Forceps
Material Required
Procedure
32
BASIC LABORATORY TECHNIQUES
Using Rider
Precautions
(a) Pans must be properly cleaned before and after weighing. Chemicals should never
be placed directly on the pans for weighing.
(b) Always release the beam gently.
(c) Avoid overloading the balance.
(d) Always transfer the weights from one place to another with the help of forceps.
(e) Do not allow the weights to get spoiled by corrosion.
(f) Never weigh a hot/cold object on the balance.
(g) Always keep weights on the right pan and object on the left pan of the balance
(if you are a right handed person).
33
LABORATORY MANUAL CHEMISTRY
Discussion Questions
EXPERIMENT 2.1
Aim
Oxalic acid
Preparation of (250 mL of 0.1M) standard solution* of oxalic acid.
Theory
A solution of exactly known concentration is considered to be a
standard solution. There are various ways of expressing the
concentration of a standard solution. Standard solution of an acid/
base is used to determine the unknown concentration of a solution
of bases / acids by volumetric analysis. For example, a standard
solution of oxalic acid can be used to determine the unknown
concentration of an alkali solution. The strength of a standard
solution is usually expressed in moles per litre. The formula of
hydrated crystalline oxalic acid is
34
BASIC LABORATORY TECHNIQUES
and its molar mass is 126 g. If 126 g of oxalic acid is present in one
litre of the solution, it is known as one molar (1.0 M) solution.
For the preparation of one litre of 0.1 M oxalic acid solution, we
126
require =12.6g of hydrated oxalic acid. Therefore, for preparing
10
250 mL of 0.1 M oxalic acid solution, we require:
12.6 g × 250 mL
= 3.1500 g of hydrated oxalic acid.
1000 mL
In general for preparing a solution of required molarity, the amount
given below :
Material Required
Procedure
(i) Weigh an empty, clean and dry watch glass/weighing tube
accurately (Weight 1). Oxalic acid
(ii) Weigh 3.1500 g oxalic acid by placing it on the above watch
glass/in a weighing tube (Weight 2). Always note weight up to
the fourth decimal place and clean the balance before and after
weighing the chemical.
(iii) Transfer oxalic acid carefully from the watch glass/weighing
tube into a clean and dry measuring flask using a funnel.
Weigh the empty watch glass again (Weight 3) and find out the
mass of oxalic acid transferred to the measuring flask by
substracting this mass (Weight 3) from the combined mass of
watch glass and oxalic acid (Weight 2). Calculate the exact
molarity of solution from this mass. Wash funnel several times
with distilled water by using a wash bottle to transfer the
sticking particles if any into the measuring flask. While washing
the funnel, add water in small amounts so that its volume in
the flask does not exceed ¼th of the volume of the measuring
flask as shown in Fig. 2.27 a, b.
35
LABORATORY MANUAL CHEMISTRY
(iv) Swirl the measuring flask till solid oxalic acid is completely
dissolved. Add more distilled water with shaking. Make up
the volume with distilled water to the etched mark by
adding last few mL dropwise. Stopper the flask and shake it
thoroughly to make the solution uniform throughout
(Fig. 2.27 c, d). Label it as 0.1 M oxalic acid solution.
Precautions
(a) The pan of the balance should be cleaned before and after weighing.
(b) Never touch the weights with hand. Use forceps to transfer weights from the weight-
box to the pan of the balance.
(c) Always use spatula to transfer the reagent from the bottle on to the watch glass.
(d) Stopper the reagent bottle immediately after withdrawing the substance.
(e) Always use distilled water to prepare the standard solution.
(f) Always check the adjustment of the balance before weighing the substance.
(g) Care should be taken while weighing the chemicals. These should not be spilled
on the pan of the balance.
(h) Watch glass/weighing bottle and funnel should be washed several times by using
small amounts of distilled water each time.
(i) While making the solution, water should be added carefully so that the lower
part of the meniscus just touches the etched mark of the measuring flask.
(j) To ensure uniform composition of the solution, stopper the flask and shake it
carefully and thoroughly.
36
BASIC LABORATORY TECHNIQUES
Discussion Questions
(i) What is the formula and the basicity of hydrated oxalic acid and anhydrous oxalic acid?
(ii) What do you mean by a molar solution?
(iii) Why are the standard solutions always prepared in a volumetric flask?
(iv) How will you prepare 250 mL of 0.05 M oxalic acid solution?
(v) Can solid NaOH be used to prepare its standard solution?
(vi) What type of substance can be used for preparing standard solution?
(vii) What is meant by “weighing by transfer”? When is this used?
37
UNIT-3
PURIFICATION AND
CRITERIA OF PURITY
F
OR the identification of a compound, qualitative analysis of pure substance
is required. Therefore, first we have to purify the substance and then check
its purity. There are many techniques namely, crystallisation, distillation
sublimation, chromatography etc. available for purification of a compound. In
this unit you will learn about crystallisation as a technique for purification of a
compound. The purity of a compound may be checked by determining its melting
or boiling point. The technique for determination of melting and boiling points
will also be described in this unit. Pure solid and liquid compounds possess
sharp melting and boiling points. Therefore, melting and boiling points of a
compound can be used as a criteria of purity.
EXPERIMENT 3.1
Aim
Purification of sample of a compound (any one of the following Potash alum,
Copper sulphate or Benzoic acid) by crystallisation.
Theory
Crystallisation is one of the techniques for the purification of an impure compound
particularly when the original crude material obtained after a reaction is in a
very impure condition. First step of the process involves choosing a single solvent
or a mixture of solvents, which dissolves the crude material readily when hot,
but only to a small extent when cold. The crude substance is then dissolved in
the minimum amount of boiling solvent to obtain a saturated solution. Insoluble
impurities are removed by filtering the hot solution. It is then checked for
crystallisation point and then cooled slowly when the solute crystallises out leaving
the greater part of impurities in the solution. The crop of crystals is collected by
filtration and the process is repeated until the crystals of pure substance are
obtained. Sometimes during cooling minute quantity of the substance (solid which
is being purified) is added to the solution to facilitate the initial crystallisation.
This is called seeding. The added tiny crystal acts as a ‘nucleus’ for the growth
of new crystals. Growth of crystals depends upon the conditions in which
crystallisation is carried out. For obtaining good crystals, rapid cooling should
be avoided because it results into small or disfigured crystals.
Purity of crystals is often judged from the colour of the crystals. For example,
pure crystals of alum, copper sulphate and benzoic acid are white, blue and
PURIFICATION AND CRITERIA OF PURITY
Material Required
Procedure
(i) Take 30-50 mL distilled water in a beaker and prepare a Copper sulphate
saturated solution of potash alum/copper sulphate in it at
room temperature by adding the impure solid sample in
small amounts with stirring. Stop adding the solid when it
does not dissolve further. To prepare saturated solution of
benzoic acid use hot water.
(ii) Filter the saturated solution so prepared and transfer the
filtrate into a porcelain dish. Heat it on a sand bath till nearly
¾th of the solvent is evaporated. Dip a glass rod into the
solution, take it out and dry it by blowing air from the
mouth. If a solid film deposits on the rod, stop heating.
(iii) Cover the porcelain dish with a watch glass and keep the
content of the dish undisturbed for cooling.
(iv) When crystals are formed, remove the mother liquor (liquid
left after crystallisation) by decantation.
(v) Wash the crystals of potash alum and copper sulphate, thus
obtained first with very small quantity of alcohol containing
small amount of cold water to remove the adhering mother
liquor and then with alcohol to remove moisture. Wash the
crystals of benzoic acid with cold water. Benzoic acid is
soluble in alcohol. Do not use alcohol to wash its crystals.
(vi) Dry the crystals between the folds of a filter paper.
(vii) Store the dry crystals thus obtained at a safe and dry place.
(viii) Repeat steps (ii-vii) for obtaining maximum amount of pure
substance.
Precautions
(a) Do not evaporate the entire solvent while concentrating the solution.
(b) Do not disturb the solution while it is being cooled.
(c) Use the washing liquid in 3-4 very small installments rather than in one installment.
39
LABORATORY MANUAL CHEMISTRY
Discussion Questions
EXPERIMENT 3.2
Aim
Determination of melting point of a solid organic compound.
Theory
The kinetic energy of molecules of a substance increases on heating.
When it becomes high enough to overcome the attractive forces
operating between the molecules, the lattice structure of the solid
breaks, the solid melts and comes into the liquid state. Melting
point of a substance is the temperature at which solid state of a
substance begins to change into the liquid state, when the pressure
is one atmosphere.
40
PURIFICATION AND CRITERIA OF PURITY
Material Required
• Liquid paraffin
• Thiele’s tube
/Conc. H2SO4 : As per need
/Kjeldhal’s flask/beaker : One
• Organic Compound
• Thermometer : One
(Naphthalene/
• Capillary tubes : As per need
p-Dichlorobenzene/
• Iron stand with clamps : One
p-Toluidine) : As per need
Procedure
(i) Take a capillary tube of approximately 8 cm in length. Seal
its one open end by heating it in a Bunsen flame. Rotate the p-Dichlorobenzene
capillary while sealing to ensure complete closure of the
opening.
p-Toluidine
(ii) Crush the desired substance (about 100 mg) into fine
particles and fill the substance in the capillary tube up to
nearly 1cm length. For filling the capillary, dip its open end Naphthalene
in to the powder. Hold the sealed end between the index finger
and the thumb and tap the upper end gently with the other
hand so that solid particles are tightly packed and capillary Hazard Warning
is prevented from breaking.
• Avoid contact with skin
(iii) Moisten the capillary tube with liquid paraffin and stick it to and eyes and don’t inhale
the thermometer. It will stick to the thermometer by cohesive vapours of these
forces. See that the lower ends of the capillary tube and the chemicals.
thermometer bulb are at the same level. The thermometer is
fitted into a rubber cork, which has a groove on its side for
the escape of air and vapours.
(iv) Take a Thiele’s tube (Fig. 3.1 a) and fill it with 50 to 60 mL
liquid paraffin so that it crosses the bent portion of the Thiele’s
tube. Alternatively, Kjeldahl flask’s may be used in place of
Thiele’s tube.
(v) Dip the thermometer along with the capillary tube in liquid
paraffin and adjust the rubber cork in such a way that the
thermometer bulb and the filled portion of the capillary is
completely dipped in the liquid paraffin and the open end of
the capillary remains in the air as shown in Fig. 3.1 a. The
thermometer and the capillary tube should not touch the
sides of the Thiele’s tube.
(vi) 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.
41
LABORATORY MANUAL CHEMISTRY
Fig. 3.1 : (b) Different apparatus used for determining melting point
42
PURIFICATION AND CRITERIA OF PURITY
Precautions
(a) Keep the lower end of the capillary tube and the thermometer at the same level.
(b) Capillary tube should not be very thick.
(c) Packing of the powder should be uniform without any big air gaps in between
the solid particles.
(d) Thiele’s tube should be heated at the side arm by using a low flame.
(e) The cork of the Thiele’s tube or Kjeldhal flask holding the thermometer should
have a side groove so that vapours can escape through it during the process of
heating to prevent bursting of the tube or flask.
(f) Never fill the bulb of Kjeldahl flask’s more than half.
Note : Paraffin can be safely heated upto 220°C. Therefore for determination of melting point of a substance
possessing melting point higher than this, conc. H2SO4 may be used which can be heated upto 280°C.
Sulphuric acid has been suggested for use but is not recomended. Silicone oils are most satisfactory
liquids and can be used in place of sulphuric acid.
Discussion Questions
EXPERIMENT 3.3
Aim
Determination of boiling point of a liquid organic compound.
Theory
The boiling point of a liquid is the temperature at which vapour
pressure of the liquid becomes equal to the atmospheric pressure,
which the surface of the liquid experiences. At 1.013 bar
atmospheric pressure the boiling point of the liquid is termed as
normal boiling point. Different liquids have different boiling point.
The difference in the boiling points of liquids is essentially due to
the difference in the intermolecular forces operating between the
molecules of the liquid.
43
LABORATORY MANUAL CHEMISTRY
Material Required
Concentrated H2SO4
Procedure
(i) Fill Thiele’s tube with the liquid
paraffin so that it crosses the bent
portion of the Thiele’s tube.
(ii) Take 1-2 drops of the given liquid
in an ignition tube and tie the
ignition tube with the thermometer
with a rubber band as shown in
Fig. 3.2. Note that the lower end of
the ignition tube and the
thermometer bulb are at the same
level.
(iii) Seal one end of the capillary tube
of approximately 8 cm length by
heating in the flame.
(iv) Place the capillary tube with its
open end dipped in the liquid
present in the ignition tube.
(v) Heat the side arm of Thiele’s tube
with a low flame.
(vi) Observe the escape of bubbles at
the lower end of the capillary
dipped in the liquid organic
compound. Note the temperature
at which bubbles start coming
briskly and continuously. This
temperature is the boiling point of
Fig. 3.2: Determination of boiling point the liquid.
44
PURIFICATION AND CRITERIA OF PURITY
Precautions
(a) Record the temperature as the boiling point at which brisk and continuous
evolution of the bubbles starts from the lower end of the capillary dipped in the
liquid organic compound.
(b) Keep the lower end of the ignition tube and the thermometer bulb at the same
level.
(c) Heat the side arm of the Thiele’s tube gently.
(d) Boiling point of the liquid filled in Thiele’s tube should be 50-60°C higher than
that of the liquid, of which boiling point is to be determined.
Discussion Questions
(i) Suggest a suitable liquid, which can be filled in the Thiele’s tube for the determination of
the boiling point of carbon tetrachloride?
(ii) In place of liquid paraffin, can any other liquid be used for the purpose of determination of
boiling point?
(iii) Suppose boiling point of a liquid in Delhi is 100°C. At hill station, will it be the same or
different? Give reasons.
(iv) Why is food cooked more quickly in a pressure cooker?
(v) How would the boiling point of water vary with the addition of equimolar quantities of
urea, potassium chloride and potassium sulphate?
(vi) Why do different isomers of alcohol represented by the formula C4H10O differ in their boiling
points?
Do you know?
Learning technique of crystallisation is not only important from the point of view of
purification of compounds but also from the point of developing large single crystals; because
studies on single crystals have shown them to have many optical and electrical properties
of great use. For example, slices from large crystals of silicon containing traces of certain
impurities are used in making solar batteries used for the operation of instruments in
satellites. Frequency control in radar, television and radio is done by making use of slices of
some crystals. Also, use of crystals of some compounds is made in microphones and
earphones. You can now realize how important it is for chemist to learn these techniques.
45
UNIT–4
CHEMICAL EQUILIBRIUM
(IONIC EQUILIBRIUM IN SOLUTION)
C
HEMICAL reactions can be classified into two categories; namely reversible
and irreversible reactions. Reversible reactions take place in the same
reaction vessel and can proceed in the forward and backward direction
simultaneously under the same conditions of temperature and pressure. Further
in the case of reversible reactions a state is reached, when the rate of the forward
reaction becomes equal to the rate of the reverse reaction and it appears as though
the reaction has come to a stand still. This state is referred to as the state of
dynamic equilibrium. Consider the following simple reversible reaction at the
given temperature, T.
A+B C+D
According to the law of mass action, rate of forward reaction, r1, will be directly
proportional to the product of concentrations of A and B and the rate of backward
reaction, r2, will be directly proportional to the products of concentrations of C
and D.
Thus, r1 = k1[A][B] and r2 = k 2 [C][D]
where k1 and k2 are the rate constants for the forward and the backward
reactions respectively and [A], [B], [C] and [D] are the molar concentrations of A,
B, C and D respectively.
At equilibrium, r1 will be equal to r2
k1 [A][B] = k 2 [C][D]
k1 [C][D]
⇒ =
k2 [A][B]
k1
Putting k = Kc we have
2
[C][D]
Kc =
[A][B]
Kc is called equilibrium constant. Its value is independent of initial
concentration of reactants and is a function of temperature but remains constant
at a constant temperature. At a given temperature, if the concentration of any
one of the reactants or products is changed, then equilibrium is disturbed and
according to Le Chatelier principle, reaction proceeds in that direction which
counteracts the change in concentration , so as to maintain the equilibrium.
CHEMICAL EQUILIBRIUM (IONIC EQUILIBRIUM IN SOLUTION)
EXPERIMENT* 4.1
Aim
Study of shift in equilibrium in the reaction of ferric ions and
thiocyanate ions by increasing the concentration of any one of
these ions.
Theory
The equilibrium reaction between ferric chloride and potassium
thiocyanate is conveniently studied through the change in the
intensity of colour of the solution.
3+ – 2+
Fe (aq) + SCN (aq)
[Fe(SCN)] (aq)
(Blood red colour)
The equilibrium constant for the above reaction may be
written as:
2+
[[Fe (SCN)] (aq)]
K = 3+ –
[Fe (aq)] [SCN (aq)]
Here K is constant at a constant temperature. Increasing the
concentration of either Fe3+ ion or thiocyanate ion would result in
2+
a corresponding increase in the concentration of [Fe(SCN)] ions.
In order to keep the value of K constant, there is a shift in
equilibrium, in the forward direction and consequently an increase
2+
in the intensity of the blood red colour which is due to [Fe(SCN)] .
At equilibrium colour intensity remains constant.
Material Required
* The very nature of the experiment is purely qualitative. therefore, preparation of solution in terms of molarity has
not been stressed.
47
LABORATORY MANUAL CHEMISTRY
Procedure
Ferric chloride (i) Dissolve 0.100 g ferric chloride in 100 mL of water in a beaker
and 0.100 g potassium thiocyanate in 100 mL of water in
another beaker.
Hazard Warning (ii) Mix 20 mL of ferric chloride solution with 20 mL of potassium
• Avoid contact with skin thiocyanate solution. Blood red colour will be obtained. Fill
and eyes. this solution in a burette.
(iii) Take five boiling tubes of same size and mark them as a,b,c,
d and e.
(iv) Add 2.5 mL of blood red solution to each of the boiling tubes
from the burette.
(v) Add 17.5 mL of water to the boiling tube ‘a’ so that total volume
of solution in the boiling tube ‘a’ is 20 mL. Keep it for reference.
