PRACTICAL CHEMISTRY B. Sc G. S. Gugale A. V. Nagawade R. A. Pawar S. S. Jadhav V. D. Bobade A. D. Natu D. R. Thube P. C. Mhaske L. K. Nikam Nirali Prakashan

316 Pages·2019·1.85 MB·English

by  Gugale A. V. Nagawade R. A. Pawar S. S. Jadhav V. D. Bobade A. D. Natu D. R. Thube P. C. Mhaske L. K. Nikam

A Book Of

PPRRAACCTTIICCAALL
CCHHEEMMIISSTTRRYY
T.Y.B.Sc. Chemistry : CH-347, CH-348, CH-349
As Per New Revised Syllabus of Savitribai Phule Pune University
With Effect from June 2015

Dr. G. S. Gugale
Head & Associate Professor,
Dept. of Chemistry,
H. V. Desai College, PUNE

Dr. A. V. Nagawade Dr. R. A. Pawar
Associate Professor, Dept. of Chemistry, Associate Professor, Dept. of Chemistry
Ahmednagar College, Baburaoji Gholap College,
AHMEDNAGAR. Sangvi, PUNE.

Dr. S. S. Jadhav Dr. V. D. Bobade
Vice-Principal, Head & Associate Professor, Associate Professor, Dept. of Chemistry,
New Arts, Commerce and Science College, H.P.T. Arts, R.Y.K. Science College,
AHMEDNAGAR. NASHIK.

Dr. A. D. Natu Dr. D. R. Thube
Ex. Head, Dept. of Chemistry, Head, PG Dept. of Chemistry,
Abasaheb Garware College, New Arts, Commerce & Science College,
PUNE. Parner, AHMEDNAGAR.

Dr. P. C. Mhaske Dr. L. K. Nikam
Associate Professor, Associate Professor, Dept. of Chemistry,
Dept. of Chemistry Baburaoji Gholap College,
S. P. College, PUNE. Sangvi, PUNE.
Price ` 240.00

N1848
T.Y.B.Sc. : Practical Chemistry ISBN 978-93-51645-84-9
Second Edition : July 2017
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Preface …

It gives us an immense pleasure to place this “Text Book of Practical Chemistry” in
the hands of T.Y.B.Sc. students. The Book has been written according to the revised
semester pattern of Savitribai Phule Pune University implemented from June 2015.
The book is divided into three sections : (i) Physical, (ii) Inorganic, (iii) Organic
Chemistry Practicals. An attempt is made to give appropriate theoretical background of
each experiment. Procedures, observation tables and calculations are made more simple.
At the end of each experiment, viva-voce questions are given for practice.
All the experiments are written keeping in view the specification of learning
objectives. Micro techniques, double burette methods are adopted wherever possible.
Sincere efforts are made to make the practicals more simple.
We feel that the book will be very useful to the students during their regular
practicals as well as at the time of examination.
We are thankful to Mr. Dineshbhai Furia and Mr. Jignesh Furia for taking keen
interest in publishing this book.
We are also thankful to staff of Nirali Prakashan especially, Mr. Ilyas Shaikh, Mr. Kiran
Velankar and Mrs. Anjali Muley for completing this book on time.
We are also thankful to Marketing staff especially, Mr. Nilesh Deshmukh and others
for coordinating the matter well in time.
Suggestions for improving the book will be highly appreciated.

