practical inorganic chemistry practical inorganic

Shikha GulatiJL Sharma

Shagun Manocha

CBS Publishers & Distributors Pvt Ltd

PracticalInorganicChemistry

Practical Inorganic Chem

istryG

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ano

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Dedicated to Education

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under Choice-Based Credit System (CBCS) Scheme ofDelhi University for BSc (Hons and Programme) Courses

9 789386 310880

ISBN: 978-93-86310-88-0

PracticalInorganic Chemistryunder Choice-Based Credit System (CBCS) Scheme ofDelhi University for BSc (Hons and Programme) Courses

is primarily a laboratory manual on inorganic chemistry, based upon the syllabi of Delhi University under choice-based credit system (CBCS) scheme, aimed to meet the requirements of undergraduate students, teachers, researchers, industrial chemists and laboratory staff. Each experiment is supplemented with detailed theory, illustrations, observation table with calculation and viva vove questions for practice. Topics like LABORATORY SAFETY INSTRUCTIONS and FIRST AID are also included. In addition, teachers’ notes to each experiment are given for reference to help the teachers, researchers, industrial chemists and laboratory staff.

Simple and lucid style of presentationAdheres to choice-based credit system (CBCS) scheme of Delhi UniversityCore underlying concept of each experiment with theory, elaborate illustrations, observation table and calculationViva voce questions on each experimentExperiment-related problems and their solutionsTeachers’ notes Important points to remember

Salient Features of the book•••

••••

Shikha Gulati PhD

JL Sharma PhD

Shagun Manocha MSc

is currently Assistant Professor, Department of Chemistry, Sri Venkateswara College, University of Delhi. She joined Green Chemistry Network Centre (GCNC), Department of Chemistry, University of Delhi, in 2009 as a doctoral student. She has authored several research papers in international journals and wrtitten books as well as topics in diverse books. She has handled various instruments such as GC-MS, ED-XRF, IR, AAS, auto-titrator, UV–VIS spectrophotometer, microwave digester, etc. She has been awarded several prizes in poster and given oral presentations, and demonstrated chemistry experiments in several national and international workshops. She is affiliated to Royal Society of Chemistry (RCS), London, and Indian Society of Analytical Scientists (ISAS).

is currently Associate Professor, Department of Chemistry, Kirori Mal College, University of Delhi. He has 33 years of experience in teaching at undergraduate level. He actively takes part in organizing seminars/symposiums/conferences for promoting scientific culture among youngsters teaching inorganic chemistry and environmental chemistry, and research related to trace analysis in environmental applications. He has compiled chemistry dictionaries. He is Chairman, Petrotech Society of India, Delhi–NCR, and Vice Chairman, Indian Society of Analytical Scientists (ISAS–DC).

is currently Assistant Professor, Department of Chemistry, Maitreyi College, University of Delhi. She has been teaching for several years in prestigious colleges of Delhi University at undergraduate level. She actively takes part in conferences and workshops. She has been associated with ISAS.

PracticalInorganic Chemistry


Shikha Gulati PhD

Department of ChemistrySri Venkateswara College

University of DelhiE-mail: [email protected]

JL Sharma PhD

Department of ChemistryKirori Mal CollegeUniversity of Delhi

Shagun Manocha MSc

Department of ChemistryMaitreyi College

University of Delhi


New Delhi • Bengaluru • Chennai • Kochi • Kolkata • MumbaiHyderabad • Nagpur • Patna • Pune • Vijayawada

PracticalInorganic Chemistry


ISBN: 978-93-86310-88-0

Copyright © Authors and Publisher

First Edition: 2017

All rights reserved. No part of this book may be reproduced or transmitted in any form or by anymeans, electronic or mechanical, including photocopying, recording, or any information storageand retrieval system without permission, in writing, from the authors and the publisher.

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Practical Inorganic Chemistry

Disclaimer

Science and technology are constantly changingfields. New research and experience broaden thescope of information and knowledge. The authorshave tried their best in giving information availableto them while preparing the material for this book.Although, all efforts have been made to ensureoptimum accuracy of the material, yet it is quitepossible some errors might have been leftuncorrected. The publisher, the printer and the authorswill not be held responsible for any inadvertent errors,omissions or inaccuracies.

tomy husband

Amit

—Shikha Gulati

viivii

The book is primarily a laboratory manual on inorganic chemistry for advanced collegeeducation, which has been designed keeping in mind the Delhi University syllabi underchoice-based credit system (CBCS) scheme for BSc (Hons and Programme) courses.