(vi) Now take three burettes and label them as A, B, and C.
(vii) Fill burette A with ferric chloride solution, burette B with
potassium thiocynate solution and burette C with water.
(viii) Add 1.0 mL, 2.0 mL, 3.0 mL and 4.0 mL of ferric chloride
solution to boiling tubes b, c, d and e respectively from
burette A.
(ix) Now add 16.5 mL, 15.5 mL, 14.5 mL, and 13.5 mL of water
to boiling tubes b, c, d and e respectively from burette C so
that total volume of solution in each boiling tube is 20 mL.
Note : • Colour intensity of the solution will decrease very much on dilution.
It will not be deep blood red colour.
• Total volume in each test tube is 20 mL.
• Each test tube has 2.5 mL equilibrium mixture.
• Amount of FeCl3 is increasing from test tubes ‘b’ to ‘e’.
48
CHEMICAL EQUILIBRIUM (IONIC EQUILIBRIUM IN SOLUTION)
(x) Compare the colour intensity of the solution in each boiling tube
with the colour intensity of reference solution in boiling tube ‘a’.
(xi) Take another set of four clean boiling tubes. Add 2.5 mL of
blood red solution to each of the boiling tubes from the
burette. Repeat the experiment by adding 1.0 mL, 2.0 mL,
3.0 mL and 4.0 mL of potassium thiocynate solution from
burette B to the boiling tubes b′, c′, d′, and e′ respectively
followed by addition of 16.5 mL, 15.5 mL, 14.5 mL and
13.5 mL of water respectively to these test tubes. Again
compare the colour intensity of the solution of these test tubes
with reference equilibrium solution in boiling tube ‘a’.
(xii) Record your results in tabular form as in Tables 4.1 and 4.2.
(xiii) You may repeat the observations with different amounts of
potassium thiocyanate and ferric chloride solution and
compare with the reference solution.
Change in colour
Volume of ferric
intensity as matched Direction of shift in
Boiling Tube chloride solution taken
with reference solution in equilibrium
in the system in mL
boiling tube “a”
a Reference solution for matching colour containing Equilibrium
2.5 mL blood red solution + 17.5 mL water position
(20 mL equilibrium mixture)
b 1.0
c 2.0
d 3.0
e 4.0
Change in colour
Volume of thiocyanate
intensity as matched Direction of shift in
Boiling Tube solution taken in the
with reference solution in equilibrium
system in mL
boiling tube “a”
a Reference solution for matching colour containing Equilibrium
2.5 mL blood red solution + 17.5 mL water position
(20 mL equilibrium mixture)
b′ 1.0
c′ 2.0
d′ 3.0
e′ 4.0
49
LABORATORY MANUAL CHEMISTRY
Precautions
(a) Use very dilute solutions of ferric chloride and potassium thiocyanate.
(b) Compare the colour of the solutions by keeping the boiling tube and the reference
test tube side by side.
(c) To judge the change in colour of the solution in an effective manner, note the
colour change in diffused sunlight.
(d) Use boiling tubes of the same size.
Discussion Questions
(i) Explain why representing the ionic reaction between ferric and thiocyanate ions as given
in the text viz.
3+ –
Fe (aq) + SCN (aq) [Fe (SCN)]2+ (aq)
is more appropriate in the following form ?
3+ –
[Fe (H2O)6] + SCN (aq ) [Fe (H2O)5 (SCN)]2+ + H2O.
(ii) Does the constancy in colour intensity indicate the dynamic nature of equilibrium? Explain
your answer with appropriate reasons.
(iii) What is equilibrium constant and how does it differ from the rate constant?
(iv) It is always advisable to carry out the present experiment with dilute solutions. Why?
(v) What will be the effect of adding solid potassium chloride to the system at equilibrium?
Verify your answer experimentally.
(vi) Why boiling tubes of same size are used in the experiment?
EXPERIMENT 4.2
Aim
Study of the shift in equilibrium in the reaction between
2+ –
[Co(H2O)6] and Cl ions, by changing the concentration of any
one of these ions.
Theory
2+ –
In the reaction between [Co (H2O)6] and Cl ions, the following
displacement reaction takes place.
2+ –
[Co(H2O)6] + 4Cl
[CoCl4]2– + 6H2O
Pink Blue
50
CHEMICAL EQUILIBRIUM (IONIC EQUILIBRIUM IN SOLUTION)
Alcohol
Since the reaction occurs in the aqueous medium, it is believed
that concentration of H2O is almost constant and is included in
the value of K itself and is not shown separately in the expression
for equilibrium constant. Hazard Warning
2+
Now if at equilibrium the concentration of either [Co (H2O)6] • Acetone and alcohol are
–
ion or Cl ions is increased, then this would result in an increase inflamable, do not let the
2–
in [CoCl4] ion concentration thus, maintaining the value of K as bottles open when not in
constant. In other words we can say that equilibrium will shift in use.
• Keep the bottles away
the forward direction and will result in a corresponding change
from flames.
in colour. • Wash your hands after
use.
• Wear safety spectacles.
Material Required
Procedure
(i) Take 60 mL of acetone in a 100 mL conical flask and dissolve
0.6000 g CoCl2 in it to get a blue solution.
(ii) Take 5 test tubes of same size and mark them as A, B, C, D
and E. Add 3.0 mL of cobalt chloride solution in each of the
test tubes from ‘A’ to ‘E’ respectively. Now add 1.0 mL,
0.8 mL, 0.6 mL, 0.4 mL and 0.2 mL of acetone respectively in Note : • In the first set
these test tubes. Add 0.2 mL, 0.4 mL, 0.6 mL and 0.8 mL of of experiments
concentration of
water to test tubes B, C, D and E respectively, so that the total
chlorocomplex is
volume of solution in each of the test tubes is 4.0 mL. constant and
(iii) Note the gradual change in colour of the mixture from blue concentration of
to pink with an increase in the amount of water. water is changing.
• In the second set
(iv) Take 10 mL cobalt chloride solution in acetone prepared
concentration of
above and add 5 mL distilled water to it. A solution of pink aqua complex is
colour will be obtained. constant and
(v) Take 1.5 mL of pink solution from step (iv) in five different concentration of
test tubes labeled as A′ B′, C′, D′ and E′. Add 2.0 mL, chloride ions is
increasing.
1.5 mL, 1.0 mL and 0.5 mL of water to the test tubes labelled
51
LABORATORY MANUAL CHEMISTRY
from A′ to D′ and 0.5 mL, 1.0 mL, 1.5 mL, 2.0 mL and 2.5 mL
concentrated HCl respectively in the test tubes A′ to E′ so that
total volume of solution in the test tubes is 4 mL.
(vi) Note the gradual change in colour of pink solution to light
blue with increasing amounts of hydrochloric acid. Record
your observations in tabular form (Tables 4.3 and 4.4).
–
Table 4.4 : Shift in equilibrium on adding Cl ions
Sl. Test Volume of conc. Volume of aquo complex Volume of water Colour
No. tube HCl added in mL solution added in mL added in mL of mixture
1. A′ 0.5 1.5 2.0
2. B′ 1.0 1.5 1.5
3. C′ 1.5 1.5 1.0
4. D′ 2.0 1.5 0.5
5. E′ 2.5 1.5 0.0
Precautions
(a) Take all the precautions of experiment 4.1.
(b) Use distilled water for the experiment.
(c) Use burette or graduated pipette for adding water or solutions.
Discussion Questions
(i) What will be the effect of increasing the temperature of the reaction mixture at equilibrium?
(ii) Can an aqueous solution of sodium chloride replace concentrated HCl? Verify your answer
experimentally.
(iii) Why should the total volume of the solution in each test tube be kept same?
52
UNIT-5
PH AND PH CHANGE IN
AQUEOUS SOLUTIONS
Y
OU have already performed experiments on dynamic equilibrium between
unionised salt and the ions produced by it on dissolving in a solvent. In
this unit we will learn about shift in ionic equilibrium between unionised
+ –
water molecules and H and OH ions. The conductivity experiments prove that
even pure water ionises to some extent although it has very low conductivity. On
this basis it can be concluded that ionic equilibrium exists in pure water also.
This ionic equilibrium can be represented as
H2O(l)
+ –
H (aq) + OH (aq)
Since H+ ion cannot have independent existence in water because of its positive
charge and small ionic radius, a better representation of this equilibrium is
2H2O(l)
+ –
H3O (aq) + OH (aq)
This is self ionisation of water. Equilibrium constant for this chemical
equation can be written as follows:
+ –
[H3 O ] [OH ]
K= 2
[H2 O]
Since water is in large excess, its concentration can be assumed to be constant
and combining it with K provides a new constant Kw, which can be written as follows:
+ –
Kw = [H3O ] [OH ]
Kw is self ionisation constant of water or simply ionization constant of water.
–14
It remains constant at constant temperature. At 25°C value of Kw is 1.0×10 .
Thus, it is quite evident that at a given temperature in any aqueous solution,
+ –
this product i.e. [H3O ] [OH ] remains constant whether acidic, alkaline or neutral
in nature. If dissolution of a substance shifts the equilibrium in such a way that
at equilibrium the hydronium ion concentration is more than hydroxyl ion
concentration then the solution is acidic in nature. If dissolution of a substance
–
shifts the equilibrium in such a way that at equilibrium concentration of OH
ions is greater than the concentration of hydronium ions, then the solution is
alkaline in nature. Thus, concentration of hydronium ion in an aqueous solution
can provide information about acidic, basic and neutral nature of the solution.
+
The concentration of H3O ions in a solution is measured in terms of pH which is
defined as the negative logarithm of hydronium ion concentration and is given
by the following expression.
+
pH = –log [H3O ]
LABORATORY MANUAL CHEMISTRY
EXPERIMENT 5.1
Aim
To determine the pH of some fruit juices.
Theory
Several dyes show different colours at different pH. These act as
acid-base indicators. Solution of a mixture of dyes can be used to
obtain approximate pH value of a solution. A solution of a mixture
of dyes can be obtained to measure pH values from zero to 14. It
is called universal indicator. Some universal indicators can
measure the pH change of even 0.5. In fact, dyes themselves are
weak acids or bases. Colour change occurs as a result of change
in the structure of dye due to acceptance or release of protons.
Different forms of a dye have different colours and hence, colour
change is observed when pH of the solution changes. A standard
chart for the colour change of the universal indicator with pH is
supplied with the indicator paper or solution and the comparison
of observed colour change with the chart provides a good estimate
of the pH of the solution.
54
PH AND PH CHANGE IN AQUEOUS SOLUTIONS
Material Required
Procedure
(i) Procure fresh juices of lemon, orange, apple and pineapple
in separate beakers of 100 mL capacity each.
(ii) Transfer nearly 2 mL of the fresh juice (20 drops) with the
help of a separate dropper for each juice in four different
test tubes marked 1, 2, 3 and 4 respectively.
(iii) Add two drops of the universal indicator in each test tube
and mix the content of each test tube thoroughly by shaking.
(iv) Match the colour appearing in each test tube with the
standard pH chart.
(v) Record your observations in Table 5.1.
(vi) Repeat the experiment using pH papers to ascertain the pH
of different juices and match the colour in each case with
the one obtained with universal indicator.
(vii) Arrange the pH value of the four juices in increasing order.
Lemon
Orange
Apple
Pineapple
Result
Increasing order of pH value of juices is ____________.
55
LABORATORY MANUAL CHEMISTRY
Precautions
(a) Add equal number of drops of universal indicator to equal volumes of solutions
in each of the test tubes.
(b) Match the colour of the solution with pH chart carefully.
(c) Store pH papers at a safe place to avoid contact with acidic and basic reagents
kept in the laboratory.
(d) Use only fresh juice for the experiment.
Discussion Questions
(i) Out of the four juices, which one is least acidic? Explain.
(ii) If we dilute each of the juices, what effect is likely to be observed on the pH values?
(iii) On mixing any two juices, would the pH alter or remain the same? Verify your answer
experimentally.
(iv) How can you ascertain the pH of a soft drink ?
EXPERIMENT 5.2
Aim
To observe the variation in pH of acid/base with dilution.
Theory
Hydrogen ion concentration per unit volume decreases on dilution.
Therefore, change in pH is expected on dilution of the solution.
Material Reqiured
Procedure
(i) Take four boiling tubes and mark them as A, B, C and D.
(Fig. 5.1).
(ii) Take 2mL of 0.1 M HCl in boiling tube A.
56
PH AND PH CHANGE IN AQUEOUS SOLUTIONS
H2SO4
HCl
Hazard Warning
• Never add water to the
acid.
• For dilution add acid
slowly into water.
(v) Take 5mL of diluted HCl from boiling tube C in boiling tube
D and add 15 mL water to it.
(vi) Cut a pH paper into small pieces and spread these on a clean
glazed tile.
(vii) Take out some solution from boiling tube A with the help of
a dropper and pour one drop on one of the pieces of pH
paper kept on the glazed tile. Compare the colour of the pH
paper with the standard chart.
(viii) Similarly test the pH of solutions of boiling tubes B, C, and
D respectively and record your results as in Table 5.2.
(ix) Calculate the hydrogen ion concentration of solution B, C
and D.
(x) Take out 1mL of solution from each boiling tube and
transfer in separate test tubes. Add 2 drops of universal
indicator to each of these test tubes. Shake the test tubes
well and match the colour of these solutions with the
standard pH chart to estimate the pH.
(xi) Similarly observe the change in pH of 0.05 M H2SO4 and
0.1M NaOH solution with dilution as detailed in steps (i) to
(ix) above.
(xii) Record your observations in Table 5.2.
(xiii) Compare the result obtained by using universal indicator
paper and that obtained by using universal indicator
solution.
57
LABORATORY MANUAL CHEMISTRY
Result
(i) Concentration of solutions of test tube B, C and D are ____________.
(ii) Write your conclusion about the variation of pH with dilution.
Precautions
(a) Add equal number of drops of the universal indicator to equal amounts of solution
in each of the boiling tubes.
(b) Match the colour of the solution with pH chart carefully.
Discussion Questions
(i) What trend is observed in the variation of pH with dilution for acidic as well as for basic
solutions?
(ii) How do you explain the results of variation in pH with dilution?
(iii) If any two acidic solutions (say A and C) are mixed, what would happen to the pH of the
mixture? Verify your answer experimentally.
(iv) For each acidic solution, whether we use HCl or H2SO4, pH is same to a reasonably good
extent, even though HCl is 0.1M, and H2SO4 is 0.05M. How do you explain this result?
(v) Will the pH of 0.1M acetic acid be the same as that of 0.1M hydrochloric acid? Verify your
result and explain it?
EXPERIMENT 5.3
Aim
To study the variation in pH by common ion effect in case of weak
acids and weak bases.
58
PH AND PH CHANGE IN AQUEOUS SOLUTIONS
Theory
It is a known fact that the ionisation in the case of either a weak acid
or a weak base is a reversible process. This can be represented as:
(1) HA
H+ + A– (weak acid)
(2) BOH
+
B + OH
–
(weak base)
– +
The increase in concentration of A ions in case (1) and that of B
ions in case (2) would shift the equilibrium in the reverse direction
+ –
thereby decreasing the concentration of H ions and OH ions in
cases (1) and (2) respectively so as to maintain the constancy of
+
equilibrium constant K. This change either in H ion concentration
–
or OH ion concentration brings a change in the pH of the system,
which can be judged either with the help of a pH paper or by using
a universal indicator solution.
Material Required
• Sodium ethanoate : 2g
• Beakers (100 mL) : Four
• Ammonium chloride : 2g
• Pipettes (25 mL) : Two • Ethanoic acid (1.0 M) : 50 mL
• Test tubes : Four • Ammonia solution (1.0 M) : 50 mL
• pH chart : One • pH paper and
universal indicator : As per need
Procedure
(i) Take four 100 mL beakers and mark them as A, B, C and D.
Ammonia solution
(ii) Transfer 25 mL of 1M ethanoic acid in beaker ‘A’ and 25 mL
of (1M) ammonia solution in beaker ‘B’. Ethanoic acid
(iii) Similarly transfer 25 mL of (1 M) ethanoic acid in beaker ‘C’
and 25 mL of (1.0 M) ammonia solution in beaker ‘D’. Now
Ammonium chloride
add 2 g sodium ethanoate in beaker ‘C’ and dissolve it.
Likewise add 2 g of ammonium chloride in beaker ‘D’ and
dissolve it by shaking the content of the beaker thoroughly.
(iv) Take approximately 2 mL (20 drops) of the solution from
beakers A, B, C and D respectively into test tubes marked
as 1, 2, 3 and 4.
(v) In each of the test tubes add 2 drops of universal indicator
solution. Shake the content of the test tubes well and match
the colour in each case with the standard pH chart.
(vi) Record your observations as given in Table 5.3.
(vii) Compare pH of the solution in test tubes 1 and 3 and record
the change in pH.
(viii) Similarly compare pH of the solution in test tubes 2 and 4
and record the change in pH.
59
LABORATORY MANUAL CHEMISTRY
1 CH3COOH in water
3 CH3COOH + CH3COONa
4 NH4OH+NH4Cl
Result
Precautions
(a) Try only weak acid/weak base and its salt for the study of the common ion effect.
(b) Handle the bottle of ammonium hydroxide with care.
(c) Add equal number of drops of the universal indicator in each of the test tubes.
(d) Store pH papers at a safe and dry place.
Discussion Questions
(i) The addition of sodium acetate to acetic acid increases the pH whereas, the addition of
NH4Cl to aqueous NH3 solution (NH4OH) decreases the pH of the system. How do you
explain these observations?
(ii) Suggest suitable replacement for CH3COONa for system 3 and NH4Cl for system 4.
(iii) Suggest other pairs of weak acid and its salt and weak base and its salt to carry out the
present investigations.
(iv) In salt analysis/mixture analysis, point out the situations where the variation in pH is
carried out by common ion effect.
(v) How do buffer solutions resist change in the pH? Explain with a suitable example.
60
PH AND PH CHANGE IN AQUEOUS SOLUTIONS
EXPERIMENT 5.4
Aim
To study the change in pH during the titration of a strong acid
with a strong base by using universal indicator.
