Table Of ContentA Book Of
PRACTICAL
CHEMISTRY
(CH - 223)
For S.Y.B.Sc.
As per New Revised Syllabus with Effect from June 2014
Dr. S. S. Jadhav
Vice Principal,
New Arts, Commerce and Science College,
AHMEDNAGAR
Dr. G. S. Gugale Dr. A. V. Nagawade
Head and Associate Professor Associate Professor
Department of Chemistry, Department of Chemistry,
H. V. Desai College Ahmednagar College,
PUNE – 411002. AHMEDNAGAR.
Dr. A. D. Natu Dr. V. D. Bobade
Ex. Head, Associate Professor
Department of Chemistry, Department of Chemistry,
Abasaheb Garware College, H.P.T. Arts, R. Y. K Science College,
PUNE – 411020. NASHIK – 422210.
N2258
S.Y.B.Sc. Practical Chemistry ISBN 978-93-5164-008-0
Fourth Edition : July 2018
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Preface …
It gives us an immense pleasure to place this text book of S.Y.B.Sc. Practical
Chemistry (CH-223) in the hands of S.Y.B.Sc. students. This book has been presented to
you according to the new revised syllabus implemented from June 2014.
We hope that the book will fulfil the expectations of students and teachers. We hope
that this book will cater the exact requirements of students.
We are grateful to our dynamic publisher Shri. Dineshbhai Furia, Shri. Jignesh Furia,
Mr. M. P. Munde and all staff of Nirali Prakashan especially Mr. Ilyas Shaikh, Mr. Kiran
Velankar and Ms. Chaitali Takle for their efforts and keen interest in publishing this book
in a very limited span of time.
Any comment, criticism and suggestions from the readers for improving the book will
be highly appreciated.
AUTHORS
Contents …
Page
(A) Physical Chemistry Practicals (Any Five)
1. To determine the critical solution temperature of phenol-water system. 1-4
2. To determine molecular weight of given organic liquid by steam 5-9
distillation method.
3. Determination of solubility of benzoic acid at different temperature and 9-14
to determine ∆H of dissolution process.
4. To study neutralization of acid (HCl) by base (NaOH), CH3COOH by 14-22
NaOH and H2SO4 by NaOH.
5. To determine the rate constant (or to study kinetics) of acid catalysed 26-29
ester hydrolysis.
6. To determine the rate constant of base catalysed ester hydrolysis. 29-31
7. Partition coefficient of iodine between water and carbon tetrachloride. 32-38
(B) Inorganic Chemistry Practicals (Minimum Five Mixtures)
Inorganic Qualitative Analysis 39-58
1. One simple mixture (without phosphate or borate).
2. Two mixtures containing PO3− (with PO3− removal).
4 4
3. Two mixtures containing BO3− (with BO3− removal).
3 3
Inorganic Qualitative Analysis of Binary Mixtures (including phosphate and
borate removal).
Sodium carbonate extract is to be used wherever necessary for detecting
acidic radicals.
(C) Organic Chemistry Practicals
(a) Organic qualitative analysis of binary mixtures without ether 59-76
separation (Four only).
Two: solid-solid, one: solid-liquid, one; liquid-liquid.
(b) Organic Preparations :
(Any two including Crystallization, MP, TLC)
1. Phthalic anhydride to phthalimide 77-78
2. Glucose to glucosazone 78-80
3. Acetanilide to p-bromoacetanilide 81-82
4. Benzaldehyde to dibenzylidene acetone 82-84
(D) Analytical Chemistry Practicals (Any Five)
1. Estimation of sodium carbonate content of washing soda. 85-90
2. Determination of calcium in the presence of magnesium using EDTA. 90-94
3. (a) Preparation of standard 0.05 N oxalic acid solution and 95-101
standardisation of approx. 0.05 N KMnO4 solution.
(b) Determination of the strength of given H2O2 solution with
standardised 0.05 N KMnO4 solution.
4. Estimation of Aspirin from a given tablet and to find errors in 102-107
quantitative analysis.
5. Estimation of Al (III) from the given aluminium salt solution by using 107-111
Eriochrome Black-T indicator (Black titration method)
6. Iodometric estimation of copper. 112-117
7. Report on one day industrial educational visit. 118-120
Appendix - I 121-123
Appendix - II 124-128
− − −
SECTION - A
PHYSICAL CHEMISTRY PRACTICALS
(Any Five)
Experiment No. 1
PHENOL-WATER SYSTEM
AIM :
To determine the critical solution temperature of phenol-water system.
THEORY :
Phenol and water are partially miscible liquids with each other at room temperature.
Thus, when water is mixed with phenol, following two separate layers are formed :
(i) Saturated solution of phenol in water, (ii) Saturated solution of water in phenol. We know
that the solubility increases with increase in temperature. Consequently at a particular
temperature, two liquids become completely soluble (miscible) with each other. The
miscibility temperature depends on the percent composition of two liquids present in the
solution. In case of phenol-water system, miscibility temperature is highest for a particular
composition. This temperature is called as critical solution temperature of phenol-water
system. Above the critical solution temperature, phenol and water are completely miscible
with each other for all the compositions. Thus, above critical solution temperature, only one
phase (homogeneous solution) is obtained when phenol and water are mixed with each
other in any proportions. Below this temperature the system may exist in miscible form or
immiscible form depending upon the composition and temperature both.