All the laboratory experiments of inorganic chemistry are organized into ten chapters,which provide theoretical as well as practical aspects of each experiment. The topicsinclude semi-micro qualitative analysis, volumetric, gravimetric and spectrophotometricanalysis, inorganic compounds preparations, preparation of inorganic reagents andsome miscellaneous experiments are described in detail with illustrations. Topics likelaboratory safety instructions and first aid are typically not available in practical booksbut indispensable for safe working in a chemistry laboratory are also included.Comprehensive theory to each experiment has been provided, so that the purpose ofdoing an experiment can be easily understood. In each experiment, observation tablesalong with the calculations are given which are highly beneficial for students. Someimportant questions related to the experiments for viva voce examination are providedat the end of each experiment. Teachers’ notes to each experiment have been given atthe end, which can be a ready-reckonor for teachers and researchers. Also, a chapter onthe preparation of laboratory inorganic reagents has been included which will not onlyhelp teachers but the laboratory staff who prepare these shelf and bench reagents. Hence,this textbook not only provides training to the students but also serves as a referencebook for teachers, laboratory staff, researchers and industrial chemists.

In fact, this is a modest endeavour on our part. Perhaps, we could not have startedsuch an endeavor because of our confines but for Cardinal Newman’s motivating words,‘A man would do nothing, if he waited until he could do it so well that no one could find faultwith what he has done’.

We believe that this book will be useful not only to the chemistry department butalso for other science departments especially biochemistry, botany and zoology, wheremany of these experiments are performed.

Though, all efforts have been made to make this book error free, yet some errorsmight have crawled in inadvertently. Constructive criticism and suggestions are highlywelcome.


Shagun Manocha

Preface

Acknowledgements

ixix

I thank God for his showers of blessings throughout my life. After God, I would like toexpress my deepest gratitude to Dr P Hemalatha Reddy, Principal, Sri VenkateswaraCollege for her munificent and fruitful advice, motherly encouragement, selfless support,and continuous follow-up during work, readiness to help all the time, and facilitatingsuitable family like environment in the college. I also thank her for providing wellequipped ICT laboratory and library which helped me a lot during this work. I expressmy gratitude to my parents, husband and all teachers for their encouragement andinspiration. Shikha GulatiI thank God, the almighty for his blessings throughout my life and conceding me thepotential to complete the book successfully. JL SharmaI would like to express my sincere gratitude to all my teachers for their helpfulsuggestions and insightful comments during the preparation of the book which helpedus a lot. Shagun ManochaWe express our gratitude to Dr Nitin Kohli for his precious advice and constantencouragement. However, several people have knowingly and unknowingly helpedus in the successful completion of this book, so we would like to thank them all.


Shagun Manocha

xi

Contents

Preface vii1. LABORATORY SAFETY RULES AND FIRST AID 1

Introduction 1Classification of Hazards in a Chemistry Laboratory 1General Chemistry Safety and Laboratory Rules 3Safety Symbols 7First Aid in Chemistry Laboratory 7

2. CALIBRATION OF APPARATUS 11Introduction 11Sample Problem 14Viva Voce Questions 14

3. VOLUMETRIC ANALYSIS 15Introduction 15Standard Solution 16Indicator 16Types of Titration 17Units of Concentration in Volumetric Analysis 17Calculation in Titration 21Know Your Volumetric Apparatus 22Cleaning of Titration Apparatus 26Acid–Base Titration 26Detection of End Point: Acid–Base Indicators 27Titration Curve 30

Experiment 3.1: Determination of strength of sodium hydroxide (NaOH) solutionvolumetrically 33Experiment 3.2: Determination of strength of sodium carbonate (Na2CO3) solution usingstandardized HCl (~ N/20) 35Experiment 3.3: Determination of strength of sodium carbonate and sodium bicarbonatepresent together in the mixture by titrating against HCl solution (~ N/20) 38Experiment 3.4: Determination of strength of sodium carbonate and sodium hydroxidepresent together in the mixture by titrating against HCl solution (~ N/20) 43Experiment 3.5: Determination of the amount of free alkali present in different soaps/detergents 48Experiment 3.6: Determination of total alkalinity in water samples from different sources 51