Theory
It is assumed that strong acids and strong bases are completely
dissociated in solution. During the process of neutralisation,
H+ ions obtained from the acid combine with the OH– ions produced
by base and form water. Therefore, when a solution of strong acid
is added to a solution of strong base or vice versa, the pH of the
solution changes. As the titration proceeds, initially there is slow
change in the pH but in the vicinity of the equivalence point there
is very rapid change in the pH of the solution.
Material Required
Procedure
(i) Take 25 mL hydrochloric acid solution (0.1 M) in 100 mL Hydrochloric acid
conical flask.
(ii) Add five drops of universal indicator solution to it. Sodium hydroxide
61
LABORATORY MANUAL CHEMISTRY
1. 0 0
2. 12.5 12.5
3. 10.0 22.5
4. 2.3 24.8
5. 0.1 24.9
6. 0.1 25.0
7. 0.1 25.1
8. 0.1 25.2
9. 0.1 25.3
Precautions
(a) To get good results perform the reaction with solutions of strong acid and strong
base of same concentration.
(b) Handle the bottle of acid and base with care.
(c) Use small amount of indicator.
Result
Write down your result on the basis of data.
Discussion Questions
(i) What trend of pH change will you observe in the neutralisation of strong acid with strong
base?
(ii) Do you expect the same trend of pH change for neutralisation of weak acid (acetic acid)
with a strong base (sodium hydroxide)?
(iii) In which pH range should the indicator show colour change if the hydrochloric acid is to be
neutralised by sodium hydroxide? Give answer after looking at the graph of the experiment.
(iv) Explain how does the study of pH change help in choosing the indicator for neutralisation
reaction.
62
PH AND PH CHANGE IN AQUEOUS SOLUTIONS
EXPERIMENT 5.5
Aim
To study pH of solutions of sodium chloride, ferric chloride and
sodium carbonate.
Theory
Salts of strong acid and strong base form neutral solutions while
salts of weak acid/base and strong base/acid are basic and acidic
respectively in nature. Salts of weak acid/base with strong base/
acid are hydrolysed in water while salts formed by neutralization
of strong acid and strong base do not hydrolyse in solution. You
have already learnt about this in your chemistry textbook.
Material Required
Procedure
(i) Take three boiling tubes and mark them as A, B and C.
(ii) Take 20 mL of 0.1 M solution(s) of NaCl, FeCl3 and Na2CO3
in boiling tubes A, B and C respectively.
(iii) Cut the pH paper in small pieces and spread the pieces on a
clean glazed tile.
(iv) Test the pH of the solution in boiling tubes A, B and C as in
the experiment 5.1.
(v) Arrange three clean test tubes in a test tube stand.
(vi) Number the test tubes as 1, 2 and 3.
(vii) Pour 4 mL solution from boiling tube A in each of the test
tubes.
(viii) Add 5 mL, 10 mL and 15 mL water in the test tubes 1, 2 and
3 respectively.
(ix) Note the pH of the solutions of test tubes 1, 2 and 3 with the
help of pH paper and universal indicator.
(x) Repeat the experiment with the solutions of boiling tubes B
and C.
(xi) Note your results in tabular form as in Table 5.5.
63
LABORATORY MANUAL CHEMISTRY
pH of solution
Solution
Test tube 1 Test tube 2 Test tube 3
NaCl
FeCl3
Na2CO3
Result
Write down the result on the basis of your observations.
Precautions
Discussion Questions
64
UNIT-6
TITRIMETRIC ANALYSIS
Y
OU are already aware that a substance is analysed to establish its qualitative
and quantitative chemical composition. Thus, chemical analysis can be
categorised as qualitative analysis and quantitative analysis. In this unit
you will learn about determination of the amount of substance in solution. Depending
upon the method adopted for determining the amount of chemical substances in
solution, there are two methods of analysis namely, titrimetric analysis and
gravimetric analysis. In titrimetric analysis measurement of only volumes is involved
while in gravimetric analysis measurement of volumes as well as mass is involved.
Titrimetric analysis involves determination of the volume of a solution of
accurately known concentration, which is required to react quantitatively with
the measured volume of the solution of a substance, concentration of which is to
be determined. The solution of accurately known concentration is called standard
solution. The mass of the substance dissolved in the solution of unknown
concentration is calculated from the volume of the standard solution used, the
chemical equation and the relative molecular masses of the reacting compounds.
The reagent of known concentration is called titrant and the substance being
titrated is termed as titrand.
To carry out titrimetric analysis, standard solution is usually added from
the long graduated tube called burette. The process of adding the standard
solution to the solution of unknown concentration until the reaction is just
complete is called titration. The point at which reaction is completed is called
equivalence point or the theoretical or stoichiometric end point. It is not
possible all the time to take standard solution in the burette. You will come to know
about it later in this unit in the titration of sodium hydroxide with oxalic acid.
66
TITRIMETRIC ANALYSIS
67
LABORATORY MANUAL CHEMISTRY
Methyl orange
Methyl orange is a weak base and is yellow in colour in the unionised
form. Sodium salt of methyl orange is represented as follows:
Choice of Indicator
In the titration of strong acid and a weak base, methyl orange is
chosen as indicator. When titration between strong base and weak
acid is to be performed then phenolphthalein is a good indicator.
In this case alkali is dropped from the burette and acid is taken in
the tiration flask. Colour of the solution taken in the titration flask
68
TITRIMETRIC ANALYSIS
EXPERIMENT 6.1
Aim
Determination of the concentration (strength) of a given sodium
hydroxide solution by titrating it against a standard solution of
oxalic acid.
Theory
In the titration of a strong acid with a strong base, the amount of
acid and base becomes chemically equivalent at the end point and
the chemical reaction is called neutralization reaction. Near the
end point there is a sudden change in the pH of the solution. If
after end point even a small amount of base/acid is added the
solution would become slightly alkaline or acidic respectively. In
the titration between oxalic acid (weak acid) and sodium hydroxide
(strong base), following reaction takes place:
a1 M1 V1 = a2 M2 V2 ...(4)
69
LABORATORY MANUAL CHEMISTRY
Material Required
Procedure
70
TITRIMETRIC ANALYSIS
(viii) Read the lower meniscus of the solution in the burette again
and record it as final reading.
(ix) Repeat the procedure until three concordant readings are
obtained. Record your readings as in Table 6.1.
Table 6.1 : Titration of sodium hydroxide vs oxalic acid solution
71
LABORATORY MANUAL CHEMISTRY
Calculations
Molarity of NaOH solution can be calculated by using the equation:
Oxalic acid Sodium hydroxide
a1 M1V1 = a2 M2V2
where, M1 and V1 are the molarity and volume of the oxalic
acid solution.
M2 and V2 are the molarity and volume of the sodium hydroxide
solution.
a1 and a2 are respectively the basicity of oxalic acid and acidity
of sodium hydroxide. In this case a1= 2 and a2 = 1.
–1
Also, Molar mass of oxalic acid, (COOH) 2.2H2O = 126 g mol
–1
and Molar mass of sodium hydroxide (NaOH) = 40 g mol
Calculate the concentration of sodium hydroxide solution in g/L
by using the equation given below.
Concentration (strength) in g/L = Molarity×Molar mass
Result
Concentration of NaOH solution is ——————— g/L.
Precautions
(a) Always rinse the burette with the solution, which is to be taken in it.
(b) Remove the air gap if any, from the burette before titrating the solution. Make
sure that the nozzle of burette is also filled.
(c) Never forget to remove the funnel from the burette before noting the readings of
the burette and ensure that no drop is hanging from the nozzle of the burette.
(d) Always read the lower meniscus for all transparent solutions and upper meniscus
for coloured solutions.
(e) To note the burette readings place the eye exactly at the level of the meniscus.
(f) Never hold the pipette at the bulb.
(g) Never use the pipette and burette with a broken nozzle.
(h) Never suck a strong acid or an alkali with the pipette.
(i) Always keep the lower end of the pipette dipped in the liquid while sucking the
liquid.
(j) Do not blow out the last drop of the solution from the jet end of the pipette into
the flask.
(k) The concentration (strength) of the solution must be calculated up to the fourth
place of decimal.
72
TITRIMETRIC ANALYSIS
Discussion Questions
(i) Why are the burette and the pipette rinsed with the solution with which these are filled?
(ii) What is an indicator? Which indicator is used in the titration of oxalic acid vs sodium
hydroxide? Can the titration be performed by using some other indicator?
(iii) Why should one read the lower meniscus in the case of colourless and transparent solutions
and the upper meniscus for solutions of dark colour?
(iv) Explain the term ‘end point’?
(v) What do you mean by 1.0 M solution?
(vi) Why should the last drop of the solution not be blown out of a pipette?
(vii) Explain the term basicity of an acid and acidity of a base?
(viii) For titrating NaOH vs HCl, phenolphthalein and methyl orange, both are suitable indicators.
Why?
(ix) What is meant by the term , ‘concordant readings’?
(x) Can one take oxalic acid solution in the burette and sodium hydroxide solution in the
titration flask? Point out the limitations of doing so if any.
The complete neutralisation is possible only when the amount of alkali is in equivalent
proportion to the amount of acid. Therefore, at the end point equivalent mass of acid dissolved
in volume V1 of solvent should be equal to the equivalent mass of the base dissolved in
Volume V2 of solvent. If N1 and N2 are equivalent masses of acid and base respectively dissolved
in per litre of solution then N1V1 = N2V2 … (i)
Equivalent mass of acids and bases is given by the following expression:
molar mass
Equivalent mass of acid = … (ii)
basicity
molar mass
Equivalent mass of base = ... (iii)
acidity
The number of gram equivalent mass of solute dissolved in one litre of the solution is
called the normality of the solution. For acids and bases
Number of gram equivalent mass w/ Equivalent mass
Normality (N)= = … (iv)
Volume of solution in litre (V ) Volume of solution in litre (V )
Where w = mass of substance in grams
73
LABORATORY MANUAL CHEMISTRY
Molar mass
Equivalent mass = … (vi)
a
From equations (v) and (vi) we can write
w Molar mass
=
N ×V a
a (w/Molar mass )
Or N=
V
w/Molar mass
But is the molarity (M)
V
Therefore, N = a M … (vii)
Equation (vii) is the expression for the relationship between normality and molarity.
By using equation (vii) in equation (i) we have a1M1V1 = a2M2V2 .... (viii)
Where a1 and a2 are basicity and acidity of acid and base respectively and M1 and M2 are
the molar masses of acid and base respectively. Thus we see that equation (i) can also be
used to calculate the strength of the solution. Equation (viii) can be used for making the
solution by dilution. For solutions of the same substance a1 = a2. Therefore for using equation
(viii) for dilution of solution –
M1V1 = M2V2 ...(ix)
Therefore, to obtain V2 volume of a solution of molarity M2 from a solution of molarity M1,
the volume V1 of the solution of molarity M1 which is required for dilution, can be calculated
from equation (ix). (V2–V1) volume of solvent will be required to be added to V1 volume of the
solution of molarity M1.
EXPERIMENT 6.2
Aim
Preparation of (0.1 M) standard solution of sodium carbonate.
Theory
Sodium carbonate has characteristics nearer to the primary
standards therefore its standard solution can be made by direct
weighing.
To prepare 0.1 M Na2CO3 solution, 10.6000g of sodium
carbonate should be dissolved per litre of the solution (Molar mass
–1
of sodium carbonate is 106 g mol ).
Therefore, to prepare 100 mL of 0.1M Na2CO3 solution 1.0600 g
of sodium carbonate is dissolved in minimum quantity of water
and the solution is diluted to exactly 100 mL by adding water to it.
74
TITRIMETRIC ANALYSIS
Material Required
Procedure
Follow the same procedure as in Experiment 2.1.
EXPERIMENT 6.3
Aim
Determination of the strength of a given solution of dilute
hydrochloric acid by titrating it against a standard solution of sodium
carbonate.
Theory
The strength of hydrochloric acid is determined by titrating it against
a standard solution of sodium carbonate. The following reaction
takes place:
Na2CO3 + 2HCl → 2 NaCl + CO2 + H2O
In this titration, methyl orange, a weak base (yellow in the
unionised form) is used as an indicator.
In this experiment also, the titration follows the usual course,
i.e., the proton furnished by the addition of the acid first neutralises
sodium carbonate solution. When the entire sodium carbonate
solution is neutralised, the last drop of the acid added from the burette
produces the pinkish red colour change, which is the end point.
The concentration (strength) of the unknown solution is
calculated in g/L. It is calculated from the molarity of the solution.
Here, the molarity equation is written as
Base Acid
a1M1V1 = a2M2V2
where, a1 and a2 are the acidity and basicity of the alkali and the
acid respectively. M1 and M2 are the molarities, V1 and V2 are the
volumes of the base and acid respectively used to neutralise each
other.
75
LABORATORY MANUAL CHEMISTRY
Material Required
Procedure
(A) Preparation of 0.1 M standard solution of sodium
carbonate
Hydrochloric acid
Follow the procedure as described in Experiment 2.1.
(B) Titration of hydrochloric acid and standard sodium
carbonate solution.
Follow the procedure as given in the Experiment 6.1.
In this case, hydrochloric acid is taken in the burette and
sodium carbonate solution in the conical flask. Methyl orange is
used as an indicator. The colour change at the end point will be
from yellow to pinkish-red. Record your observations in Table 6.2.
Table 6.2 : Titration of Hydrochloric acid with standard sodium carbonate solution
76
TITRIMETRIC ANALYSIS
Calculations
Calculate the strength of HCl solution by using the equation
Na2CO3 solution HCl solution
a1M1V1 = a2M2V2
where M 1 and V1 are the molarity and volume of sodium carbonate solution
–
respectively and a1 is the number of moles of OH (aq) ions supplied by one
mole of the base (i.e. the acidity of the Na2CO3 solution).
∴ a1 = 2
∴ a2 = 1
–1 –1
Molar mass of Na2CO3 = 106 g mol , Molar mass of HCl = 36.5 g mol ,
Result
The concentration (strength) of the given HCl solution is _______g/L.
Precautions
(a) Care should be taken while handling the acid and base.
(b) Always rinse the burette and the pipette with the solution which is to be taken in
them.
(c) Remove the air gap if any, from the burette before titration.
(d) Never forget to remove the funnel from the burette before noting the initial reading
of the burette and ensure that no drop is hanging from the nozzle.
(e) Always read the lower meniscus for all transparent solutions and upper meniscus
for the coloured solutions.
(f) Never use burette and pipette with a broken nozzle.
(g) Never suck a strong acid or an alkali with the pipette, use pipette bulb.
(h) Always keep the lower end of the pipette dipped in the liquid while sucking the
liquid.
(i) While transferring the solution to the flask, do not blow out the last drop of the
solution from the jet of the pipette.
(j) The strength of the solution must be calculated up to the fourth decimal place.
77
LABORATORY MANUAL CHEMISTRY
Discussion Questions
(i) Which indicator is used in the titration of sodium carbonate against hydrochloric acid and
what is the colour change at the end point?
(ii) How will you prepare 250 mL of 0.05 M solution of sodium carbonate?
(iii) Though sodium carbonate is a salt yet its aqueous solution is weakly alkaline in nature.
Explain why?
(iv) How can you determine the acidity of sodium carbonate solution?
(v) Why is methyl orange not an Arrhenius base?
(vi) How can you titrate a solution of the mixture of Na2CO3 and NaHCO3 against HCl?
(vii) What is the difference between an end point and an equivalence point?
(viii) Can you directly prepare standard solution of HCl, HNO3 and H2SO4 ?
78
UNIT-7
SYSTEMATIC QUALITATIVE
ANALYSIS
A
NALYSIS always does not mean breaking of substance into its ultimate
constituents. Finding out the nature of substance and identity of
its constituents is also analysis and is known as qualitative analysis.
Qualitative analysis of inorganic salts means the identification of cations and
anions present in the salt or a mixture of salts. Inorganic salts may be obtained
by complete or partial neutralisation of acid with base or vice-versa. In the
formation of a salt, the part contributed by the acid is called anion and the part
contributed by the base is called cation. For example, in the salts CuSO4 and
2+ 2– –
NaCl, Cu and Na+ ions are cations and SO4 and Cl ions are anions. Qualitative
analysis is carried out on various scales. Amount of substance employed in
these is different. In macro analysis, 0.1 to 0.5 g of substance and about 20 mL
of solution is used. For semimicro analysis, 0.05 g substance and 1 mL solution
is needed while for micro analysis amount required is very small. Qualitative
analysis is carried out through the reactions which are easily perceptible to our
senses such as sight and smell. Such reactions involve:
(a) Formation of a precipitate
(b) Change in colour
(c) Evolution of gas etc.
Systematic analysis of an inorganic salt involves the following steps:
(i) Preliminary examination of solid salt and its solution.
(ii) Determination of anions by reactions carried out in solution (wet tests)
and confirmatory tests.
(iii) Determination of cations by reactions carried out in solution (wet tests)
and confirmatory tests.
Preliminary examination of a salt often furnishes important information, which
simplifies further course of analysis. Although these tests are not conclusive but
sometimes they give quite important clues for the presence of certain anions or
cations. These tests can be performed within 10–15 minutes. These involve noting
the general appearance and physical properties, such as colour, smell, solubility
etc. of the salt. These are named as dry tests.
Heating of dry salt, blow pipe test, flame tests, borax bead test, sodium
carbonate bead test, charcoal cavity test etc. come under dry tests. Some of these
tests are given later in this unit.
LABORATORY MANUAL CHEMISTRY
EXPERIMENT 7.1
Aim
To detect one cation and one anion in the given salt from the following ions:
2+ 2+ 3+ 3+ 3+ 2+ 2+ 2+ 2+ 2+ 2+ 2+
Cations - Pb , Cu , As , Al , Fe , Mn , Ni , Zn , Co , Ca , Sr , Ba ,
2+ +
Mg , NH 4
2– 2– 2– 2– – – – – – 3– 2–
Anions - CO3 , S , SO3 , SO 4 , NO2 , NO3 , Cl , Br , I , PO 4 , C 2 O 4 ,
–
CH3COO .
