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1

DEPARTMENT OF CHEMISTRY

GITAM INSTITUTE OF SCIENCE

GITAM UNIVERSITY

M.Phil / Pre-Ph.D. Syllabus w.e.f. 2008-09 admitted batch

Paper – I Advanced topics in the board area of concerned discipline (one paper to be

opted)

SRPCH–121/ SRFCH–121: Advanced topics in Inorganic Chemistry

SRPCH–122/ SRFCH–122: Advanced topics in Organic Chemistry

SRPCH–123/ SRFCH–123: Advanced topics in Physical Chemistry

SRPCH–124/ SRFCH–124: Advanced topics in Analytical Chemistry

SRPCH–125/ SRFCH–125: Advanced topics in Environmental Chemistry

Paper- II Research methods and methodology (one paper to be opted)

SRPCH–131/ SRFCH–131: Research methodology – Inorganic Materials

SRPCH–132/ SRFCH–132: Research methodology – Separation techniques and

spectroscopic methods

SRPCH–133/ SRFCH–133: Research methodology – General laboratory techniques and

numerical methods of analysis

SRPCH–134/ SRFCH–134: Research methodology – Modern methods of analysis in

Environmental Analytical Chemistry

SRPCH–135/ SRFCH–135: Research methodology- Chemical Kinetics

SRPCH–136/ SRFCH–136: Research methodology- Modern methods of analysis

SRPCH–137/ SRFCH–137: Research methodology- Extraction techniques

SRPCH–138/ SRFCH–138: Research methodology- Separation techniques

SRPCH–139/ SRFCH–139: Research methodology- Drug analysis

2

GITAM UNIVERSITY (Syllabus for M.Phil / pre-Ph.D degrees, w.e.f. 2008-2009 admitted batch)

SRPCH–121/ SRFCH–121: Advanced Topics in Inorganic Chemistry Inorganic Reaction Mechanisms:

Kinetics of inorganic reactions. Ligand substitution reactions on square-planar complexes,

tetrahedral, five coordinated and octahedral complexes, chelation in square planar

complexes, replacement involving multidentage ligands, substitution in metalloproteins.

Outer-sphere and inner-sphere electron transfer reactions, mixed outer- and inner-sphere

reactions, Two electron transfer reactions, Intermolecular electron transfer reactions,

Induced electron transfer, Electron transfer in proteins.

Bioinorganic Chemistry:

Structure-function relationships of key metalloenzymes; Zinc enzymes – caborxypeptidase

and carbonic enhydrase; Iron enzyme – cytochrome P-450. Copper enzyme – superoxide

dismutase; Molybdenum oxatransferase enzyme – Coenzyme vitamin B12. Therapeutic

compounds, Superoxide dismutage mimics, Vanadium based diabetes durgs, platinum

containing anticancer agents. Diagnostic agents, Technetium Imaging agents, Gadolinium

as Magnetic Resonance Image (MRI) contrasting agent.

Supramolecular Chemistry: Concepts of supramolecular Chemistry, Chemistry of Molecular recognition,

Supramolecular synthesis of organic, metal-organic and inorganic compounds, Guest-host

Chemistry, spherical and tetrahedral recognistion; Molecular self-assembly, self

organisation processes, Supramolecular assembly of Metal ions- Racks, Ladders and Grids.

Metal-organic Framework materials.

Organometallic Chemistry:

General properties of organometallic compounds, bonding in metal atoms and organic π-

systems- Linear π systems, cyclic π systems, fullerene complexes; complexes containing

M-C, M=C and M≡C bonds – alkyl and related complexes, carbine complexes, carbine

complexes; spectral analysis and characterisation of organomettalic complexes.

Books and articles:

1. Kinetics and Mechanism of reactions of Transition metal complexes, R.G.Wilkins,

Wiley-VCH Verlog GmbH Co., 2002.

2. ‘Principles of Bioinorganic Chemistry’, S. J. Lippard, and J. M. Berg,

3. ‘Bioinorganic Chemistry – A short course’ Rosette M. Roat-Malone, John Wiley &

Sons Inc., 2002.