Redox Titration 54Redox Titration Curve 55

xii Practical Inorganic Chemistry

Detection of the End Point in Redox Titration 58Experiment 3.7: Determination of strength of oxalic acid solution by titrating againstpotassium permanganate solution 60Experiment 3.8: Determination of strength of Mohr’s salt solution (ferrous ammoniumsulphate) by titrating against KMnO4 solution 63Experiment 3.9: Determination of number of water molecules of crystallization in Mohr’ssalt 66Experiment 3.10: Determination of strength of Mohr’s salt solution by titrating againstpotassium dichromate using diphenylamine 68Experiment 3.11: Determination of strength of Mohr’s salt solution by titrating againstK2Cr2O7 using N-phenylanthranilic acid 71Experiment 3.12: Determination of strength of oxalic acid and sodium oxalate 74Experiment 3.13: Determination of content of iron present in the given ore by titrating againstK2Cr2O7 77

Iodimetric and Iodometric Titrations 80Experiment 3.14: Determination of strength of copper sulphate solution iodometrically 82Experiment 3.15: Determination of strength of K2Cr2O7 solution iodometrically 86Experiment 3.16: Determination of strength of tartar emetic solution iodimetrically 89Experiment 3.17: Determination of chlorine in commercial sample of bleaching powderiodometrically 92Experiment 3.18: Determination of dissolved oxygen (DO) in water sample iodo-metrically 94

Complexometric Titrations 96Experiment 3.19: Determination of strength of Mg2+ ions or magnesium sulphatecomplexometrically by titrating against EDTA solution using Eriochrome black-T 101Experiment 3.20: Determination of strength of Zn2+ ions or zinc sulphate complexometricallyby titrating it against EDTA using Eriochrome black-T 105Experiment 3.21: Determination of total, temporary and permanent hardness of watercomplexometrically using Eriochrome black-T 108Experiment 3.22: Determination of strength of solution of Ca2+ ions as calcium carbonate(CaCO3) complexometrically by titrating against EDTA using Eriochrome black-T 112Experiment 3.23: Determination of strength of Ca2+ ions present in the given milk sample byEDTA back titration 115Experiment 3.24: Determination of strength of Zn2+ ions complexometrically by titratingagainst EDTA using xylenol orange 118Experiment 3.25: Determination of strength of Al3+ ions by EDTA back titration 120Experiment 3.26: Determination of strength of Mg2+ and Zn2+ ions by titrating against EDTAsolution using Eriochrome black-T and xylenol orange 123Experiment 3.27: Determination of strength of Mg2+ and Al3+ ions in the mixture by titratingagainst EDTA using masking agent 127Experiment 3.28: Determination of strength of Ba2+ ions 131

Precipitation Titrations 134Solubility Product: Basis for Precipitation Titrations 134Common Ion Effect 135Titration Curve for Precipitation Titration 135

Experiment 3.29: Determination of strength of sodium chloride solution using Mohr’smethod 138Experiment 3.30: Determination of strength of silver nitrate solution using Volhard’smethod 140Experiment 3.31: Determination of strength of sodium chloride solution using Fajan’smethod 142

Viva Voce Questions 145

4. GRAVIMETRIC ANALYSIS 148Introduction 148Steps Involved in Gravimetric Analysis 148Know Your Gravimetric Analysis Apparatus 148Precipitation Method in Gravimetric Analysis 150Colloidal Precipitate 151Experimental Section 156

Experiment 4.1: Estimation of Ni(II) ions as dimethylglyoximato nickel(II) complex solutionusing dimethylglyoxime (DMG) gravimetrically 156Experiment 4.2: Estimation of copper as CuSCN gravimetrically 159

Contents xiii

Experiment 4.3: Estimation of iron as iron(III) oxide (Fe2O3) gravimetrically 161Experiment 4.4: Estimation of Al(III) gravimetrically 159