(Insoluble salts to be excluded)
Theory
Two basic principles of great use in the analysis are:
(i) the Solubility product and
(ii) the Common ion effect
When ionic product of a salt exceeds its solubility product, precipitation takes
place. Ionic product of salt is controlled by making use of common ion effect
which you have studied in the textbook of chemistry.
Material Required
80
SYSTEMATIC QUALITATIVE ANALYSIS
Procedure
(a) Take 0.1 g of the salt in a test tube and add 1–2 mL of
dilute sulphuric acid. Observe the change, if any, at
room temperature. If no gas is evolved, warm the
Fig. 7.1 : Testing a Gas
content of the test tube. If gas is evolved test it by using
the apparatus shown in Fig.7.1 and identify the gas
evolved (See Table 7.1).
Inference
Observations
Gas evolved Possible Anion
81
LABORATORY MANUAL CHEMISTRY
2- 2– 2- – –
Confirmatory tests for CO3 S , SO3 , NO2 and CH3COO
Confirmatory (wet) tests for anions are performed by using water extract when
salt is soluble in water and by using sodium carbonate extract when salt is
2–
insoluble in water. Confirmation of CO3 is done by using aqueous solution of
the salt or by using solid salt as such because sodium carbonate extract contains
carbonate ions. Water extract is made by dissolving salt in water. Preparation of
sodium carbonate extract is given below.
*Sulphite ( SO3 )
2–
(a) Take 1 mL of water extract or sodium carbonate
extract in a test tube and add barium chloride
solution. A white precipitate is formed which dissolves
in dilute hydrochloric acid and sulphur dioxide gas
is also evolved.
(b) Take the precipitate of step (a) in a test tube and add
a few drops of potassium permanganate solution
acidified with dil. H 2 SO 4 . Colour of potassium
permanganate solution gets discharged.
– (a) Take 1 mL of water extract in a test tube. Add a few
Nitrite ( NO2 )
drops of potassium iodide solution and a few drops of
starch solution, acidify with acetic acid. Blue colour
appears.
(b) Acidify 1 mL of water extract with acetic acid. Add
2-3 drops of sulphanilic acid solution followed by 2-3
drops of 1-naphthylamine reagent. Appearance of red
colour indicates the presence of nitrite ion.
* Like CO2 sulphur dioxide also turns lime water milky. But CO2 is odourless gas and SO2 has a
characteristic smell.
82
SYSTEMATIC QUALITATIVE ANALYSIS
–
Acetate (CH3COO ) (a) Take 0.1 g of salt in a china dish. Add 1 mL of ethanol
and 0.2 mL conc. H 2SO 4 and heat. Fruity odour
confirms the presence of acetate ion.
(b) Take 0.1 g of salt in a test tube, add 1-2 mL distilled
water, shake well filter if necessary. Add 1 to 2 mL
neutral** ferric chloride solution to the filtrate. Deep
red colour appears which disappears on boiling and
a brown-red precipitate is formed.
** Prepareation of neutral Ferric Chloride : Add dilute NaOH solution to ferric chloride solution drop by drop
with shaking until a small but permanent precipitate of ferric hydroxide is obtained. Filter the precipitate
and use the filtrate for analysis.
If CO2 gas is passed in excess through lime water, the milkiness produced
disappears due to the formation of calcium hydrogen carbonate which is soluble
in water.
2–
2. Test for Sulphide ion [S ]
(a) With warm dilute H2SO4 a sulphide gives hydrogen sulphide gas which
smells like rotten eggs. A piece of filter paper dipped in lead acetate
solution turns black on exposure to the gas due to the formation of
lead sulphide which is black in colour.
Na2S + H2SO4 → Na2SO4 + H2S
(CH3COO)2Pb + H2S → PbS + 2CH3COOH
Lead sulphide
Black precipitate
(b) If the salt is soluble in water, take the solution of salt in water make it
alkaline with ammonium hydroxide and add sodium nitroprusside
solution. If it is insoluble in water take sodium carbonate extract and
add a few drops of sodium nitroprusside solution. Purple or violet
83
LABORATORY MANUAL CHEMISTRY
Barium
The gas turns potassium dichromate paper acidified with dil. H2SO4, green.
compounds
K2Cr2O7 + H2SO4 + 3SO2 → K2SO4 + Cr2 (SO4)3 + H2O
Chromium
sulphate (green)
Potassium (b) An aqueous solution or sodium carbonate extract of the salt produces a
permanganate white precipitate of barium sulphite on addition of barium chloride solution.
Na2SO3 + BaCl2 → 2NaCl + BaSO3
This precipitate gives following tests.
(i) This precipitate on treatment with dilute HCl, dissolves due to
decomposition of sulphite by dilute HCl. Evolved SO2 gas can be tested.
BaSO3 + 2HCl → BaCl2 + H2O + SO2
(ii) Precipitate of sulphite decolourises acidified potassium permanganate
solution.
BaSO3 + H2SO4 → BaSO4 + H2O + SO2
2KMnO4 + 3H2SO4 → K2SO4 + 2MnSO4 + 3H2O + 5 [O]
SO2 + H2O + [O] → H2SO4
–
4. Test for Nitrite ion [NO2 ]
(a) On treating a solid nitrite with dil. H2SO4 and warming , reddish brown
fumes of NO2 gas are evolved. Addition of potassium iodide solution to
the salt solution followed by freshly prepared starch solution and
acidification with acetic acid produces blue colour. Alternatively, a filter
paper moistened with potassium iodide and starch solution and a few
drops of acetic acid turns blue on exposure to the gas due to the
interaction of liberated iodine with starch.
(i) 2NaNO2 + H2SO4 → Na2SO4 + 2HNO2
3HNO2 → HNO3 + 2NO + H2O
2NO + O2 → 2NO2
Brown gas
84
SYSTEMATIC QUALITATIVE ANALYSIS
– –
(ii) NO2 + CH3COOH → HNO2 + CH3COO
85
LABORATORY MANUAL CHEMISTRY
(b) Acetate gives deep red colour on reaction with neutral ferric chloride
solution due to the formation of complex ion which decomposes on
heating to give Iron (III) dihydroxyacetate as brown red precipitate.
– 3+ + +
6 CH3COO + 3Fe + 2H2O → [Fe3(OH)2 (CH3COO)6] + 2H
+ +
[Fe3(OH)2 (CH3COO)6] + 4H2O → 3[Fe (OH)2 (CH3COO)] + 3CH3COOH + H
Iron(III)dihydroxyacetate
(Brown-red precipitate)
Inference
Observations Gas/vapours evolved Possible anions
86
SYSTEMATIC QUALITATIVE ANALYSIS
– – – 2–
Table 7.4 : Confirmatory tests for Cl , Br , I , NO3– and C2O4
Chloride (Cl )
–
(a) Take 0.1 g of salt in a test tube, add a pinch of
manganese dioxide and 3-4 drops of conc. sulphuric
acid. Heat the reaction mixture. Greenish yellow
chlorine gas is evolved which is detected by its pungent
odour and bleaching action.
(b) Take 1 mL of sodium carbonate extract in a test tube,
acidfy it with dil. HNO3 or take water extract and add silver
nitrate solution. A curdy white precipitate is obtained
which is soluble in ammonium hydroxide solution.
(c) Take 0.1 g salt and a pinch of solid potassium
dichromate in a test tube, add conc. H2SO4, heat and
pass the gas evolved through sodium hydroxide
solution. It becomes yellow. Divide the solution into
two parts. Acidify one part with acetic acid and add
lead acetate solution. A yellow precipitate is formed.
Acidify the second part with dilute sulphuric acid and
add 1 mL of amyl alcohol followed by 1 mL of 10%
hydrogen peroxide. After gentle shaking the organic
layer turns blue.
–
Bromide (Br ) (a) Take 0.1 g of salt and a pinch of MnO2 in a test tube.
Add 3-4 drops conc.sulphuric acid and heat. Intense
brown fumes are evolved.
(b) Neutralise 1 mL of sodium carbonate extract with
hydrochloric acid (or take the water extract). Add 1
mL carbon tetrachloride (CCl4)/chloroform (CHCl3)/
carbon disulphide. Now add an excess of chlorine
water dropwise and shake the test tube. A brown
colouration in the organic layer confirms the presence
of bromide ion.
(c ) Acidify 1 mL of sodium carbonate extract with dil.
HNO3 (or take 1 mL water extract) and add silver
nitrate solution. A pale yellow precipitate soluble with
difficulty in ammonium hydroxide solution is obtained.
–
Iodide ( I ) (a) Take 1 mL of salt solution neutralised with HCl and
add 1 mL chloroform/carbon tetrachloride/carbon
disulphide. Now add an excess of chlorine water drop
wise and shake the test tube. A violet colour appears
in the organic layer.
(b) Take 1 mL of sodium carbonate extract acidify it with
dil. HNO3 (or take water extract). Add, silver nitrate
solution. A yellow precipitate insoluble in NH 4OH
solution is obtained.
87
LABORATORY MANUAL CHEMISTRY
Hazard Warning (c) Salt solution acidified with dilute HNO3 on addition of silver
nitrate solution gives a curdy white precipitate soluble in
• The solution obtained after ammonium hydroxide solution. This indicates the presence
–
dissolving AgCl/AgBr/AgI of Cl ions in the salt.
precipitate in ammonium
hydroxide should be NaCl + AgNO3 → NaNO3 + Ag Cl
acidified with 2M HNO 3 Silver chloride
and should be discarded (White precipitate)
quickly to avoid serious
explosion. AgCl + 2NH4OH → [Ag(NH3)2 ]Cl + 2H2O
Diammine silver (I)
chloride
* This test can also be performed by adding first ferrous sulphate solution and then conc. H2SO4 .
88
SYSTEMATIC QUALITATIVE ANALYSIS
(d) Mix a little amount of salt and an equal amount of solid potassium
dichromate (K2Cr2O7) in a test tube and add conc. H2SO4 to it. Heat the
test tube and pass the evolved gas through sodium hydroxide solution.
If a yellow solution is obtained, divide the solution into two parts. Acidify
the first part with acetic acid and then add lead acetate solution.
Formation of a yellow precipitate of lead chromate confirms the presence
of chloride ions in the salt. This test is called chromyl chloride test.*
4NaCl + K2Cr2O7 + 6H2SO4 → 2KHSO4 + 2CrO2Cl2 + 4NaHSO4 + 3H2O Chromyl
(Chromyl chloride
chloride)
CrO2Cl2 + 4NaOH → Na2CrO4 + 2NaCl + 2H2O
Lead
(CH3COO)2Pb + Na2CrO4 → PbCrO4 + 2CH3COONa chromate
Sodium Lead chromate
chromate (Yellow precipitate)
Acidify the second part with dilute sulphuric acid and add small amounts of
amyl alcohol and then 1 mL of 10% hydrogen peroxide solution. On gentle shaking
2–
organic layer turns blue. CrO4 ion formed in the reaction of chromyl chloride
with sodium hydroxide reacts with hydrogen peroxide to form chromium pentoxide
(CrO5) (See structure) which dissolves in amyl alcohol to give blue colour.
2– +
CrO4 + 2H + 2H2O2 → Cr O5 + 3H2O
Chromium
pentoxide
–
2. Test for Bromide ion (Br )
If on heating the salt with conc. H2SO4 reddish brown fumes of bromine are
–
evolved in excess, this indicates the presence of Br ions. The fumes get intensified
on addition of MnO2. Bromine vapours turn starch paper yellow.
Bromine
2NaBr + 2H2SO4 → Br2 + SO2 + Na2SO4 + 2H2O very toxic
by
2NaBr + MnO2 + 2H2SO4 → Na2SO4 + MnSO4 + 2H2O + Br2 inhalation
corrosive
(a) Add 1 mL of carbon tetrachloride (CCl4)/chloroform (CHCl3)** and excess
of freshly prepared chlorine water dropwise to the salt solution in water
or sodium carbonate extract neutralised with dilute HCl. Shake the test
tube vigorously. The appearance of an orange brown colouration in the
organic layer due to the dissolution of bromine in it, confirms the
presence of bromide ions.
2NaBr + Cl2 → 2NaCl + Br2
3+
* Chromyl chloride test should be performed with minimum amount of substance to avoid pollution by Cr
ions.
** In place of carbon tetrachloride or chloroform, carbon disulphide or dichloromethane (CH2Cl2) can also be
used.
89
LABORATORY MANUAL CHEMISTRY
(b) Acidify the sodium carbonate extract of the salt with dil. HNO3. Add
silver nitrate (AgNO3) solution and shake the test tube. A pale yellow
precipitate is obtained which dissolves in ammonium hydroxide with
difficulty.
NaBr + AgNO3 → NaNO3 + AgBr
Silver bromide
Pale yellow precipitate
–
3. Test for Iodide ion ( I )
(a) If on heating the salt with conc. H2SO4 , deep violet vapours with a
pungent smell are evolved. These turns starch paper blue and a violet
sublimate is formed on the sides of the test tube, it indicates the presence
–
of I ions. Some HI, sulphur dioxide, hydrogen sulphide, and sulphur
are also formed due to the following reactions.
Iodine,
harmful by
2NaI + 2H2SO4 → Na2SO4 + SO2 + 2H2O + I2
inhalation
and I2 + Starch → Blue colour
contact solution
with skin
Chloroform,
6NaI + 4H2SO4 → 3I2 + 4H2O +S + 3Na2SO4
harmful and
toxic by 8NaI + 5 H2SO4 → 4I2 + H2S + 4Na2SO4 + 4H2O
inhalation
On adding MnO2 to the reaction mixture, the violet vapours become
dense.
2NaI + MnO2 + 2H2SO4 → I2 + MnSO4 + Na2SO4 + 2H2O
(b) Add 1 mL of CHCl3 or CCl4 and chlorine water in excess to the salt
solution in water or sodium carbonate extract neutralised with dil.HCl
and shake the test tube vigorously. Presence of violet colouration in the
organic layer confirms the presence of iodide ions.
2NaI + Cl2 → 2NaCl + I2
Iodine dissolves in the organic solvent and the solution becomes violet.
(c) Acidify sodium carbonate extract of the salt with dil.HNO3 and add
AgNO3 solution. Appearance of a yellow precipitate insoluble in excess
of NH4OH confirms the presence of iodide ions.
NaI + AgNO3 → AgI + NaNO3
silver iodide
(Yellow precipitate)
90
SYSTEMATIC QUALITATIVE ANALYSIS
–
4. Test for Nitrate ion [ NO3 ]
(a) If on heating the salt with conc. H2SO4 light brown fumes are evolved
then heat a small quantity of the given salt with few copper turnings or
chips and conc. H2SO4. Evolution of excess of brown fumes indicates
the presence of nitrate ions. The solution turns blue due to the formation
of copper sulphate. Copper
sulphate
NaNO3 + H2SO4 → NaHSO4 + HNO3
4HNO3 → 4NO2 + O2 + 2H2O
2NaNO3 + 4H2SO4 + 3Cu → 3 CuSO4 + Na2SO4 + 4H2O + 2NO
Nitric
Copper sulphate
acid
(Blue)
2NO + O2 → 2NO2
(Brown fumes)
(b) Take 1 mL of an aqueous solution of the salt and add 2 mL conc. H2SO4 Oxalates
slowly. Mix the solutions thoroughly and cool the test tube under the
tap. Now, add freshly prepared ferrous sulphate solution along the sides
of the test tube dropwise so that it forms a layer on the top of the liquid
already present in the test tube. A dark brown ring is formed at the
junction of the two solutions due to the formation of nitroso ferrous
sulphate (Fig. 7.2). Alternatively first ferrous sulphate is added and
then concentrated sulphuric acid is added.
91
LABORATORY MANUAL CHEMISTRY
Pass the gas evolved through lime water. A white precipitate is formed
which dissolves on passing the gas for some more time.
92
SYSTEMATIC QUALITATIVE ANALYSIS
2–
1. Test of Sulphate ions [SO4 ]
(a) Aqueous solution or sodium carbonate extract of the salt acidified with
acetic acid on addition of barium chloride gives a white precipitate of
barium sulphate insoluble in conc. HCl or conc. HNO3 .
3–
2. Test for Phosphate ion [PO4 ]
(a) Add conc. HNO3 and ammonium molybdate solution to the test solution
containing phosphate ions and boil. A yellow colouration in solution
or a canary yellow precipitate of ammonium-phosphomolybdate,
(NH4)3[P (Mo3O10)4] is formed. Each oxygen of phosphate has been
replaced by Mo3O10 group.
The tests for cations may be carried out according to the following scheme.
1. Colour Test
Observe the colour of the salt carefully, which may provide useful information
about the cations. Table 7.6 gives the characteristic colours of the salts of some
cations.
93
LABORATORY MANUAL CHEMISTRY
Table 7.7 : Inferences from the colour of the salt in cold and on heating
3. Flame Test
The chlorides of several metals impart characteristic colour to the flame because
they are volatile in non-luminous flame. This test is performed with the help of a
platinum wire as follows :
(i) Make a tiny loop at one end of a platinum wire.
(ii) To clean the loop dip it into concentrated hydrochloric acid and hold it in a
non-luminous flame (Fig. 7.3).
(iii) Repeat step (ii) until the wire imparts no colour to the flame.
(iv) Put 2-3 drops of concentrated hydrochloric acid on a clean watch glass
and make a paste of a small quantity of the salt in it.
(v) Dip the clean loop of the platinum wire in this paste and introduce the loop
in the non-luminous (oxidising) flame (Fig. 7.3).
(vi) Observe the colour of the flame first with the naked eye and then through
a blue glass and identify the metal ion with the help of Table 7.8.
94
SYSTEMATIC QUALITATIVE ANALYSIS
95
LABORATORY MANUAL CHEMISTRY
96
SYSTEMATIC QUALITATIVE ANALYSIS
(a) (b)
Fig. 7.6 : (a) Making charcoal cavity (b) Heating salt in the cavity
(iii) Moisten the salt in the cavity with one or two drops of water, otherwise
salt/mixture will blow away.
(iv) Use a blowpipe to heat the salt in a luminous (reducing) flame and
observe the colour of oxide/ metallic bead formed in the cavity both
when hot and cold [ Fig. (7.6 b)]. Obtain oxidising and reducing flame as
shown in Fig. 7.7 a and b.