Authors
Contents …

Physical Chemistry Practicals
CH - 347
Group A
1. Chemical Kinetics (Any Five)
1. To study the effect of concentration of the reactants on the rate of … 7
hydrolysis of an ester.
2. To compare the relative strength of HCl and H SO by studying the kinetics … 9
2 4
of hydrolysis of an ester.
3. To compare the relative strength of HCl and H SO by studying the kinetics … 12
2 4
of inversion of cane sugar using Polarimeter.
4. To study the kinetics of iodination of acetone. … 17
5. To determine the first order velocity constant of the decomposition of … 20
hydrogen peroxide by volume determination of oxygen.
6. To determine the energy of activation of the reaction between potassium … 23
iodide and potassium persulphate.
7. To determine the order of reaction between K S O and KI by half-life … 27
2 2 8
method.
2. Viscosity
8. To determine the molecular weight of a high polymer by using solutions of … 32
different concentrations.
3. Adsorption :
9. To investigate the adsorption of oxalic acid/acetic acid by activated … 39
charcoal and test the validity of Freundlich/Langmuir isotherm.
4. Phenol-Water System
10. To study the effect of addition of salt on critical solution temperature of … 43
phenol-water system.
5. Transport Number
11. To determine the transport number of cation by moving boundary method. … 47
6. Refractometry (Any Two)
1. To determine the specific refractivities of the given liquids A and B and … 55
their mixture and hence determine the percentage composition of their
mixture C.
2. To determine the molecular refractivity of the given liquids A, B, C and D. … 57
3. To determine the molar refraction of homologues methyl, ethyl and propyl … 59
alcohol and show the constancy contribution to the molar refraction by
−CH group.
2
Group B
1. Colorimetry (Any Two)
1. Determination of λ and concentration of unknown solution of KMnO in … 63
max 4
2 N H SO .
2 4
2. Determination of λ and concentration of unknown solution of CuSO . … 64
max 4
3. To titrate Cu2+ ions with EDTA photometrically. … 68
4. To determine the indicator constant of methyl red indicator. … 70
2. Potentiometry (Any Three)
1. To prepare standard 0.2 M Na HPO and 0.1 M citric acid solution, hence … 80
2 4
prepare four different buffer solutions using them. Determine the pK value
a
of these and unknown solutions.
2. To determine the concentrations of strong acid and weak acid present in the … 83
mixture by titrating with strong base.
3. To determine the formal redox potential of Fe2+/Fe3+ system … 86
potentiometrically.
4. To determine the amount of NaCl in the given solution by potentiometric … 90
titration against silver nitrate.
5. To determine the amount of Cl− and Br− from the given halide mixture by … 93
titrating with silver nitrate solution.
3. pH Metry (Any Two)
1. To determine the degree of hydrolysis of aniline hydrochloride. … 101
2. To determine the pK value of given weak acid by pH-metric titration with … 103
a
strong base.
3. To determine the dissociation constant of oxalic acid by pH-metric titration … 105
with strong base.
4. To determine pH of various mixtures of sodium acetate and acetic acid in … 108
aqueous solution and hence to find the dissociation of acetic acid.
4. Radioactivity (Any One)
1. To determine plateau voltage of the given GM counter. … 113
2. To determine the resolving time of GM counter. … 115
3. To determine E of beta particles. … 116
max
5. Conductometry (Any Two)
1. To determine the cell constant of the given cell using 0.01 M KCl solution … 124
and hence determine dissociation constant of a given monobasic weak acid.
2. To estimate the amount of lead present in the given solution of lead nitrate … 128
by conductometric titration with sodium sulphate.
3. To investigate the conductometric titration of any one of the following : … 131
(a) Strong acid against strong base. … 131
(b) Strong acid against weak base. … 132