5. PREPARATION OF INORGANIC COMPOUNDS 168Introduction 168

Experiment 5.1: To prepare cuprous chloride from copper (II) sulphate pentahydrate 169Viva Voce Questions 171Experiment 5.2: To prepare manganese(III) phosphate (MnPO4) from manganese(II) sulphate(MnSO4) 171Viva Voce Questions 173Experiment 5.3: To prepare aluminium potassium sulphate 173Viva Voce Questions 175Experiment 5.4: To prepare chrome alum from potassium dichromate 175Viva Voce Questions 176Experiment 5.5: To prepare tetraamine copper (II) sulphate from copper sulphatepentahydrate 176Viva Voce Questions 178Experiment 5.6: To prepare tetraamine carbonato cobalt (III) nitrate complex 179Viva Voce Questions 180Experiment 5.7: To prepare potassium trioxalato ferrate (III) trihydrate complex 180Viva Voce Questions 183Experiment 5.8: To measure conductivity of (a) Tetraamine carbonato cobalt (III) nitrate(b) Tetraaminecopper (II) sulphate (c) Potassium trioxalatoferrate (III) trihydrate and tocompare their conductance with M/1000 solution of NaCl, MgCl2 and LiCl3 183Experiment 5.9: To prepare cis- and trans-potassium diaquadioxalatochromate (III)complexes 185Viva Voce Questions 189Experiment 5.10: To prepare acetylacetonate complex of Cu2+ 189Viva Voce Questions 192Experiment 5.11: To prepare acetylacetonate complexes of Fe3+ from ferric chloride 192Viva Voce Questions 193Experiment 5.12: Preparation of silver nanoparticles (AgNPs) using silver nitrate solutionand their spectroscopic characterization using UV–visible spectrophotometer 193Viva Voce Questions 196Experiment 5.13: Preparation of gold nanoparticles (AuNPs) using citrate reduction methodand their characterization using UV–visible spectroscopy 196Viva Voce Questions 198Experiment 5.14: To prepare gold naoparticles using tea leaves or cinnamon 198Viva Voce Questions 199Experiment 5.15: To synthesize ammine complexes of Ni(II) 199Viva Voce Questions 202Experiment 5.16: Synthesis of copper oxalate hydrate complexes: Kinetic vs thermodynamicfactors 202Viva Voce Questions 205

6. QUALITATIVE ANALYSIS OF IONS 206Introduction 206Basic Principles of Qualitative Inorganic Analysis 207Methods of Qualitative Analysis 209Viva Voce Questions 261

7. CHROMATOGRAPHIC SEPARATION OF IONS 263Introduction 263Types of Chromatography 264Paper Chromatography 266Experimental Section 270Chromatographic separation of metal ions 270

Experiment 7.1(a): To separate and identify Co2+ and Ni2+ ions using ascending paperchromatography (using alizarin as spraying agent) 270Experiment 7.1(b): To separate and identify Co2+ and Ni2+ ions using ascending paper

xiv Practical Inorganic Chemistry

chromatography (using DMG as spraying agent) 272Experiment 7.1(c): To separate and identify Co2+ and Ni2+ ions using ascending paperchromatography (using PAN as spraying agent) 274Experiment 7.2: To separate and identify Co2+, Ni2+, Mn2+ and Zn2+ ions using ascendingpaper chromatography 275Experiment 7.3: To separate and identify Fe3+ and Al3+ ions using ascending paperchromatography 277Experiment 7.4: To separate and identify Fe3+, Al3+ and Cr3+ ions using ascending paperchromatography 279Experiment 7.5(a): To separate and identify Cu2+ and Cd2+ ions using ascending paperchromatography (using ammonium sulphide as spraying agent) 280Experiment 7.5(b): To separate and identify Cu2+ and Cd2+ ions using ascending paperchromatography (using dithiozone as spraying agent) 282

Viva Voce questions 283

8. SPECTROPHOTOMETRIC ANALYSIS 285Introduction 285Basic Principles of Spectrophotometry 285Experimental Section 289

Experiment 8.1: (a) To determine the wavelength of maximum absorption (λmax) (b) To drawthe calibration curve 289Experiment 8.2: (a) To determine the wavelength of maximum absorption (λmax) of thecomplex formed between Fe2+ and 1,10-penanthroline (b) To draw the calibration curve 292Experiment 8.3: To determine composition of the Fe3+–salicylic acid complex by Job’smethod 296Experiment 8.4: Preparation of silver nanoparticles 299Experiment 8.5: Preparation of acetylacetanato complexes of Cu2+ and Fe3+ 299Experiment 8.6: Measurement of 10 Dq for [Ti(H2O)6]3+ by spectrophotometric method 300