(v) Always bore a fresh cavity for testing the new salt.
Fig. 7.7 : Obtaining oxidising and reducing flame (a) Oxidising flame (b) Reducing
flame
97
LABORATORY MANUAL CHEMISTRY
Heat
CuO + C
→ Cu + CO
Red colour
In case of ZnSO4 :
Heat
ZnSO4 + Na 2 CO3 → ZnCO3 + Na 2 SO4
Heat
ZnCO3 → ZnO + CO2
Yellow when hot,
White when cold
Yellow residue when hot and grey metal when cold Pb2+
White residue with the odour of garlic As3+
Brown residue Cd2+
Yellow residue when hot and white when cold Zn2+
98
SYSTEMATIC QUALITATIVE ANALYSIS
Group Analysis
(a ) Take 0.1 g of salt in a test tube and add 1-2 mL of NaOH solution to
it and heat. If there is a smell of ammonia, this indicates the presence
of ammonium ions. Bring a glass rod dipped in hydrochloric acid
near the mouth of the test tube. White fumes are observed.
(b) Pass the gas through Nessler’s reagent. Brown precipitate is obtained.
+
Chemistry of Confirmatory Tests for NH4 ion
99
LABORATORY MANUAL CHEMISTRY
Flow Chart*
Original Solution
Dil.HCl
100
SYSTEMATIC QUALITATIVE ANALYSIS
Experiment Observation
Dissolve the precipitate in hot water and divide
the hot solution into three parts.
1. Add potassium iodide solution to the first A yellow precipitate is obtained.
part.
2. To the second part add potassium chromate A yellow precipitate is obtained which
solution. is soluble in NaOH and insoluble in
ammonium acetate solution.
3. To the third part of the hot solution add few A white precipitate is obtained
drops of alcohol and dilute sulphuric acid. which is soluble in ammonium
acetate solution.
2+
Chemistry of the Confirmatory Tests of Pb ions
Lead is precipitated as lead chloride in the first group. The precipitate is soluble
in hot water.
1. On adding potassium iodide (KI) solution, a yellow precipitate of lead
2+
iodide is obtained which confirms the presence of Pb ions.
PbCl2 + 2KI → PbI2 + 2KCl
(Hot solution) Yellow precipitate
* Here only those cations are given which are in the syllabus.
101
LABORATORY MANUAL CHEMISTRY
2+ 2+
Black precipitate of Group II A ions (Pb , Cu ) If a yellow precipitate soluble in
insoluble in yellow ammonium sulphide is formed. yellow ammonium sulphide is
3+
formed then As ion is present.
Boil the precipitate of Group II A with dilute nitric Acidify this solution with dilute
acid and add a few drops of alcohol and dil. H2SO4. HCl. A yellow precipitate is formed.
Heat the precipitate with
concentrated nitric acid and add
White precipitate confirms If no precipitate is
2+ ammonium molybdate solution. A
the presence of Pb ions. formed, add excess of canary yellow precipitate is formed.
Dissolve the precipitate in ammonium hydroxide
ammonium acetate solution. A blue solution
solution. Acidify with is obtained, acidify it
acetic acid and divide the with acetic acid and add
solution into two parts. potassium ferrocyanide
(i) To the first part add solution. A chocolate
potassium chromate brown precipitate is
solution, a yellow formed.
precipitate is formed.
(ii) To the second part,
add potassium iodide
solution, a yellow
precipitate is formed.
2+
1. Test for Lead ion (Pb )
Lead sulphide precipitate dissolves in dilute HNO3. On adding dil. H2SO4 and a
few drops of alcohol to this solution a white precipitate of lead sulphate appears.
This indicates the presence of lead ions.
3PbS + 8HNO3 → 3Pb (NO3)2 + 2NO + 4H2O + 3S
103
LABORATORY MANUAL CHEMISTRY
(a) Copper sulphide dissolves in nitric acid due to the formation of copper
nitrate.
3CuS + 8HNO3 → 3Cu(NO3)2 + 2NO + 3S + 4H2O
On heating the reaction mixture for long time, sulphur is oxidised to
sulphate and copper sulphate is formed and the solution turns blue. A
small amount of NH4OH precipitates basic copper sulphate which is soluble
in excess of ammonium hydroxide due to the formation of
tetraamminecopper (II) complex.
S + 2HNO3 → H2SO4 + 2NO
2− +
2Cu2++ SO 4 +2NH3+2H2O → Cu(OH)2. CuSO4+ 2NH4
– 2−
Cu(OH)2.CuSO4 + 8NH3 → 2 [Cu(NH3)4]SO4 + 2OH + SO 4
Tetraamminecopper (II)
sulphate (Deep blue)
(b) The blue solution on acidification with acetic acid and then adding
potassium ferrocyanide [K4Fe(CN)6 ] solution gives a chocolate colouration
due to the formation of copper ferrocyanide i.e.Cu2[Fe(CN)6].
[Cu(NH3)4] SO4 + 4CH3COOH → CuSO4 + 4CH3COONH4
104
SYSTEMATIC QUALITATIVE ANALYSIS
If group-II is absent, take original solution and add 2-3 drops of conc. HNO3 to
oxidise Fe2+ ions to Fe3+ ions. Heat the solution for a few minutes. After cooling
add a small amount of solid ammonium chloride (NH4Cl) and an excess of ammonium
hydroxide (NH4OH) solution till it smells of ammonia. Shake the test tube. If a brown
or white precipitate is formed, this indicates the presence of group-III cations.
Confirmatory tests of group-III cations are summarised in Table 7.14.
Observe the colour and the nature of the precipitate. A gelatinous white
3+
precipitate indicates the presence of aluminium ion (A1 ). If the precipitate is
3+
brown in colour, this indicates the presence of ferric ions (Fe ).
Dissolve the precipitate in dilute HCl Dissolve the white precipitate in dilute
and divide the solution into two parts. HCl and divide into two parts.
(a) To the first part add potassium (a) To the first part add sodium hydroxide
ferrocyanide solution [Potasium solution and warm. A white
hexacyanoferrate (II)]. A blue gelatinous precipitate soluble in
precipitate/colouration appears. excess of sodium hydroxide solution.
(b) To the second part add potassium (b) To the second part first add blue
thiocyanate solution. A blood red litmus solution and then ammonium
colouration appears. hydroxide solution drop by drop along
the sides of the test tube. A blue
floating mass in the colourless
solution is obtained.
105
LABORATORY MANUAL CHEMISTRY
(b) In the second test when blue litmus is added to the solution, a red
colouration is obtained due to the acidic nature of the solution. On addition
of NH4OH solution drop by drop the solution becomes alkaline and
aluminium hydroxide is precipitated. Aluminium hydroxide adsorbs blue
colour from the solution and forms insoluble adsorption complex named
‘lake’. Thus a blue mass floating in the colourless solution is obtained. The
test is therefore called lake test.
3+
2. Test for ferric ions (Fe )
Reddish brown precipitate of ferric hydroxide dissolves in hydrochloric acid and
ferric chloride is formed.
Fe(OH)3 + 3HCl → FeCl3 + 3H2O
(a) When the solution containing ferric chloride is treated with potassium
ferrocyanide solution a blue precipitate/colouration is obtained. The colour
of the precipitate is Prussian blue. It is ferric ferro-cyanide. The reaction
takes place as follows:
4FeCl3 + 3K4[Fe(CN)6] → Fe4[Fe(CN)6]3 + 12KCl
Potassium Prussian blue
ferrocyanide precipitate
If potassium hexacyanoferrate (II) (i.e. potassium ferrocyanide) is added in
excess then a product of composition KFe[Fe(CN)6] is formed. This tends to
form a colloidal solution (‘soluble Prussian blue’) and cannot be filtered.
FeCl3 + K4[Fe(CN)6] → KFe[Fe(CN)6] + 3KCl
(Soluble prussian blue)
(b) To the second part of the solution, add potassium thiocyanate (potassium
sulphocyanide) solution. The appearance of a blood red colouration
3+
confirms the presence of Fe ions.
3+ – 2+
Fe + SCN → [Fe(SCN)]
Blood red colour
106
SYSTEMATIC QUALITATIVE ANALYSIS
107
LABORATORY MANUAL CHEMISTRY
108
SYSTEMATIC QUALITATIVE ANALYSIS
2+
4. Test for Cobalt ion (Co )
Cobalt sulphide dissolves in aqua regia in the same manner as nickel sulphide.
When the aqueous solution of the residue obtained after treatment with aqua
regia is treated with a strong solution of potassium nitrite after neutralisation with
ammonium hydroxide and the solution is acidified with dil. acetic acid, a yellow
precipitate of the complex of cobalt named potassium hexanitritocobaltate (III)
is formed.
CoS + HNO3 + 3HCl → CoCl2 + NOCl + S + 2H2O
CoCl2 + 7KNO2 + 2CH3COOH → K3 [Co(NO2)6] + 2KCl + 2CH3COOK + NO + H2O
Potassium
hexanitritocobaltate(III)
(Yellow precipitate)
Dissolve the precipitate by boiling with dilute acetic acid and divide
2+ 2+ 2+
the solution into three parts one each for Ba , Sr and Ca ions
2+ 2+ 2+
Ba ions Sr ions Ca ions
(a) To the first part add (a) If barium is absent, take (a) If both barium and
potassium chromate second part of the solution strontium are absent,
solution. A yellow and add ammonium take the third part of
precipitate appears. sulphate solution. Heat the solution. Add
and scratch the sides of the ammonium oxalate
(b) Perform the flame test tube with a glass rod solution and shake
test with the and cool. A white well. A white
preserved precipitate. precipitate is formed. precipitate of calcium
A grassy green flame oxalate is obtained.
is obtained. (b) Perform the flame test with
the preserved precipitate. (b) Perform the flame test
A crimson-red flame with the preserved
confirms the presence of precipitate. A brick red
Sr2+ ions. flame, which looks
greenish-yellow through
blue glass, confirms the
2+
presence of Ca ions.
109
LABORATORY MANUAL CHEMISTRY
(b) Flame test – Perform the flame test as mentioned above. Calcium imparts
brick red colour to the flame which looks greenish-yellow through blue glass.
110
SYSTEMATIC QUALITATIVE ANALYSIS
Precautions
111
LABORATORY MANUAL CHEMISTRY
(h) Be careful while dealing with the explosive compounds, inflammable substances,
poisonous gases, electric appliances, glass wares, flame and the hot substances.
(i) Keep your working surroundings clean. Never throw papers and glass in the
sink. Always use dustbin for this purpose.
(j) Always wash your hands after the completion of the laboratory work.
(k) Always use the reagents in minimum quantity. Use of reagents in excess, not
only leads to wastage of chemicals but also causes damage to the environment.
Discussion Questions
(ii) Can we use glass rod instead of platinum wire for performing the flame test? Explain
your answer.
(iii) Why is platinum metal preferred to other metals for the flame test?
(iv) Name the anions detected with the help of dilute H2SO4?
(v) Why is dilute H2SO4 preferred over dilute HCl while testing anions?
(viii) What is lime water and what happens on passing carbon dioxide gas through it?
(ix) Carbon dioxide gas and sulphur dioxide gas both turn lime water milky. How will you
distinguish between the two?
(xi) What is the composition of dark brown ring which is formed at the junction of two layers
in the ring test for nitrates?
(xiii) What is chromyl chloride test ? How do you justify that CrO2Cl2 is acidic in nature?
(xiv) Why do bromides and iodides not give tests similar to chromyl chloride test?
(xv) Describe the layer test for bromide and iodide ions.
112
SYSTEMATIC QUALITATIVE ANALYSIS
(xviii) Why does iodine give a blue colour with starch solution?
(xx) Why is original solution for cations not prepared in conc. HNO3 or H2SO4?
(xxi) Why cannot conc. HCl be used as a group reagent in place of dil. HCl for the precipitation
of Ist group cations?
(xxii) How can one prevent the precipitation of Group–IV radicals, with the second group
radicals?
(xxiii) Why is it essential to boil off H2S gas before precipitation of radicals of group–III?
(xxiv) Why is heating with conc. nitric acid done before precipitation of group–III?
(xxvi) Why is NH4OH added before (NH4)2CO3 solution while precipitating group–V cations?
(xxvii) Why do we sometimes get a white precipitate in group–VI even if the salt does not
2+
contain Mg radical?
(xxxi) Why are the group–V radicals tested in the order Ba2+, Sr2+ and Ca2+ ?
(xxxii) Why does conc. HNO3 kept in a bottle turn yellow in colour?
(xxxiv) Why is the reagent bottle containing sodium hydroxide solution never stoppered?
113
LABORATORY MANUAL CHEMISTRY
Aim
To analyse the given salt for one anion and one cation present in it.
Material required
• Boiling tubes, test tubes, test tube holder, test tube stand, delivery tube, corks,
filter papers, reagents
2+ 2+ 2+ 2+
1. Noted the colour of the given White Cu , Fe , Ni ,Co ,
2+
salt. Mn are absent.
2– 2– –
2. Noted the smell of the salt. No specific smell. S , SO3 , CH3COO
may be absent.
2–
3. Heated 0.5 g of the salt in a (i) No gas was evolved. (i) CO 3 may be
– –
dry test tube and noted the present, NO3 , NO2 ,
–
colour of the gas evolved and Br may be
change in the colour of the absent.
2+
residue on heating and (ii) No particular (ii) Zn may be
cooling. change in colour of absent.
the residue is
observed when
heated and when
cooled.
2+ 2+ 2+ 2+
4. Prepared a paste of the salt No distinct colour of the Ca , Sr , Ba Cu
with conc. HCl and performed flame seen. may be absent.
the flame test.
– – – – –
7. Heated 0.1 g of salt with 1 mL No gas evolved. Cl , Br , I , NO3 , C2O4
conc. H2SO4. are absent.
3–
8. Acidified 1mL of aqueous salt No yellow precipitate PO4 absent.
solution with conc. HNO 3 .
Warmed the contents and then
added 4-5 drops of ammonium
molybdate solution.
114
SYSTEMATIC QUALITATIVE ANALYSIS
2–
9. Acidified water extract of the A white ppt. is obtained SO4 present.
salt with dil. HCl and then which is
added 2mL of BaCl2 solution. insoluble in conc. HNO3
and conc. HCl.
+
10. Heated 0.1 g of salt with 2 mL Ammonia gas is not NH4 absent.
NaOH solution. evolved.
11. Attempted to prepare original Clear solution formed Water soluble salt is
solution of the salt by present.
dissolving 1g of it in 20 mL
water.
13. Passed H2S gas through one No precipitate formed. Group–II absent.
portion of the solution of step 12.
Result
The given salt contains:
2–
Anion : SO4
2+
Cation : Mg
115
LABORATORY MANUAL CHEMISTRY
EXPERIMENT 7.2
Aim
Detection of nitrogen, sulphur and halogens in an organic compound.
Theory
In contrast to inorganic compounds the atoms in an organic compound are
linked to each other by covalent bonds, hence organic compounds don’t furnish
ions in solutions. Therefore, in order to test the presence of above elements in an
organic compound, it is fused with sodium metal to form ionisable sodium salts.
Though we may also fuse the organic compounds with potassium; we prefer
sodium because it is easily available and its reaction is easily controllable as
compared to potassium. Following reactions occur on fusion of the organic
compound with sodium metal.
Na + C + N t NaCN
2Na + S t Na2S
Material Required
Note: Chloroform and carbon tetrachloride should never be subjected to Lassaigne’s solution
test as violent explosions may result.
116
SYSTEMATIC QUALITATIVE ANALYSIS
Procedure
(a) Preparation of Sodium Extract of [Lassaigne’s extract]
(i) Dry a small piece of sodium between the folds of a filter paper. Cut a small
piece of the metal with the help of a sharp knife. Clean it and insert it into
the ignition tube. Melt the metal by gently heating the ignition tube in the
flame to expose the clean surface. A shining globule of metal is formed. Cool
the ignition tube slightly then add a pinch of organic compound into the
ignition tube, so as to cover the sodium metal completely with the organic
compound as shown in the fig. 7.10 (a)
Fig. 7.10: (a) Covering the sodium metal with organic commpound.
(b) Dropping the ignition tube in water after ignition
(ii) Heat the ignition tube gently in the flame. If a vigorous initial reaction occurs,
remove it from the flame and keep it out of the flame until the reaction
subsides. Then continue heating. Repeat the process till organic compound
reacts completely. After completion of the reaction heat the ignition tube
strongly till it becomes red hot.
(iii) Drop the red hot ignition tube quickly into the china dish containing 15mL
of distilled water and cover the china dish immediately with a wire guaze.
Break the tube. Repeat this process twice or thrice to obtain Lassaigne’s
extract of sufficient concentration.
(iv) Boil the contents of the china dish for about 10 minutes and then filter the
solution. The filtrate so obtained is named as Lassaigne’s extract or sodium
extract. It is alkaline due to sodium hydroxide formed by the reaction of
unreacted sodium metal during fusion with water.
(ii) Boil the mixture obtained in step (i) and finally cool. A green precipitate
of ferrous hydroxide is formed. If it is not formed add a few drops of
sodium hydroxide solution, boil the solution again and cool.
(iii) Acidify the solution obtained in step (ii) with a few drops of dilute
sulphuric acid and warm. Add ferric chloride solution. A Prussian
blue precipitate or green/blue colouration indicates the presence
of nitrogen.
∆
6NaCN + Fe(OH )2 → Na 4 [Fe(CN )6 ] + 2NaOH
Sodium (I)
hexacyanidoferrate (II)
+ 4−
4Fe3 + 3 [Fe(CN )6 ] ∆
→ Fe 4 [Fe(CN )6 ]3
Prussian blue or
Iron (III) hexacyanidoferrate (II)
If hexacyanidoferrate(II) ion is in excess in solution then on adding ferric
chloride solution blue coloured soluble sodium(I) iron (III) hexacyanidoferrate(II)
is formed.
+ 4−
Na + Fe3 + [Fe(CN )6 ] → NaFe [Fe(CN )6 ]
Sodium (I) Iron (III)
hexacyanidoferrate (II)
If a small amount of CN– ions is formed during fusion then a green solution
is obtained at first, which deposits prussian blue on standing.