4. Supramolecular Chemistry, Jean-Marie Lehn, VCH

5. Inorganic Chemistry, 3ed, Gary l Miessler & Donald A Torr, Pearson Prentice

Hall, 2004

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3

GITAM UNIVERSITY Pre-Ph.D/M.Phil Examinations

(Chemistry)

Model Paper

SRPCH–121/ SRFCH–121: Advanced Topics in Inorganic Chemistry

Max. Marks: 100 Time: 3hrs

----------------------------------------------------------------------------------------- Answer any FIVE of the following:

(5 X 20 = 100)

1. Describe ligand substitution involving multidentate lignads.

2. Describe mixed outer- and inner sphere electron transfer reactions.

3. Explain structure and function of zinc enzyme carboxypeptidase.

4. Describe platinum containing anticancer agents.

5. Explain the Supramolecular assembly of Metal ions into Racks, Ladders and Grids.

6. Briefly explain Metal-organic framework (MOF) materials.

7. Describe bonding of metal with organic linear π systems and cyclic π systems

8. How the IR spectroscopy helps in characterising organometallic compounds.

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4


SRPCH–122/ SRFCH–122: Advanced Topics in Organic Chemistry

1. Disconnection approach; Basic principles, Chemoselectivity, Stereoselectivity,

Regeoselectivity, Protecting groups – alcohols, carbonyl, carboxylic and amino

groups.

2. Applications of disconnection approach to the synthesis of linear and simple cyclic

compounds - one group C–X (X = hetero atom), C-C disconnections, two groups

C–X and C-C disconnections with reference to 1,1 ;1,2; 1,3; 1,4;1,5

difunctionalised compounds.

3. Transition metal complexes in organic synthesis – Applications of Organo

Palladium compounds, Rhodium complexes, Metal carbonyl complexes of Fe, Co

and Ni.

4. Phase transfer catalysts – Application of phase transfer catalysts in organic

synthesis with reference to Tetraalkylammonium, Tetraalkylphosphonium,

Trialkylsulphonium salts and Crown ethers.

5. Enzyme Chemistry: Introduction to Catalysis, Introduction to Enzymes, Multi

functional catalysis, Enzymes in synthetic organic chemistry, Enzyme analogue

built polymers, Host - Guest Complexation chemistry.

REFERENCE BOOKS:

1. Organic Synthesis: The Disconnection Approach, S.Warren, John Wiley and Sons,

New York, 1984.

2. Advances in Phase Transfer Catalysis.E.V. Dehmlow, Angew,

Chem.Int.ed.Engl.16, 493-505,1977.

3. ‘Two Phase Reactions in Organic Chemistry’ in ‘Survey of Progress in Chemistry’,

Vol.9, Ch.I.Ed.A.F.Scott, Academic Press, New York, 1980.

4. ‘Host – Guest Complex Chemistry III’ in ‘Topics in Current Chemistry 121’, Eds.

F.Vogtle and E. Weber, Springer – Verlag, New York 1984.

5. Organic named reactions by Jai Jack lie – Springer Verlog

6. Advanced organic chemistry part A and Part B by F.A. Carey and R.J. Sunderg,

Springer

7. Some modern methods of organic synthesis by W. Carruthers, Cambridge

University press edition

8. Organic synthesis by Dr. Jagadamba Singh and Dr. L.D. S. Yadav : Pragati

Prakasan, Meerut.

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5


(Chemistry)

Model Paper

SRPCH–122/ SRFCH–122: Advanced Topics in Organic Chemistry



(5 X 20 = 100)

1. What are the basic principles of the disconnection approach and how it is

relevant to the synthesis of linear and simple cyclic compounds

2. Write a short note on the following.

a) Regioselectivity b) Protecting groups c) Stereoselectivity

d) Chemoselectivity

3. Describe the role of Enzymes as reagents and catalysts in organic synthesis

4. Write a short note on the following

a) Enzyme analogue built polymers, b) Host-Guest Complexation chemistry

5. Write any two applications of Organo Palladium compounds and Rhodium

complexes in organic synthesis

6. Write a detailed note on Phase transfer catalysts and Crown ethers

7. Discuss the applications for the following

a) Tetraalkylammonium salt b) Tetraalkylphosphonium salt

c) Trialkylsulphonium salt

8. Discuss the two group C–C disconnections of 1,5 and 1,3 difunctionalised

compounds with suitable examples.

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6


SRPCH–123/ SRFCH–123: Advanced Topics in Physical Chemistry

1. Fundamental Principles of Irreversible Thermodynamics – Open Systems – Evolution of

Criteria of Conservation Mass of energy – compared to closed systems – Entropy flow

of open systems – Microscopic reversibility and Onsagar relations

2. Elements of Statistical Mechanics, Micro and Macro States – Classical distribution Law

– Quantum Statistics – Bose – Einstein, Fermi – Dirac Statistics – Conditions for the

applicability of Maxwell – Boltzman Statistics – Fermi Energy of Metals, Free electron

models (Electron gas concept) – Electronic heat capacity of metals – Fermi Energy

levels – Super conductivity and various theories of super conductivity – Negative

absolute temperature – Evaluation of partition functions – translational, rotational,

vibrational, electronic and nuclear partition functions – statistical evolution of

thermodynamic function – energy – Heat capacity – Entropy – free energy.