9. MISCELLANEOUS EXPERIMENTS 306Experiment 9.1: Estimation of Cu and Ni in Alloy 306Experiment 9.2: Estimation of Cu and Zn in Alloy 307Experiment 9.3: Estimation of Analysis of Cement 308Experiment 9.4: Estimation of Zinc Oxide (Pigment) 309Experiment 9.5: Estimation of Manganese in Steel by Absorption Spectrophotometry 310Experiment 9.6: To Determine pH Value Using pH Meter 313Experiment 9.7: To Determine pH of Soil Sample 315Experiment 9.8: Separation of Cl–, Br– and I– by Ascending Paper Chromatography 316Experiment 9.9: To Estimate Copper (II), Calcium (II) and Chloride Ions 317Viva Voce Questions 318

10. PREPARATION OF INORGANIC REAGENTS 319Introduction 319How to Prepare Reagent Solution? 319General Formula for Calculation of Molar Concentration 320General Formula for Calculation of Volume of Solution Required for Dilution 320Preparation of Inorganic Laboratory Reagents 321Preparation of Dilute Acids and Bases 322Preparation of Side-Bench Reagents 324Preparation of Reagents for Qualitative Analysis 326Preparation of Reagents for Volumetric Analysis 332Preparation of Special Solutions and Reagents 334

Contents xv

xvxv

Syllabi

CORE COURSE(Honours in Chemistry)

SEMESTER I(Credits: Practicals–02)

Practical C–I Lab:(A) Titrimetric Analysis

(i) Calibration and use of apparatus(ii) Preparation of solutions of titrants of

different molarity/normality(B) Acid–Base TitrationsPrinciples of acid–base titrations to be discussed.

(i) Estimation of sodium carbonate usingstandardized HCl.

(ii) Estimation of carbonate and hydroxidepresent together in a mixture.

(iii) Estimation of carbonate and bicarbonatepresent together in a mixture.

(iv) Estimation of free alkali present indifferent soaps/detergents

(C) Oxidation–Reduction TitrimetryPrinciples of oxidation–reduction titrations(electrode potentials) to be discussed.

(i) Estimation of Fe(II) and oxalic acid usingstandardized KMnO4 solution

(ii) Estimation of oxalic acid and sodiumoxalate in a given mixture.

(iii Estimation of Fe(II) with K2Cr2O7 usinginternal indicator (diphenylamine,N-phenylanthranilic acid) and discussionof external indicator.

SEMESTER III(Credits: Practicals-02)

Practical C–V Lab:(A) Iodo / Iodimetric Titrations

(i) Estimation of Cu(II) and K2Cr2O7 usingsodium thiosulphate solution (Iodometri-cally).

(ii) Estimation of antimony in tartar emeticiodimetrically

(B) Complexometric titrations using disodiumsalt of EDTA

(i) Estimation of Mg2+, Zn2+

(ii) Estimation of Ca2+ by substitutionmethod

(C) Inorganic preparations(i) Cuprous Chloride, Cu2Cl2

(ii) Manganese(III) phosphate, MnPO4.H2O(iii) Aluminium potassium sulphate

KAl(SO4)2·12H2O (potash alum) orchrome alum.

SEMESTER IV(Credits: Practicals-02)

Practical C–VIII Lab:Gravimetric Analysis:

i. Estimation of nickel (II) using dimethyl-glyoxime (DMG).

ii. Estimation of copper as CuSCNiii. Estimation of iron as Fe2O3 by precipi-

tating iron as Fe(OH)3.iv. Estimation of Al(III) by precipitating with

oxine and weighing as Al(oxine)3 (alumi-nium oxinate).

Inorganic Preparations:i. Tetraamminecopper (II) sulphate,

[Cu(NH3)4]SO4.H2Oii. Acetylacetonate complexes of Cu2+/Fe3+

iii. Tetraamminecarbonatocobalt (III) nitrateiv. Potassium tri(oxalato)ferrate(III)

Properties of Complexesi. Measurement of 10 Dq by spectrophoto-

metric methodii. Verification of spectrochemical series.

for BSc (Hons and Programme Courses) under Choice-Based Credit System (CBCS) Scheme of Delhi University

xvi Practical Inorganic Chemistry

iii. Synthesis of ammine complexes of Ni(II)and its ligand exchange reactions (e.g.bidentate ligands like acetylacetone,DMG, glycine) by substitution method.