The ferric ions are formed by the oxidation of ferrous sulphate by the oxygen
of the air in the presence of dilute sulphuric acid. Therefore, some times there is
no need of adding ferric chloride solution. Some times blood red colour is obtained
when sulphur and nitrogen both are present, the test for which is given later in
this section.
118
SYSTEMATIC QUALITATIVE ANALYSIS
119
LABORATORY MANUAL CHEMISTRY
Precautions
· (a) Sodium metal is highly reactive so handle it with care. Never touch sodium metal
with fingers.
· (b) Dry the sodium metal between the folds of filter paper before use.
· (c) Use only distilled water to prepare Lassaigne’s extract.
(d) While performing test for halogens, test tube rinsed with distilled water should
be used.
· (e) Ensure dryness of ignition tube before using it for fusion. Moisture present in
the ignition tube may cause a vigorous reaction with sodium metal.
· (f) Always take a small piece of sodium metal for fusion, as the unreacted sodium
(excess of sodium) may react with water violently during the process of breaking
the ignition tube in water.
· (g) Solutions obtained after dissolving precipitates of AgCl/AgBr/AgI should be
acidified with 2M nitric acid and the solution should be discarded immediately
to avoid explosion.
· (h) Aqueous solution of sodium nitropruside is not stable hence always use freshly
prepared solution.
Discussion Questions
(ii) Why is the sodium extract prepared for the detection of elements in an organic
compound?
(iii) Why should the sodium extract be boiled with concentrated nitric acid before
using for the test of halogens?
120
SYSTEMATIC QUALITATIVE ANALYSIS
(iv) Why chlorine water is added in the layer test for bromine and iodine? Can any
other reagent be used in its place?
(v) Apply the concept of electrode potential to justify the occurrence of the following
reactions:
(vi) Can chlorine be librated from sodium chloride solution by adding bromine water?
(vii) Out of AgCl and [Ag(NH3)2]Cl, the value of solubility product of which substance is
high? Explain
(viii) Can a sodium salt be used in place of sodium metal in the fusion reaction? If so,
name the compound.
121
PROJECTS
BACKGROUND INFORMATION
ABOUT INVESTIGATORY PROJECTS
INTRODUCTION
The expansion of scientific knowledge and consequently the change in the system
of education has led to a modification in the methods of instruction. Today the
stress is laid on inquiry approach and discussion method instead of the age-old
lecture method of teaching. A new dimension in the teaching of science has been
added by including the project-work at the higher secondary level. Teaching
through project work is an individualized instructional technique. It provides an
opportunity to the student to define a problem, to plan his/her work, to search
appropriate resources, to carry out his/her plans, and to draw conclusions. This
way, students are exposed to the fundamental scientific principles, methods and
processes and get a first hand knowledge about the various phases involved in a
scientific investigation. Thus the project work helps to: (a) stimulate interest in
science; (b) arouse scientific curiosity; (c) develop independent critical thinking;
(d) provide experience of using various tools and techniques in the field of science
and (e) develop self-confidence. The modern trend in the teaching of science
therefore encourages more project work.
Any kind of investigation; formulated, designed and carried out in the library,
laboratory, in the field, or at home constitutes an investigatory project. A project
may be as simple as collection of samples of minerals and it may be as difficult as
developing an original indigenous process for the production of a chemical. Some
of the projects can be completely theoretical and involve only the library work.
Others may involve the experimental work to be carried out in the laboratory.
The experimental work in science exposes the students to a number of scientific
instruments, tools, techniques and intellectual skills.
SELECTION OF PROJECTS
Projects should usually be selected by the students. The idea of a project originates
from studying a subject in the classroom, reading the reports of various projects,
science news, popular science articles from science journals etc. Sometimes the
idea of a science project may strike during classroom discussion on topics, which
may require testing, quantifying and interpreting. Some of the science journals
for getting the ideas for a project are : (a) Journal of Chemical Education;
(b) Chemistry Education; (c) Education in Chemistry; (d) New Scientist; (e) School
BACKGROUND INFORMATION ABOUT INVESTIGATORY PROJECTS
MANAGING TIME
123
LABORATORY MANUAL CHEMISTRY
LABORATORY FACILITIES
124
BACKGROUND INFORMATION ABOUT INVESTIGATORY PROJECTS
PROJECT 1
Title
To test the contamination of water by bacteria by checking the
sulphide ion concentration and find out the cause of contamination.
Objective
To check the bacterial contamination in samples of water collected
from different sources by determining sulphide ion concentration.
Background Information
Sulphide ions are present in water when anaerobic bacteria
decompose organic matter or reduce sulphates. These are found
in stagnent water. Generally pollutants from paper mills, gas works,
tanneries, sewage works and other chemical plants are responsible
for the growth of such bacteria.
Brief Procedure
Collection of Samples
Sulphides are readily oxidised, therefore care should be taken at
the time of sampling to exclude air by flushing it with nitrogen or
carbon dioxide. But the best way is to ‘fix’ the sample immediately
after collection. This can be done by adding small volume of
cadmium-zinc acetate solution. For this take 80 mL of water and
add cadmium-zinc acetate solution 20 mL to obtain a total volume
of about 100 mL. To make Cd-Zn acetate solution dissolve 50 g
cadmium acetate and 50 g zinc acetate in 1.0 L of water. If collected
sample is acidic in nature, then first neutralize it with little excess
of alkali.
125
LABORATORY MANUAL CHEMISTRY
PROJECT 2
Title
To study the methods of purification of water.
Objectives
• To study level of purity achieved by using different methods
of purification.
• To study advantages and disadvantages of using different
method for purification.
• To know about specific uses of pure water.
Background Information
Purity of water obtained from different natural sources is different.
The type of contamination and impurity present depends upon
the source from which water is obtained. Besides drinking
purposes, we require pure water for various other purposes e.g.
in chemical analysis. There are various methods for the purification
of water. these remove impurities and contamination to different
extent. There are some advantages and disadvantages in using
these methods. Comparison of various methods of purification will
provide an idea about obtaining water of specific purity for a
specific purpose.
Brief Procedure
Students may find out level of puriety achieved by various
techniques in use, for the purification of drinking water. They can
survey the literature and visit industries etc. to find out uses of
water of specific purity. Students may work in groups for the study
of various aspects of the project.
PROJECT 3
Title
Testing the hardness, presence of iron, fluoride, chloride etc. in
drinking water obtained from different regions and a study of the
cause of presence of these ions above permissible limits.
126
BACKGROUND INFORMATION ABOUT INVESTIGATORY PROJECTS
Objectives
• To test the total hardness, iron, fluoride and chloride etc. in
different samples of water.
• To collect information about local sources of above ions in
water.
• To study the effect of these ions on health if present beyond
permissible limits.
• To find out whether any such problem exists in the locality
and around.
Background Information
Quality of drinking water has direct relationship with the
human health and life. If iron, fluoride, chloride etc. are
present in water above permissible limits, they may cause
several health problems. For example, if fluoride is present
above permissible limit, people of the region may suffer from
fluorosis. Hardness of water is due to the presence of calcium
and magnesium ions. It is well known fact that hard water is
not fit for laundary purposes. Thus, it is very important to
know the ions and their amount present in water.
Brief Procedure
Students may collect samples of water from different sources. They
can detect the presence of different ions by usual methods of
analysis. Total hardness of water can be estimated by standard
– –
procedure of complexometric titration. Estimation of Cl , F and
2+
Fe is difficult at this level. Therefore existing data from approved
labs can be taken for the purpose of investigation.
PROJECT 4
Title
Investigation of the foaming capacity of different washing soaps
and the effect of addition of sodium carbonate on their foaming
capacity.
Objective
To study the foaming capacity of soaps and the effect of addition
of sodium carbonate on their foaming capacity.
127
LABORATORY MANUAL CHEMISTRY
Brief Procedure
Weigh 1 gram of a sample of soap and dissolve it completely in
100 mL of distilled water. Take 10 mL of the soap solution in a
boiling tube close the mouth of the boiling tube with the help of a
cork and shake the solution making 20 regular strokes so that
foam increases uniformly. Measure the length of the boiling tube
up to which the foam rises. Similarly, perform the experiment with
other soap solutions.
Dissolve 0.5g of sodium carbonate in 50 mL of each of the
above soap solutions separately. Now take 10 mL of a solution in
a boiling tube and shake it equal number of times (e.g. 20 regular
strokes). Measure the length up to which foam appears. Similarly,
perform the experiment with other soap solutions. Record the
observations in a tabular form.
Compare the height upto which foam produced rises in different
soap solutions with and without the presence of Na2CO3 and draw
conclusions.
PROJECT 5
Title
Study of the acidity of different samples of tea leaves and reasons
for the variation in colour of tea prepared from these leaves.
Objective
To estimate the concentration of acids present in different tea
samples and the effect of addition of acids or bases on the colour
of tea extract.
Brief Procedure
128
BACKGROUND INFORMATION ABOUT INVESTIGATORY PROJECTS
PROJECT 6
Title
Study the rates of evaporation of different liquids
Objective
To study the relationship between the rates of evaporation of different
liquids and their chemical constitution.
Brief Procedure
Take five clean and dry weighing tubes and mark them as A, B, C, D
and E. Weigh each weighing tube with its stopper. Now pour 10 mL
of different liquids (ethanol, ether, tetrachloromethane, acetone etc.)
in different weighing tubes. Weigh each weighing tube again and
find the mass of the liquid taken in each weighing tube.
Remove the stoppers of the weighing tubes and keep them at
room temperature for one hour. After exactly one hour, close the
mouth of all the weighing tubes with their stoppers and weigh them
again one by one.
Calculate the loss in mass of each liquid. The temperature and
the surface area should be the same for the evaporation of each
liquid. Determine the rate of evaporation of each liquid in grams of
liquid evaporated per second. Relate the difference in rates of
evaporation of liquids with their chemical constitution and variation
in intermolecular/intra-molecular interactions.
129
LABORATORY MANUAL CHEMISTRY
PROJECT 7
Title
Study the effect of acids and alkalies on the tensile strength of
fibres
Objective
To study the effect of acids on the tensile strength of different types
of fibers.
Brief Procedure
The tensile strength of a fibre is measured by noting the minimum
weight required just to break the thread. It may be done as follows:
Take a thread of about 20 cm length and tie its one end with a
ring fixed on the iron stand and the other end with a hanger which
carries the weights. Increase the weight on the hanger and find
out the minimum weight required to just break the thread. Repeat
the experiment with threads of equal length and thickness but of
different materials (eg. cotton, wool, silk, terylene etc.). These
weights are the measure of tensile strength of the fibre.
The effect of acids and alkalies on the tensile strength of fibres
can be determined by dipping them separately in dilute HC1 or
dilute NaOH solution of equal strengths for equal intervals of time.
After a small but fixed interval of time, the fibres are removed from
the solution, washed with water and dried. Then minimum weight
required to just break these threads are determined. These weights
are the measures of the tensile strengths of fibres after treatment
with acid or alkali. Interpret your observations in terms of chemical
constitution of the material of fibre.
PROJECT 8
Title
Study of the acids and mineral contents of vegetables and fruits.
Objective
(a) To determine the amount of acids present in various
vegetables and fruits.
(b) To detect the presence of iron, carbohydrate, protein and
sugar etc. in vegetables and fruits.
130
BACKGROUND INFORMATION ABOUT INVESTIGATORY PROJECTS
Brief Procedure
Title
A study of the variation of viscosity of organic compounds of same
homologous series with variation in the (a) molecular masses and
(b) structures of carbon chains.
Background Information
Some liquids like honey or Mobil oil flow very slowly while others
like water or kerosene flow rapidly. Liquids that flow slowly are
known as viscous liquids while others that flow rapidly are known
as non-viscous liquids. The resistance offered by a liquid to flow is
known as viscosity. It is related to intermolecular forces existing in a
liquid. Different liquids have different values of viscosity due to the
existence of different magnitudes of intermolecular forces. The
comparison of viscosities of various homologues and isomers in a
particular homologous series would give an idea about the
magnitude of intermolecular forces existing in them.
131
LABORATORY MANUAL CHEMISTRY
Objectives
The objectives of this project are to establish a relationship between
(a) viscosity and molecular masses; and (b) viscosity and nature of
carbon chain in organic compounds.
Principle Involved
The resistance to flow offered by a liquid is measured in terms of
coefficient of viscosity which is defined as follows:
‘Coefficient of viscosity of a liquid at a specified temperature is
the steady force required to maintain a velocity difference of unity
between two parallel layers of a liquid, a unit distance apart and
having a unit area of contact’. Coefficient of viscosity is measured
by Ostwald viscometer method. For two liquids whose coefficient
of viscosity are d1 and d2, η1 , η2 the time of flow in seconds are t1
Hazard Warning and densities are d1 and respectively d2 then the following relation
• Acetone and alcohols are holds:
inflamable, do not let the
bottles open when not in
use. η 1 d1 × t1
=
• Keep the bottles away η 2 d2 × t2
from flames.
• Wash your hands after
use. Hence if the viscosity of one liquid is known, the viscosity of
• Wear safety spectacles. other can be determined.
Material required
Ostwald viscometer, stop-watch, beaker (250 mL), pipette, graduated cylinder, kerosene,
petrol, diesel, methyl alcohol, ethyl alcohol, propyl alcohol, isopropyl alcohol, butyl
alcohol, isobutyl alcohol, tert butyl alcohol and amyl alcohol.
Brief Procedure
The viscometer was washed, rinsed with alcohol and dried.
10 mL of the liquid under investigation was filled in it and the time
required for the flow of liquid between two marks of viscometer was
noted with the help of a stop watch. These observation were recorded
in Tables I and II. The viscosities of various liquids were calculated
by the formula discussed under the heading principles involved.
132
BACKGROUND INFORMATION ABOUT INVESTIGATORY PROJECTS
Table 2 : Data for the viscosity vs molecular mass relationship of various compounds
Note : * If the homologues/isomers of alcohols are not available, other suitable compounds, which
are available or are easily manageable can be used for this study.
** Time of flow recorded in the tables are specific for a viscometer and should not be taken as
standard values.
Conclusion
As seen from the Table 1, the viscosities of various hydrocarbon
fractions, i.e. petrol, kerosene and diesel oil are on an average 6.4,
16.4 and 18.0 respectively. Since the molecular mass of these
fractions increases from petrol to diesel oil, this indicates that
viscosity increases with increase in molecular mass. The
intermolcular attractions tend to increase with increase in molecular
mass.
133
LABORATORY MANUAL CHEMISTRY
Precaution
References
KEENAN, C.W.; WOOD, J.H. General Chemistry IVth Edition., Harper
and Row Publishers Inc. New York.
134
APPENDICES
APPENDIX I
Laboratory assistants must see that the reagent bottles on each shelf are properly arranged, labelled and
contain sufficient quantity of the freshly prepared reagents.
(a) Solids
1. Ammonium chloride 8. Potassium dichromate
2. Borax 9. Sodium carbonate
3. Ferrous sulphate 10. Sodium hydrogencarbonate
4. Fusion mixture 11. Sodium hydroxide
5. Manganese dioxide 12. Sodium nitrate
6. Oxalic acid 13. Sodium nitroprusside
7. Potassium chromate 14. Sodium peroxide
(b) Metals
1. Copper 3. Zinc granules
2. Tin 4. Zinc powder
(c) Papers
1. Lead acetate paper 5. Starch iodide paper
2. Litmus paper (blue) 6. Starch paper
3. Litmus paper (red) 7. Turmeric paper
4. Potassium dichromate paper 8. Universal indicator paper
135
APPENDIX II
Sl. No. Inorganic Chemicals Grade* Sl. No. Inorganic Chemicals Grade
* L. R. = Laboratory reagent
A. R. = Analytical reagent
136
APPENDIX II
Sl. No. Organic Chemicals Grade Sl. No. Organic Chemicals Grade
Sl. No. Glassware (Borosilicate glass) Sl. No. Glassware (Borosilicate glass)
1. Beaker (50 mL) 18. Measuring cylinder (10 mL)
2. Beaker (100 mL) 19. Measuring cylinder (50 mL)
3. Beaker (150 mL) 20. Measuring cylinder (100 mL)
4. Beaker (250 mL) 21. Measuring flask (100 mL)
6. Beaker (500 mL) 22. Measuring flask (250 mL)
7. Boiling tubes 23. Petri dish (8 cm diameter)
8. Burette (50 mL)
24. Pipette (10 mL)
9. Conical flask (100 mL)
25. Pipette (25 mL)
10. Conical flask (150 mL)
26. Round bottom flask (500 mL)
11. Conical flask (250 mL)
27. Round bottom flask (1 litre)
12. Flat bottomed flask (1 litre)
28. Separating funnel (250 mL)
13. Funnel (8 cm diameter)
29. Test tube (15 mL)
14. Glass droppers
30. Thiele’s tube
15. Kipp’s apparatus (diameter 1000 mm)
31. Watch glass (9 cm diameter)
16. Kjeldal’s flask
32. Water aspirator weighing bottle
17. Liebig’s condenser
137
LABORATORY MANUAL CHEMISTRY
Miscellaneous Articles
30. Key (one way) 62. Weight box (for chemical balance)
138
APPENDIX III
I. Concentration acids
1. Dil. Acetic acid 5 M (5 N) Dilute 285 mL of glacial acetic acid with distilled water
water and make up the volume to 1 litre.
2. Dil. Hydrochloric acid 5 M (5 N) Add 430 mL of conc. HCl in the distilled water and make
up the volume to 1 litre.
3. Dil. Nitric acid 5 M (5 N) Add 320 mL of conc. nitric acid to distilled water and
make up the volume to litre.
4. Dil. Sulphuric acid 2.5 M (5 N) Pour 140 mL of conc. sulphuric acid slowly and with
constant stirring in 500 mL of distilled water. Cool and
make up the volume to 1 litre.
III. Bases
2. Ammonium chloride 5 M (5 N) 53.5 Dissolve 267.5 g of the salt in distilled water and
dilute to one litre.