In this experiment, phenol and water proportions are varied in their solutions and for
each proportion miscibility temperature is experimentally measured by heating. Graph of
% phenol versus miscibility temperature is plotted from which, critical solution temperature
and critical composition (% of phenol and % of water) are obtained.
(1)
S.Y.B.Sc. Practical Chemistry 2 Physical Chemistry Practicals
th
1
thermometer
10
Stirrer
Rubber�cork
Water�bath
Iron�stand
Mixture�of�phenol�and�water�and
it�should�be�completely�dipped
in�the�water�of�water�bath
Wire�gauze
Burner
Tripod�stand
Fig. 1.1: Experimental set up of phenol-water system
APPARATUS :
th
250 ml beaker, hard glass test tube with rubber cork and stirrer, 1/10 thermometer,
measuring cylinder, burette etc.
CHEMICALS :
Distilled water, pure phenol.
PROCEDURE :
1. Take 10 g (9.5 ml) of phenol in a hard glass test tube using measuring cylinder. Add
to it 4 g (4 ml) distilled water using a burette.
2. Fit the cork with a thermometer and a stirrer to this tube. Mount the test tube in a
water bath or a sand bath. Refer Fig. 1.1 (Sand heats up and cools faster).
3. Heat the mixture on the bath slowly with constant stirring. While stirring mixture
appears turbid until it is immiscible indicating the presence of two distinct phases.
At an elevated temperature, the solution becomes miscible and turbidity disappears.
As soon as the turbidity disappears, note this temperature (t ). But as heating is a
1
fast process and temperature of the system increases very rapidly one cannot note
down the correct mixing temperature. Therefore as cooling is slow process and
temperature decrease very slowly. Therefore to note exact temperature of mixing
S.Y.B.Sc. Practical Chemistry 3 Physical Chemistry Practicals
remove the burner and allow the total system to cool down. But it will take a very
long time. Therefore the hard glass tube is taken outside the water bath along with
the clamp and fix it properly. Now the mixture comes in direct contact with the open
atmosphere and the cooling is faster. Let the solution cool while stirring constantly.
As soon as few white shine crystals appear, note down the temperature (t2) at which
turbidity reappears, t2 is noted as the miscibility temperature.
4. Add 3 ml of water to the contents of the tube. This will form the second composition
given in the table. Repeat the same procedure for this mixture and measure its
miscibility heating temperature (t1) and cooling temperature (t2). After completion of
set I for 10 gms of phenol, throw this mixture carefully in the basin and go for the
set II.
5. Likewise prepare the various compositions of phenol and water as given in the
observation table for set II i.e. 5 gms and set III for 2.5 gms of phenol. Repeat the
same procedure as set I for set II and III and report the heating (t1) and cooling (t2)
temperature in the observation table.
6. Plot the graph of % phenol versus miscibility temperature. It is a bell-shaped curve
as shown in Fig. 1.2. The temperature tc on Y-axis corresponding to point H on the
graph is critical solution temperature and the composition corresponding to this
point on X-axis is the critical composition C of the phenol-water system.
The expected critical solution temperature is 68.10°C and expected critical composition
is 37% phenol and 63% water.
Graph :
H
t
c
50
40
Temperature
30
20
10
10 20 30 40 50 60 70 80 90 100
%�Phenol
Fig. 1.2 : Graph of % phenol versus temperature
Note : Phenol is highly corrosive to skin, hence it should be handled with care.
S.Y.B.Sc. Practical Chemistry 4 Physical Chemistry Practicals
OBSERVATIONS :
Miscibility Temperatures
Amount of Amount of
Sr. No. % Phenol % Water
Phenol (g) Water (g) Heating (t ) Cooling (t )
1 2
1. 10 6 62.50 37.5
Set I 2. 10 9 52.60 57.4
3. 10 12 45.40 54.6
4. 10 15 40.00 60.0
Set II 5. 5 10 33.3 66.7
6. 5 15 25.0 75.0
7. 2.5 15 14.3 85.7
Set III 8. 2.5 20 11.1 88.9
9. 2.5 25 9.1 90.9
Note : 10 g phenol = 9.5 ml (density = 1.053 g/ml)
5 g phenol = 4.8 ml
2.5 g phenol = 2.4 ml
Amount of phenol
CALCULATIONS : % Phenol = × 100
Amount of phenol + Water
% Water = 100 − % Phenol
RESULTS :
1. Critical solution temperature = ……………… °C
2. % Phenol at critical solution temperature = ……………… %
3. % Water at critical solution temperature = ……………… %
QUESTIONS
1. What do you mean by critical solution temperature ?
2. How to find critical solution temperature ?
3. Whether phenol is completely soluble in water or not at room temperature ?
4. List the different types of immiscible liquids.
5. What is the effect of temperature on solubility ?
6. What is the density of phenol ?
7. What is the percentage of phenol at critical solution temperature ?
8. Explain the graph of % phenol against miscibility temperature.
9. What are conjugate solutions ?
✍ ✍ ✍