SEMESTER VI(Credits: Practicals–02)

Practical C–XIII Lab:Qualitative semimicro analysis of mixturescontaining 3 anions and 3 cations. Emphasisshould be given to the understanding of thechemistry of different reactions. The followingradicals are suggested:

2– – 2– 2– 2–3 2 3 2 3CO , NO , S , SO , S O , CH3COO–, F–,

Cl–, Br–, I–, – 3– 2– 3–3 3 2 4 4 4NO , BO , C O , PO , NH ,+ K+,

Pb2+, Cu2+, Cd2+, Bi3+, Sn2+, Sb3+, Fe3+, Al3+, Cr3+,Zn2+, Mn2+, Co2+, Ni2+, Ba2+, Sr2+, Ca2+, Mg2+.Mixtures should preferably contain one inter-fering anion, or insoluble component (BaSO4,SrSO4, PbSO4, CaF2 or Al2O3) or combination ofanions e.g. 2–

3CO and 2– –3 2SO , NO and –

3NO , Cl–

and Br–, Cl– and I–, Br– and I–, –3NO and Br–,

–3NO and I–.

Spot tests should be done whenever possible.Principles involved in chromatographic separa-tions. Paper chromatographic separation offollowing metal ions:

i. Ni (II) and Co (II)ii. Cu(II) and Cd(II)

CHEMISTRY DISCIPLINEELECTIVE COURSES

CHEMISTRY–DSE 1: (Credits: Practicals–02)

CHEMISTRY PRACTICAL–DSE LAB:NOVEL INORGANIC SOLIDS

1. Determination of cation exchangemethod.

2. Determination of total difference ofsolids.

3. Synthesis of hydrogel by co-precipitationmethod.

4. Synthesis of silver and gold metalnanoparticles.

CHEMISTRY–DSE: INORGANICMATERIALS OF INDUSTRIAL

IMPORTANCE(Credits: Practicals–02)

PRACTICALS–DSE LAB: INORGANICMATERIALS OF INDUSTRIALIMPORTANCE

1. Determination of free acidity in ammo-nium sulphate fertilizer.

2. Estimation of Calcium in Calcium ammo-nium nitrate fertilizer.

3. Estimation of phosphoric acid in super-phosphate fertilizer.

4. Electroless metallic coatings on ceramicand plastic material.

5. Determination of composition of dolo-mite (by complexometric titration).

6. Analysis of (Cu, Ni); (Cu, Zn) in alloy orsynthetic samples.

7. Analysis of Cement.8. Preparation of pigment (zinc oxide).

Generic Elective Papers (GE)(Minor–Chemistry) (any four) for otherDepartments/Disciplines:(Credits: Practicals–02)

CHEMISTRY LAB:Section A: Inorganic Chemistry–VolumetricAnalysis

1. Estimation of sodium carbonate andsodium hydrogen carbonate present in amixture.

2. Estimation of oxalic acid by titrating itwith KMnO4.

3. Estimation of water of crystallization inMohr’s salt by titrating with KMnO4.

4. Estimation of Fe (II) ions by titrating itwith K2Cr2O7 using internal indicator.

5. Estimation of Cu (II) ions iodometricallyusing Na2S2O3.

CHEMISTRY LAB:Section A: Inorganic ChemistrySemimicro qualitative analysis of mixtures usingH2S or any other scheme not more than four ionicspecies (two anions and two cations andexcluding insoluble salts) out of the following:Cations : 4NH ,+ Pb2+, Bi3+, Cu2+, Fe3+, Al3+, Co2+,Ni2+, Mn2+, Zn2+, Ba2+, Sr2+, Ca2+, K+.

Anions : 2– 2 2– –3 3 3CO , S , SO , NO , CH3COO–, Cl–,

Br–, I–, – 2– 3– 2– 2–3 4 4 3 2 4NO , SO , PO , BO , C O , F–.

(Spot tests should be carried out whereverfeasible)

GENERIC ELECTIVE COURSES(Credits: Practicals–02)

GE LABSection A: Inorganic Chemistry

1. Estimation of the amount of nickelpresent in a given solution as bis(dimethylglyoximato) nickel(II) or alumi-nium as oxinate in a given solutiongravimetrically.