139
LABORATORY MANUAL CHEMISTRY
5. Ammonium oxalate 0.5 M (1 N) 142 Dissolve 71 g of the salt in distilled water and
dilute to 1 litre.
6. Ammonia sulphate 1 M (2 N) 132 Dissolve 132 g of the salt in distilled water and
dilute to 1 litre.
7. Barium chloride
BaCl2.2H2O 0.5 M (0.5 N) 244 Dissolve 61 g of the salt in distilled water and
dilute to 1 litre.
8. Bromine water approx. saturated 160 Add 2 mL of bromine in 100 mL of distilled water
shake the mixture well. Keep it in a dark bottle.
9. Calcium chloride 0.5 M (0.5 N) 219 Dissolve 55 g of the salt in distilled water and
make up the volume to 1 litre.
11. Copper sulphate 14% 249.5 Dissolve 14 g of the salt in distilled water and
make up the volume to 100 mL.
12. Cobalt nitrate 0.15 M (0.075 N) 291 Dissolve 43.65 g of the salt in distilled water and
make up the volume to 1 litre.
23. Mercuric chloride 0.25 M (0.5 N) 272 Dissolve 70 g of the salt in small amount of
distilled water and make up the volume to 1 litre
with distilled water.
140
APPENDIX III
26. Potassium dichromate 0.15 M (1 N) 294 Dissolve 49.0 g of the salt in distilled water and
make up the volume to 1 litre.
27. Potassium ferrocyanide 0.15 M (0.5 N) 368 Dissolve 46.0 g of the salt in distilled water and
dilute to 1 litre.
28. Potassium ferricyanide 0.2 M (0.5 N) 329 Dissolve 55.0 g of the salt in distilled water and
dilute to 1 litre.
29. Potassium iodide 0.5 M (0.5 N) 166 Dissolve 83.0 g of the salt in distilled water and
make up the volume to 1 litre.
30. Potassium permanganate 0.06 M (0.3 N) 158 Dissolve 10.0 g of the salt in 1 litre distilled
water. Heat the solution and filter it through glass
wool.
31. Potassium thiocyanate 0.5 M (0.5 N) 97 Dissolve 49.0 g of the salt in distilled water and
make up the volume to 1 litre.
33. Silver nitrate 0.1 M 170 Dissolve 17 g of the salt in 250 mL of distilled
water and store it in a brown coloured bottle.
34. Sodium acetate 5 M (5 N) 82 Dissolve 410 g of salt in distilled water and dilute
to 1 litre.
141
LABORATORY MANUAL CHEMISTRY
1. Alcohol (1:1) : Mix equal volumes of rectified spirit and distilled water.
2. Alcoholic potassium hydroxide solution : Dissolve 11.2 g of potassium hydroxide in 100 mL ethand (or rectified
spirit) by boiling for 30 minutes.
6. Ceric ammonium nitrate solution : Dissolve 40 g of the reagent in 100 mL of 2 N nitric acid.
7. Copper sulphate solution : Dissolve 14 g of copper sulphate in 100 mL water (14% solution)
8. 2,4–dinitrophenylhydrazine reagent :
(i) For water soluble compounds : Add 0.5 g solid in a mixture of 42 mL conc. HCl and 54 mL water and
dissolve by warming on water bath. Add water to make up the volume to
250 mL.
(ii) For compounds not soluble in water : Dissolve 1 g of reagent in 7.5 mL conc. sulphuric acid. Add this solution
gradually to 7.5 mL rectified spirit. Make up the volume to 250 mL by
adding water.
10. *Fehling’s solution B : Dissolve 350 g of Rochelle’s salt and 100 g sodium hydroxide in 1 L
water.
15. Schiff’s reagent : Dissolve 1 g of rosaniline in 50 mL water with gentle warming, cool,
saturate with sulphur dioxide gas. Dilute the solution upto 1 L with water.
If pink colour reappears on standing add few drops of saturated aqueous
solution of SO2 with stirring until the colour just disappears.
17. Sodium hypochlorite (2M) : Dissolve 100 g of NaOH in 200 mL of water in a large beaker. Cool the
solution and add about 500 g of crushed ice. Weigh the beaker on a rough
balance and pass chlorine gas until the weight increases by 72 g. Dilute
the solution to 1 L with water. The solution must be kept in a cool dark
place. Even then it slowly decomposes.
*Before use, mix equal volumes of Fehling’s solution A and Fehling’s solution B.
142
APPENDIX IV
143
LABORATORY MANUAL CHEMISTRY
–
nitrate NO3 Most cations None
– 2+
chloride Cl Most cations Ag+, Pb2+, Hg2
– 2+
bromide Br Most cations Ag+, Pb2+, Hg2
– 2+
iodide I, Most cations Ag+, Pb2+, Hg2
2–
sulphate SO4 , Most cations Br2+, Sr2+, Pb2+, Ag+
2–
chromate CrO4 Most cations Br2+, Sr2+, Pb2+, Ag+
+
sulphide S2–, NH4 , alkali metal cations, Most other cations
– +
hydroxide OH , NH4 , alkali metal and alkaline earth Most other cations
2– +
carbonate CO3 NH4 and alkali metal cations Most other cations
3–
phosphate PO4 except Li+
144
APPENDIX V
The value given in parenthesis is the molar mass of the isotope of largest known half-life.
145
APPENDIX VI
* Force: 1 newton (N) = 1 kg m/s 2 , i.e.,the force that, when applied for 1 second, gives a
1-kilogram mass a velocity of 1 metre per second.
** The amount of heat required to raise the temperature of one gram of water from 14.50C to 15.50C.
† Note that the other units are per particle and must be multiplied by 6.022 ×1023 to be strictly
comparable.
146
APPENDIX VII
2–
S2O8 + 2e– → 2SO4
2–
+2.05 ClO– + H2O + 2e– → Cl– + 2OH– +0.89
Au+ + e– → Au +1.69 Hg 2+ –
2 +2e → 2Hg +0.79
2HClO + 2H+ + 2e– → Cl2 + 2H2O +1.63 BrO– + H2O + 2e– → Br– + 2OH– +0.76
2HBrO + 2H+ + 2e– → Br2 + 2H2O +1.60 MnO42– + 2H2O + 2e– → MnO2 + 4OH– +0.60
–
MnO4 + 8H+ + 5e– → Mn2+ + 4H2O +1.51 MnO–4 + e– → MnO42– +0.56
2–
Cr2O 7 + 14H+ + 6e– → 2Cr3+ + 7H2O +1.33 NiOOH + H2O + e– → Ni(OH)2 + OH– +0.49
ClO–4 + 2H+ +2e– → ClO–3 + 2H2O +1.23 ClO–4 + H2O + 2e– → ClO–3 + 2OH– +0.36
147
LABORATORY MANUAL CHEMISTRY
148
APPENDIX VIII
LOGARITHMS
Sometimes, a numerical expression may involve multiplication, division or rational powers of large
numbers. For such calculations, logarithms are very useful. They help us in making difficult calculations
easy. In Chemistry, logarithm values are required in solving problems of chemical kinetics, thermodynamics,
electrochemistry, etc. We shall first introduce this concept, and discuss the laws, which will have to be
followed in working with logarithms, and then apply this technique to a number of problems to show
how it makes difficult calculations simple.
We know that
23 = 8, 32 = 9, 53 = 125, 70 = 1
In general, for a positive real number a, and a rational number m, let am = b,
where b is a real number. In other words
the mth power of base a is b.
Another way of stating the same fact is
logarithm of b to base a is m.
If for a positive real number a, a ≠ 1
am = b,
we say that m is the logarithm of b to the base a.
b
We write this as lo g a = m ,
“log” being the abbreviation of the word “logarithm”.
Thus, we have
3
log 2 8 = 3, Since 2 = 8
2
log 3 9 = 2, Since 3 = 9
125 3
log 5 = 3, Since 5 = 125
0
log 7 1 = 0, Since 7 =1
Laws of Logarithms
In the following discussion, we shall take logarithms to any base a, (a > 0 and a ≠ 1)
m
Second Law: loga = loga m – logan
n
Proof: Let logam = x, logan = y
149
LABORATORY MANUAL CHEMISTRY
Then ax = m, ay = n
x
m a x−y
Hence = y
=a
n a
Therefore
m
log a = x − y = log a m − log a n
n
Third Law :
loga(mn) = n logam
Logarithms to Base 10
Because number 10 is the base of writing numbers, it is very convenient to use logarithms to the base
10. Some examples are:
log10 10 = 1, since 101 = 10
log10 100 = 2, since 102 = 100
log10 10000 = 4, since 104 = 10000
log10 0.01 = –2, since 10–2 = 0.01
log10 0.001 = –3, since 10–3 = 0.001
0
and log101 = 0 since 10 = 1
The above results indicate that if n is an integral power of 10, i.e., 1 followed by several zeros or
1 preceded by several zeros immediately to the right of the decimal point, then log n can be easily found.
If n is not an integral power of 10, then it is not easy to calculate log n. But mathematicians have
made tables from which we can read off approximate value of the logarithm of any positive number
between 1 and 10. And these are sufficient for us to calculate the logarithm of any number expressed
in decimal form. For this purpose, we always express the given decimal as the product of an integral
power of 10 and a number between 1 and 10.
150
APPENDIX VIII
25.2 1
25.2 = × 10 = 2.52 × 10
10
1038.4 3 3
∴ 1038.4 = × 10 = 1.0384 × 10
1000
In each case, we divide or multiply the decimal by a power of 10, to bring one non-zero digit to the left
of the decimal point, and do the reverse operation by the same power of 10, indicated separately.
Thus, any positive decimal can be written in the form
n = m × 10p
where p is an integer (positive, zero or negative) and 1< m < 10. This is called the “standard form of n.”
Working Rule
1. Move the decimal point to the left, or to the right, as may be necessary, to bring one non-zero digit
to the left of decimal point.
2. (i) If you move p places to the left, multiply by 10p.
(ii) If you move p places to the right, multiply by 10–p.
(iii) If you do not move the decimal point at all, multiply by 100.
(iv) Write the new decimal obtained by the power of 10 (of step 2) to obtain the standard form of
the given decimal.
151
LABORATORY MANUAL CHEMISTRY
2. Read off the characteristic p of log n from this expression (exponent of 10).
3. Look up log m from tables, which is being explained below.
4. Write log n = p + log m
If the characteristic p of a number n is say, 2 and the mantissa is .4133, then we have log n
= 2+ .4133 which we can write as 2.4133. If, however, the characteristic p of a number m is say –2 and
the mantissa is .4123, then we have log m = –2 + .4123. We cannot write this as –2.4123. (Why?) In order
to avoid this confusion we write 2 for –2 and thus we write log m = 2.4123 .
Now let us explain how to use the table of logarithms to find mantissas. A table is appended at the
end of this Appendix.
Observe that in the table, every row starts with a two digit number, 10, 11, 12,... 97, 98, 99. Every
column is headed by a one-digit number, 0, 1, 2, ...9. On the right, we have the section called “Mean
differences” which has 9 columns headed by 1, 2...9.
0 1 2 3 4 5 6 7 8 9 1 2 3 4 5 6 7 8 9
.. .. .. .. .. .. .. .. .. .. .. .. .. .. .. .. .. .. .. ..
61 7853 7860 7868 7875 7882 7889 7896 7803 7810 7817 1 1 2 3 4 4 5 6 6
62 7924 7931 7935 7945 7954 7959 7966 7973 7980 7987 1 1 2 3 3 4 5 6 6
63 7993 8000 8007 8014 8021 8028 8035 8041 8048 8055 1 1 2 3 3 4 5 6 6
.. .. .. .. .. .. .. .. .. .. .. .. .. .. .. .. .. .. .. ..
Now suppose we wish to find log (6.234). Then look into the row starting with 62. In this row, look
at the number in the column headed by 3. The number is 7945. This means that
log (6.230) = 0.7945*
But we want log (6.234). So our answer will be a little more than 0.7945. How much more? We look
this up in the section on Mean differences. Since our fourth digit is 4, look under the column headed
by 4 in the Mean difference section (in the row 62). We see the number 3 there. So add 3 to 7945. We
get 7948. So we finally have
log (6.234) = 0.7948.
Take another example. To find log (8.127), we look in the row 81 under column 2, and we find 9096.
We continue in the same row and see that the mean difference under 7 is 4. Adding this to 9096, and
we get 9100. So, log (8.127) = 0.9100.
* It should, however, be noted that the values given in the table are not exact. They are only approximate values,
although we use the sign of equality which may give the impression that they are exact values. The same
convention will be followed in respect of antilogarithm of a number.
152
APPENDIX VIII
In the antilog table, the entry under column 7 in the row .53 is 3443 and the mean difference for the
last digit 2 in that row is 2, so the table gives 3445. Hence,
antilog (.5372) = 3.445
Now since log n = 2.5372, the characteristic of log n is 2. So the standard form of n is given by
n = 3.445 × 102
or n = 344.5
Illustration 1
If log x = 1.0712, find x.
Solution: We find that the number corresponding to 0712 is 1179. Since characteristic of log x is 1, we
have
x = 1.179 × 101
= 11.79
Illustration 2
If log x = 2.1352, find x.