(c) Strong base against weak acid.
… 134
(d) Weak acid against weak base.
… 135
Appendices … 139
Inorganic Chemistry Practicals
CH - 348
(A) Gravimetric Estimations (Any Three)
1. Fe as Fe O . … 143
2 3
2. Nickel as Ni - DMG. … 145
3. Al as Aluminium oxide. … 148
4. Gravimetric estimation of Ba as BaSO using homogeneous precipitation … 151
4
method.
(B) Volumetric Estimations (Any Four)
1. Mn by Volhard’s method. … 154
2. Estimation of NO− by using KMnO . … 159
2 4
3. Estimation of % purity of given sample of Sodium chloride. … 163
4. Analysis of Brass - Estimation of copper by Iodometry. … 166
5. Fertilizer analysis (PO )3−. … 171
4
(C) Inorganic Preparations (Any Four)
1. Preparation of Hexamminenickel(II) chloride, [Ni(NH ) ]Cl . … 176
3 6 2
2. Preparation of Potassium trioxalatoferrate(III) trihydrate, … 179
K [Fe(C O ) ].3H O.
3 2 4 3 2
3. Preparation of Tetraamminecopper(II) sulphate monohydrate, … 182
[Cu(NH ) ]SO .H O.
3 4 4 2
4. Preparation of Manganese(III) acetylacetone [Mn(acac) ]. … 184
3
5. Preparation of Tris (Thiourea) Copper(I) chloride [Cu(Thiourea) ]Cl. … 186
3
(D) Colorimetric Estimations (Any Two)
1. Iron by thiocyanate method. … 188
2. Cobalt by using R-nitroso salt method. … 192
3. Titanium by H O . … 195
2 2
(E) Separation of Binary Mixture of Cations by Column Chromatography … 202
(3 Mixtures)
(One Mixture should be colourless, Zn + Al, Zn + Mg)
OR
(E) Flame Photometry Analysis (Any Three)
1. Estimation of Na by flame photometry by calibration curve method. … 208
2. Estimation by Na by flame photometry by regression method. … 211
3. Estimation of K by flame photometry by calibration curve method. … 212
4. Estimation of K by flame photometry by regression method. … 215
(F) Inorganic Qualitative Analysis
(4 Mixtures including Borates and Phosphates) … 217
Appendices … 238
Organic Chemistry Practicals
CH - 349
(A) Separation of Binary Mixtures and Qualitative Analysis
(Minimum 8 Mixtures)
(a) Solid-Solid (4 Mixtures). … 247
(b) Solid-Liquid (2 Mixtures). … 247
(c) Liquid-Liquid (2 Mixtures). … 249
Atleast one mixture from each of the following should be given : Acid-Base, Acid-Phenol,
Acid-Neutral, Phenol-Base, Phenol-Neutral, Base-Neutral, Neutral-Neutral.
(i) Separation and qualitative analysis of the binary mixtures should be carried out on
micro scale using micro scale bits.
(ii) Name and structure of the separated components of the binary mixture is not
necessary.
(iii) Students are expected to record the Type, Preliminary tests, Physical constants,
Elements and Functional groups only.
(iv) The purified samples of the separated components should be submitted.
(B) Organic Estimations (Any Four)
(1) Estimation of Acetamide. … 265
(2) Estimation of Glucose. … 268
(3) Estimation of Ethyl benzoate. … 271
(4) Determination of molecular weight of monobasic/dibasic organic acids by
volumetric methods. … 274
(C) Organic Preparations (Any Eight)
(1) Preparation of Adipic acid from Cyclohexanone (Oxidation by conc. HNO ) … 279
3
(2) Benzoquinone from Hydroquinone (Oxidation by KBrO /K CrO ) … 280
3 2 3
(3) p-nitroacetanilide from Acetanilide (Nitration) … 282
(4) 2-Naphthyl methyl ether from 2-naphthol (Methylation by DMS, NaOH) … 283
(5) Hippuric acid by Glycine (Benzoylation) … 285
(6) p-iodonitrobenzene from p-nitroaniline (Sandmeyer reaction) … 286
(7) Benzoic acid from Ethyl benzoate (Ester hydrolysis) … 288
(8) p-Bromoacetanilide from Acetanilide (Bromination) … 289
(9) Paracetamol from p-Hydroxyaniline (Acetylation) … 290
(10) Ethyl benzene from Acetophenone (Wolff Kishner reduction) … 292
Appendices … 295
− − −
Course - I

CH-347

PHYSICAL CHEMISTRY

PRACTICALS

1
T.Y.B.Sc. Practical Chemistry (Physical Practicals) Chemical Kinetics

STRUCTURE OF PRACTICAL EXAMINATION

COURSE – I
CH – 347

Physical Chemistry Practicals

Marks
Q.1 One Experiment from Group – A 35
Q.2 One Experiment from Group – B 35
Q.3 Oral 10

2