Contents xvii

2. Estimation of (i) Mg2+ or (ii) Zn2+ bycomplexometric titrations using EDTA.

3. Estimation of total hardness of a givensample of water by complexometrictitration.

4. Determination of the composition of theFe3+–salicylic acid complex/Fe2+–phenanthroline complex in solution byJob’s method.

GE LAB(Credits: Practicals–02)

Section A: Inorganic Chemistry1. Separation of mixtures by chromato-

graphy: Measure the Rf value in each case.(Combination of two ions to be given)Paper chromatographic separation ofFe3+, A13+ and Cr3+

orPaper chromatographic separation ofNi2+, Co2+, Mn2+ and Zn2+

2. Preparation of any two of the followingcomplexes and measurement of theirconductivity:

(i) tetraamminecarbonatocobalt (III)nitrate

(ii) tetraamminecopper (II) sulphate(iii) potassium trioxalatoferrate (III)

trihydrate

Compare the conductance of thecomplexes with that of M/1000 solutionof NaCl, MgCl2 and LiCl3.

BSc ProgrammeLife Sciences (Botany, Chemistry, Zoology)

CORE COURSESCore Course–CHEMISTRY I(Credits: Practicals–02)

CHEMISTRY LAB:Section A: Inorganic Chemistry–VolumetricAnalysis

1. Estimation of sodium carbonate andsodium hydrogen carbonate present in amixture.

2. Estimation of oxalic acid by titrating itwith KMnO4.

3. Estimation of water of crystallization inMohr’s salt by titrating with KMnO4.

4. Estimation of Fe (II) ions by titrating itwith K2Cr2O7 using internal indicator.

5. Estimation of Cu (II) ions iodometricallyusing Na2S2O3.

CORE COURSECHEMISTRY IV(Credits: Practicals–02)

CHEMISTRY LAB:Section A: Inorganic Chemistry

Semimicro qualitative analysis of mixtures usingH2S or any other scheme not more than four ionicspecies (two anions and two cations andexcluding insoluble salts) out of the following:

Cations: 4NH ,+ Pb2+, Bi3+, Cu2+, Fe3+, Al3+, Co2+,

Ni2+, Mn2+, Zn2+, Ba2+, Sr2+, Ca2+, K+.

Anions: 2– 2– 2– –3 3 3CO , S , SO , NO , CH3COO–, Cl–,

Br–, I–, – 2– 3– 3– 2–3 4 4 3 2 4NO , SO , PO , BO , C O , F–.

(Spot tests should be carried out whereverfeasible)

DISCIPLINE SPECIFICELECTIVE COURSES

DSE CHEMISTRY 4NOVEL INORGANIC SOLIDS(Credits: Practicals–02)

CHEMISTRY PRACTICAL–DSE LAB:NOVEL INORGANIC SOLIDS

1. Determination of cation exchangemethod

2. Determination of total difference ofsolids.

3. Synthesis of hydrogel by coprecipitationmethod.

4. Synthesis of silver and gold metal nano-particles.

DSE CHEMISTRY 11(Credits: Practicals–02) LAB

Section A: Inorganic Chemistry1. Estimation of the amount of nickel

present in a given solution as bis(dimethylglyoximato) nickel(II) or alumi-nium as oxinate in a given solutiongravimetrically.

2. Estimation of (i) Mg2+ or (ii) Zn2+ bycomplexometric titrations using EDTA.

3. Estimation of total hardness of a givensample of water by complexometrictitration.

4. Determination of the composition of theFe3+–salicylic acid complex/Fe2+–phenanthroline complex in solution byJob’s method.

xviii Practical Inorganic Chemistry

DSE CHEMISTRY 12(Credits: Practicals–02)LABSection A: Inorganic Chemistry

1. Separation of mixtures by chromato-graphy: Measure the Rf value in eachcase.(Combination of two ions to be given)Paper chromatographic separation ofFe3+, A13+ and Cr3+

Paper chromatographic separation ofNi2+, Co2+, Mn2+ and Zn2+

2. Preparation of any two of the followingcomplexes and measurement of theirconductivity:

(i) tetraamminecarbonatocobalt (III)nitrate

(ii) tetraamminecopper (II) sulphate(iii) potassium trioxalatoferrate (III)

trihydrate

Compare the conductance of thecomplexes with that of M/1000 solutionof NaCl, MgCl2 and LiCl3.

practical inorganic chemistry practical inorganic

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