Solution: From antilog tables, we find that the number corresponding to 1352 is 1366. Since the
characteristic is 2 i.e., –2, so
x = 1.366 × 10–2 = 0.01366
Illustration 1
Find 6.3 × 1.29
Illustration 2
1.5
(1.23)
Find
11.2 × 23.5
3
(1.23)2
Solution: Let x =
11.2 × 23.5
153
LABORATORY MANUAL CHEMISTRY
3
(1.23)2
Then log x = log
11.2 × 23.5
3
= log 1.23 – log (11.2 × 23.5)
2
3
= log 1.23 – log 11.2 – 23.5
2
Now,
log 1.23 = 0.0899
3
log 1.23 = 0.13485
2
log 11.2 = 1.0492
log 23.5 = 1.3711
log x = 0.13485 – 1.0492 – 1.3711
= 3.71455
∴ x = 0.005183
Illustration 3
5
(71.24) × 56
Find 7
(2.3) × 21
5
(71.24) × 56
Solution: Let x = 7
(2.3) × 21
1 (71.24)5 × 56
Then log x = log 7
2 (2.3) × 21
1 7
= [log (71.24)5 + log 56 − log (2.3) − log 21]
2
5 1 7 1
= log 71.24 + log 56 − log 2.3 − log 21
2 4 2 4
Now, using log tables
log 71.24 = 1.8527
log 56 = 1.7482
log 2.3 = 0.3617
log 21 = 1.3222
5 1 7 1
∴ log x = log (1.8527) + (1.7482) − (0.3617) − (1.3222)
2 4 2 4
= 3.4723
∴ x = 2967
154
LOGARITHMS
Table 1
N 0 1 2 3 4 5 6 7 8 9 1 2 3 4 5 6 7 8 9
30 4771 4786 4800 4814 4829 4843 4857 4871 4886 4900 1 3 4 6 7 9 10 11 13
31 4914 4928 4942 4955 4969 4983 4997 5011 5024 5038 1 3 4 6 7 8 10 11 12
32 5051 5065 5079 5092 5105 5119 5132 5145 5159 5172 1 3 4 5 7 8 9 11 12
33 5185 5198 5211 5224 5237 5250 5263 5276 5289 5302 1 3 4 5 6 8 9 10 12
34 5315 5328 5340 5353 5366 5378 5391 5403 5416 5428 1 3 4 5 6 8 9 10 11
35 5441 5453 5465 5478 5490 5502 5514 5527 5539 5551 1 2 4 5 6 7 9 10 11
36 5563 5575 5587 5599 5611 5623 5635 5647 5658 5670 1 2 4 5 6 7 8 10 11
37 5682 5694 5705 5717 5729 5740 5752 5763 5775 5786 1 2 3 5 6 7 8 9 10
38 5798 5809 5821 5832 5843 5855 5866 5877 5888 5899 1 2 3 5 6 7 8 9 10
39 5911 5922 5933 5944 5955 5966 5977 5988 5999 6010 1 2 3 4 5 7 8 9 10
40 6021 6031 6042 6053 6064 6075 6085 6096 6107 6117 1 2 3 4 5 6 8 9 10
41 6128 6138 6149 6160 6170 6180 6191 6201 6212 6222 1 2 3 4 5 6 7 8 9
42 6232 6243 6253 6263 6274 6284 6294 6304 6314 6325 1 2 3 4 5 6 7 8 9
43 6335 6345 6355 6365 6375 6385 6395 6405 6415 6425 1 2 3 4 5 6 7 8 9
44 6435 6444 6454 6464 6474 6484 6493 6503 6513 6522 1 2 3 4 5 6 7 8 9
45 6532 6542 6551 6561 6471 6580 6590 6599 6609 6618 1 2 3 4 5 6 7 8 9
46 6628 6637 6646 6656 6665 6675 6684 6693 6702 6712 1 2 3 4 5 6 7 7 8
47 6721 6730 6739 6749 6758 6767 6776 6785 6794 6803 1 2 3 4 5 5 6 7 8
48 6812 6821 6830 6839 6848 6857 6866 6875 6884 6893 1 2 3 4 4 5 6 7 8
49 6902 6911 6920 6928 6937 6946 6955 6964 6972 6981 1 2 3 4 4 5 6 7 8
155
LOGARITHMS
Table 1 continued
N 0 1 2 3 4 5 6 7 8 9 1 2 3 4 5 6 7 8 9
50 6990 6998 7007 7016 7024 7033 7042 7050 7059 7067 1 2 3 3 4 5 6 7 8
51 7076 7084 7093 7101 7110 7118 7126 7135 7143 7152 1 2 3 3 4 5 6 7 8
52 7160 7168 7177 7185 7193 7202 7210 7218 7226 7235 1 2 2 3 4 5 6 7 7
53 7243 7251 7259 7267 7275 7284 7292 7300 7308 7316 1 2 2 3 4 5 6 6 7
54 7324 7332 7340 7348 7356 7364 7372 7380 7388 7396 1 2 2 3 4 5 6 6 7
55 7404 7412 7419 7427 7435 7443 7451 7459 7466 7474 1 2 2 3 4 5 5 6 7
56 7482 7490 7497 7505 7513 7520 7528 7536 7543 7551 1 2 2 3 4 5 5 6 7
57 7559 7566 7574 7582 7589 7597 7604 7612 7619 7627 1 2 2 3 4 5 5 6 7
58 7634 7642 7649 7657 7664 7672 7679 7686 7694 7701 1 1 2 3 4 4 5 6 7
59 7709 7716 7723 7731 7738 7745 7752 7760 7767 7774 1 1 2 3 4 4 5 6 7
60 7782 7789 7796 7803 7810 7818 7825 7832 7839 7846 1 1 2 3 4 4 5 6 6
61 7853 7860 7768 7875 7882 7889 7896 7903 7910 7917 1 1 2 3 4 4 5 6 6
62 7924 7931 7938 7945 7952 7959 7966 7973 7980 7987 1 1 2 3 3 4 5 6 6
63 7993 8000 8007 8014 8021 8028 8035 8041 8048 8055 1 1 2 3 3 4 5 5 6
64 8062 8069 8075 8082 8089 8096 8102 8109 8116 8122 1 1 2 3 3 4 5 5 6
65 8129 8136 8142 8149 8156 8162 8169 8176 8182 8189 1 1 2 3 3 4 5 5 6
66 8195 8202 8209 8215 8222 8228 8235 8241 8248 8254 1 1 2 3 3 4 5 5 6
67 8261 8267 8274 8280 8287 8293 8299 8306 8312 8319 1 1 2 3 3 4 5 5 6
68 8325 8331 8338 8344 8351 8357 8363 8370 8376 8382 1 1 2 3 3 4 4 5 6
69 8388 8395 8401 8407 8414 8420 8426 8432 8439 8445 1 1 2 2 3 4 4 5 6
70 8451 8457 8463 8470 8476 8482 8488 8494 8500 8506 1 1 2 2 3 4 4 5 6
71 8513 8519 8525 8531 8537 8543 8549 8555 8561 8567 1 1 2 2 3 4 4 5 5
72 8573 8579 8585 8591 8597 8603 8609 8615 8621 8627 1 1 2 2 3 4 4 5 5
73 8633 8639 8645 8651 8657 8663 8669 8675 8681 8686 1 1 2 2 3 4 4 5 5
74 8692 8698 8704 8710 8716 8722 8727 8733 8739 8745 1 1 2 2 3 4 4 5 5
75 8751 8756 8762 8768 8774 8779 8785 8791 8797 8802 1 1 2 2 3 3 4 5 5
76 8808 8814 8820 8825 8831 8837 8842 8848 8854 8859 1 1 2 2 3 3 4 5 5
77 8865 8871 8876 8882 8887 8893 8899 8904 8910 8915 1 1 2 2 3 3 4 4 5
78 8921 8927 8932 8938 8943 8949 8954 8960 8965 8971 1 1 2 2 3 3 4 4 5
79 8976 8982 8987 8993 8998 9004 9009 9015 9020 9025 1 1 2 2 3 3 4 4 5
80 9031 9036 9042 9047 9053 9058 9063 9069 9074 9079 1 1 2 2 3 3 4 4 5
81 9085 9090 9096 9101 9106 9112 9117 9122 9128 9133 1 1 2 2 3 3 4 4 5
82 9138 9143 9149 9154 9159 9165 9170 9175 9180 9186 1 1 2 2 3 3 4 4 5
83 9191 9196 9201 9206 9212 9217 9222 9227 9232 9238 1 1 2 2 3 3 4 4 5
84 9243 9248 9253 9258 9263 9269 9274 9279 9284 9289 1 1 2 2 3 3 4 4 5
85 9294 9299 9304 9309 9315 9320 9325 9330 9335 9340 1 1 2 2 3 3 4 4 5
86 9345 9350 9355 9360 9365 9370 9375 9380 9385 9390 1 1 2 2 3 3 4 4 5
87 9395 9400 9405 9410 9415 9420 9425 9430 9435 9440 0 1 1 2 2 3 3 4 4
88 9445 9450 9455 9460 9465 9469 9474 9479 9484 9489 0 1 1 2 2 3 3 4 4
89 9494 9499 9504 9509 9513 9518 9523 9528 9533 9538 0 1 1 2 2 3 3 4 4
90 9542 9547 9552 9557 9562 9566 9571 9576 9581 9586 0 1 1 2 2 3 3 4 4
91 9590 9595 9600 9605 9609 9614 9619 9624 9628 9633 0 1 1 2 2 3 3 4 4
92 9638 9643 9647 9652 9657 9661 9666 9671 9675 9680 0 1 1 2 2 3 3 4 4
93 9685 9689 9694 9699 9703 9708 9713 9717 9722 9727 0 1 1 2 2 3 3 4 4
94 9731 9736 9741 9745 9750 9754 9759 9763 9768 9773 0 1 1 2 2 3 3 4 4
95 9777 9782 9786 9791 9795 9800 9805 9809 9814 9818 0 1 1 2 2 3 3 4 4
96 9823 9827 9832 9836 9841 9845 9850 9854 9859 9863 0 1 1 2 2 3 3 4 4
97 9868 9872 9877 9881 9886 9890 9894 9899 9903 9908 0 1 1 2 2 3 3 4 4
98 9912 9917 9921 9926 9930 9934 9939 9943 9948 9952 0 1 1 2 2 3 3 4 4
99 9956 9961 9965 9969 9974 9978 9983 9987 9997 9996 0 1 1 2 2 3 3 3 4
156
ANTILOGARITHMS
Table 2
N 0 1 2 3 4 5 6 7 8 9 1 2 3 4 5 6 7 8 9
00 1000 1002 1005 1007 1009 1012 1014 1016 1019 1021 0 0 1 1 1 1 2 2 2
.01 1023 1026 1028 1030 1033 1035 1038 1040 1042 1045 0 0 1 1 1 1 2 2 2
.02 1047 1050 1052 1054 1057 1059 1062 1064 1067 1069 0 0 1 1 1 1 2 2 2
.03 1072 1074 1076 1079 1081 1084 1086 1089 1091 1094 0 0 1 1 1 1 2 2 2
.04 1096 1099 1102 1104 1107 1109 1112 1114 1117 1119 0 1 1 1 1 2 2 2 2
.05 1122 1125 1127 1130 1132 1135 1138 1140 1143 1146 0 1 1 1 1 2 2 2 2
.06 1148 1151 1153 1156 1159 1161 1164 1167 1169 1172 0 1 1 1 1 2 2 2 2
.07 1175 1178 1180 1183 1186 1189 1191 1194 1197 1199 0 1 1 1 1 2 2 2 2
.08 1202 1205 1208 1211 1213 1216 1219 1222 1225 1227 0 1 1 1 1 2 2 2 3
.09 1230 1233 1236 1239 1242 1245 1247 1250 1253 1256 0 1 1 1 1 2 2 2 3
.10 1259 1262 1265 1268 1271 1274 1276 1279 1282 1285 0 1 1 1 1 2 2 2 3
.11 1288 1291 1294 1297 1300 1303 1306 1309 1312 1315 0 1 1 1 2 2 2 2 3
.12 1318 1321 1324 1327 1330 1334 1337 1340 1343 1346 0 1 1 1 2 2 2 2 3
.13 1349 1352 1355 1358 1361 1365 1368 1371 1374 1377 0 1 1 1 2 2 2 3 3
.14 1380 1384 1387 1390 1393 1396 1400 1403 1406 1409 0 1 1 1 2 2 2 3 3
.15 1413 1416 1419 1422 1426 1429 1432 1435 1439 1442 0 1 1 1 2 2 2 3 3
.16 1445 1449 1452 1455 1459 1462 1466 1469 1472 1476 0 1 1 1 2 2 2 3 3
.17 1479 1483 1486 1489 1493 1496 1500 1503 1507 1510 0 1 1 1 2 2 2 3 3
.18 1514 1517 1521 1524 1528 1531 1535 1538 1542 1545 0 1 1 1 2 2 2 3 3
.19 1549 1552 1556 1560 1563 1567 1570 1574 1578 1581 0 1 1 1 2 2 3 3 3
.20 1585 1589 1592 1596 1600 1603 1607 1611 1614 1618 0 1 1 1 2 2 3 3 3
.21 1622 1626 1629 1633 1637 1641 1644 1648 1652 1656 0 1 1 2 2 2 3 3 3
.22 1660 1663 1667 1671 1675 1679 1683 1687 1690 1694 0 1 1 2 2 2 3 3 3
.23 1698 1702 1706 1710 1714 1718 1722 1726 1730 1734 0 1 1 2 2 2 3 3 4
.24 1738 1742 1746 1750 1754 1758 1762 1766 1770 1774 0 1 1 2 2 2 3 3 4
.25 1778 1782 1786 1791 1795 1799 1803 1807 1811 1816 0 1 1 2 2 2 3 3 4
.26 1820 1824 1828 1832 1837 1841 1845 1849 1854 1858 0 1 1 2 2 3 3 3 4
.27 1862 1866 1871 1875 1879 1884 1888 1892 1897 1901 0 1 1 2 2 3 3 3 4
.28 1905 1910 1914 1919 1923 1928 1932 1936 1941 1945 0 1 1 2 2 3 3 4 4
.29 1950 1954 1959 1963 1968 1972 1977 1982 1986 1991 0 1 1 2 2 3 3 4 4
.30 1995 2000 2004 2009 2014 2018 2023 2028 2032 2037 0 1 1 2 2 3 3 4 4
.31 2042 2046 2051 2056 2061 2065 2070 2075 2080 2084 0 1 1 2 2 3 3 4 4
.32 2089 2094 2099 2104 2109 2113 2118 2123 2128 2133 0 1 1 2 2 3 3 4 4
.33 2138 2143 2148 2153 2158 2163 2168 2173 2178 2183 0 1 1 2 2 3 3 4 4
.34 2188 2193 2198 2203 2208 2213 2218 2223 2228 2234 1 1 2 2 3 3 4 4 5
.35 2239 2244 2249 2254 2259 2265 2270 2275 2280 2286 1 1 2 2 3 3 4 4 5
.36 2291 2296 2301 2307 2312 2317 2323 2328 2333 2339 1 1 2 2 3 3 4 4 5
.37 2344 2350 2355 2360 2366 2371 2377 2382 2388 2393 1 1 2 2 3 3 4 4 5
.38 2399 2404 2410 2415 2421 2427 2432 2438 2443 2449 1 1 2 2 3 3 4 4 5
.39 2455 2460 2466 2472 2477 2483 2489 2495 2500 2506 1 1 2 2 3 3 4 5 5
.40 2512 2518 2523 2529 2535 2541 2547 2553 2559 2564 1 1 2 2 3 4 4 5 5
.41 2570 2576 2582 2588 2594 2600 2606 2612 2618 2624 1 1 2 2 3 4 4 5 5
.42 2630 2636 2642 2649 2655 2661 2667 2673 2679 2685 1 1 2 2 3 4 4 5 6
.43 2692 2698 2704 2710 2716 2723 2729 2735 2742 2748 1 1 2 3 3 4 4 5 6
.44 2754 2761 2767 2773 2780 2786 2793 2799 2805 2812 1 1 2 3 3 4 4 5 6
.45 2818 2825 2831 2838 2844 2851 2858 2864 2871 2877 1 1 2 3 3 4 5 5 6
.46 2884 2891 2897 2904 2911 2917 2924 2931 2938 2944 1 1 2 3 3 4 5 5 6
.47 2951 2958 2965 2972 2979 2985 2992 2999 3006 3013 1 1 2 3 3 4 5 5 6
.48 3020 3027 3034 3041 3048 3055 3062 3069 3076 3083 1 1 2 3 3 4 5 6 6
.49 3090 3097 3105 3112 3119 3126 3133 3141 3148 3155 1 1 2 3 3 4 5 6 6
157
LABORATORY MANUAL CHEMISTRY
ANTILOGARITHMS
Table 2 continued
N 0 1 2 3 4 5 6 7 8 9 1 2 3 4 5 6 7 8 9
.50 3162 3170 3177 3184 3192 3199 3206 3214 3221 3228 1 1 2 3 4 4 5 6 7
.51 3236 3243 3251 3258 3266 3273 3281 3289 3296 3304 1 2 2 3 4 5 5 6 7
.52 3311 3319 3327 3334 3342 3350 3357 3365 3373 3381 1 2 2 3 4 5 5 6 7
.53 3388 3396 3404 3412 3420 3428 3436 3443 3451 3459 1 2 2 3 4 5 6 6 7
.54 3467 3475 3483 3491 3499 3508 3516 3524 3532 3540 1 2 2 3 4 5 6 6 7
.55 3548 3556 3565 3573 3581 3589 3597 3606 3614 3622 1 2 2 3 4 5 6 7 7
.56 3631 3639 3648 3656 3664 3673 3681 3690 3698 3707 1 2 3 3 4 5 6 7 8
.57 3715 3724 3733 3741 3750 3758 3767 3776 3784 3793 1 2 3 3 4 5 6 7 8
.58 3802 3811 3819 3828 3837 3846 3855 3864 3873 3882 1 2 3 4 4 5 6 7 8
.59 3890 3899 3908 3917 3926 3936 3945 3954 3963 3972 1 2 3 4 5 5 6 7 8
.60 3981 3990 3999 4009 4018 4027 4036 4046 4055 4064 1 2 3 4 5 6 6 7 8
.61 4074 4083 4093 4102 4111 4121 4130 4140 4150 4159 1 2 3 4 5 6 7 8 9
.62 4169 4178 4188 4198 4207 4217 4227 4236 4246 42S6 1 2 3 4 5 6 7 8 9
.63 4266 4276 4285 4295 4305 4315 4325 4335 4345 4355 1 2 3 4 5 6 7 8 9
.64 4365 4375 4385 4395 4406 4416 4426 4436 4446 4457 1 2 3 4 5 6 7 8 9
.65 4467 4477 4487 4498 4508 4519 4529 4539 4550 4560 1 2 3 4 5 6 7 8 9
.66 4571 4581 4592 4603 4613 4624 4634 4645 4656 4667 1 2 3 4 5 6 7 9 10
.67 4677 4688 4699 4710 4721 4732 4742 4753 4764 4775 1 2 3 4 5 7 8 9 10
.68 4786 4797 4808 4819 4831 4842 4853 4864 4875 4887 1 2 3 4 6 7 8 9 10
.69 4898 4909 4920 4932 4943 4955 4966 4977 4989 5000 1 2 3 5 6 7 8 9 10
.70 5012 5023 5035 5047 5058 5070 5082 5093 5105 5117 1 2 4 5 6 7 8 9 11
.71 5129 5140 5152 5164 5176 5188 5200 5212 5224 5236 1 2 4 5 6 7 8 10 11
.72 5248 5260 5272 5284 5297 5309 5321 5333 5346 5358 1 2 4 5 6 7 9 10 11
.73 5370 5383 5395 5408 5420 5433 5445 5458 5470 5483 1 3 4 5 6 8 9 10 11
.74 5495 5508 5521 5534 5546 5559 5572 5585 5598 5610 1 3 4 5 6 8 9 10 12
.75 5623 5636 5649 5662 5675 5689 5702 5715 5728 5741 1 3 4 5 7 8 9 10 12
.76 5754 5768 5781 5794 5808 5821 5834 5848 5861 5875 1 3 4 5 7 8 9 11 12
.77 5888 5902 5916 5929 5943 5957 5970 5984 5998 6012 1 3 4 5 7 8 10 11 12
.78 6026 6039 6053 6067 6081 6095 6109 6124 6138 6152 1 3 4 6 7 8 10 11 13
.79 6166 6180 6194 6209 6223 6237 6252 6266 6281 6295 1 3 4 6 7 9 10 11 13
.80 6310 6324 6339 6353 6368 6383 6397 6412 6427 6442 1 3 4 6 7 9 10 12 13
.81 6457 6471 6486 6501 6516 6531 6546 6561 6577 6592 2 3 5 6 8 9 11 12 14
.82 6607 6622 6637 6653 6668 6683 6699 6714 6730 6745 2 3 5 6 8 9 11 12 14
.83 6761 6776 6792 6808 6823 6839 6855 6871 6887 6902 2 3 5 6 8 9 11 1314
.84 6918 6934 6950 6966 6982 6998 7015 7031 7047 7063 2 3 5 6 8 10 11 13 15
.85 7079 7096 7112 7129 7145 7161 7178 7194 7211 7228 2 3 5 7 8 10 12 13 15
.86 7244 7261 7278 7295 7311 7328 7345 7362 7379 7396 2 3 5 7 8 10 12 13 15
.87 7413 7430 7447 7464 7482 7499 7516 7534 7551 7568 2 3 5 7 9 10 12 14 16
.88 7586 7603 7621 7638 7656 7674 7691 7709 7727 7745 2 4 5 7 9 11 12 14 16
.89 7762 7780 7798 7816 7834 7852 7870 7889 7907 7925 2 4 5 7 9 11 13 14 16
.90 7943 7962 7980 7998 8017 8035 8054 8072 8091 8110 2 4 6 7 9 11 13 15 17
.91 8128 8147 8166 8185 8204 8222 8241 8260 8279 8299 2 4 6 8 9 11 13 15 17
.92 8318 8337 8356 8375 8395 8414 8433 8453 8472 8492 2 4 6 8 10 12 14 15 17
.93 8511 8531 8551 8570 8590 8610 8630 8650 8670 8690 2 4 6 8 10 12 14 16 18
.94 8710 8730 8750 8770 8790 8810 8831 8851 8872 8892 2 4 6 8 10 12 14 16 18
.95 8913 8933 8954 8974 8995 9016 9036 9057 9078 9099 2 4 6 8 10 12 15 17 19
.96 9120 9141 9162 9183 9204 9226 9247 9268 9290 9311 2 4 6 8 11 13 15 17 19
.97 9333 9354 9376 9397 9419 9441 9462 9484 9506 9528 2 4 7 9 11 13 15 17 20
.98 9550 9572 9594 9616 9638 9661 9683 9705 9727 9750 2 4 7 9 11 13 16 18 20
.99 9772 9795 9817 9840 9863 9886 9908 9931 9954 9977 2 5 7 9 11 14 16 18 20
158
N OTE
N OTE