3. Electrode polarization – Decomposition potential and overvoltage – Theories of over –

voltage. Polarography: basic principle – Polarogram (Description) Dropping Mercury

electrode – Diffusion current – half wave potential and its significance – 11kovic

Equation – Concentration over potential – Fick’s 1st Law of Diffusion – Thickness of

diffusion layer – Applications of Polarography.

4. Corrosion : Theories of Dry and Wet Corrosion - Types of Corrosion – Protection

against Corrosion – different methods.

5. Complex Reactions – Consecutive, parallel and opposing reactions – Equilibrium and

steady State technique, chain reactions – Mechanism and rate law of H2 – Br2 and H2

– Cl2 reactions – Flow and relaxation technique for the fast reactions.

TEXT BOOKS :

1. Physical Chemistry by Vojtech, Fries, Bulkin, etc.

2. Molecular thermodynamics by Dickerson

3. Thermodynamics for Chemists – S. Glasstone

4. Introduction to Chemical Thermodynamics by Davies.

5. An Introduction to Electrochemistry by S.GLASSTONE

6. Chemical Kineting by K.J.Laidler.

7. Corrosion Engineering by Fontenna & Green.

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7


(Chemistry)

Model Paper

SRPCH–123/ SRFCH–123: Advanced Topics in Physical Chemistry



(5 X 20 = 100)

1. Write notes on

a) Microscopic reversibility

b) Entropy flow in open systems

2. Define partition functions. Describe expressions for translational, rotational,

vibrational and electronic partition functions and discuss their significance.

3. Define over voltage. Describe the theories of over voltage

4. What is meant by corrosion? Explain the theories of dry corrosion.

5. Define chain reactions derive rate law for the reaction between H2 – Cl2 reactions

6. Write the main differences between Maxwell-Belizeans, Bose-extruded and Ferin

Dirac statistics

7. Explain Fick’s 1st law of diffusion. Explain a method to determine thickness of

diffusion layer.

8. Describe the superconductivity and explain various theories of super conductivity.

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8


SRPCH–124/ SRFCH–124: Advanced Topics in Analytical Chemistry

Quality control in analytical chemistry:

Characteristics of an analysis: Classification of errors, accuracy-absolute and comparative

method, precision, significant figures, mean and standard deviation,Q-test,T-test and F-test.

Quality of an analytical procedure, limit of detection, sensitivity, safety, cost measurability.

Selectivity and specificity, quality control-principles of Ruggedness, control chart, method

validation, calibration curve.

Quality assurance and GLP:

Quality assurance and management systems: Elements of quality assurance, quality

assurance in quality and quality management system,, quality process model, statistical

process control, process control tools, statistical quality control, acceptance sampling.

Good laboratory practice (GLP) - need for GLP, GLP implementation and organization..

Chromatography: Classification of different chromatographic methods, Principles of chromatography, different migration, adsorption phenomena, partition, adsorption and partition coefficient, adsorption and partition isotherms, retardation factor, retention time and retention volume. Column capacity Planar chromatography: Paper chromatography: Principle, experimental technique, different development methods-ascending, descending, horizontal, circular spreading, multiple development, two dimensional development, visualization and evaluation of chromatograms, applications.

Thin layer chromatography: Principle,,activation of adsorbent, development of chromatoplate, visualization methods, applications.

Titrametric Methods:

Complexation Titrations: stability of complexes, factors influencing the stability of

complexes, Chelates; EDTA, types of EDTA titration curves, masking and de-masking

agents. Detection of end point –metal ion indicators

Precipitation Titrations: Law of mass action solubility product ionic product, Principle,

Indicators for precipitation titrations, determination of silver in an alloy (Volhard method),

Determination of chloride in soluble chloride (Fajans method) and determination of

chlorides using Mohr’s method

Redox and Potentiometric Titrations: Basic concept of electro chemistry: electro chemical

cells, The Nernst Equation, Formal Potential, Feasibility of Redox titrations, Redox

indicators, Potentiometric Titrations

Solvent Extraction: Principles and processes of solvent extraction, Distribution Law, Partition coefficient ,distribution ratio, nature of partition forces, factors favouring solvent extraction, different type of solvent extraction systems - Batch extraction. Continuous extraction, Counter current extraction, solvent extraction of metals-ion association complexes and metal Chelates, supercritical fluid extraction, soxlet extraction. Basic principle of solid phase extraction

9

Textbooks:

1. Quantitative Analysis, R.A.Day & A.L.Underwood, Prentice -Hall of India,1991 2. Chemical analysis - H.A. Laitinan, McGraw Hill Book Co.,1975 3. D.A. Skogg, D.M. West and F.J. Holler, Analytical Chemistry, An Introduction,

Sanders College Publishing, New York,2004 4. Analytical Chemistry Gary D Christian, John Wiley and Sons inc,2003. 5. Volumetric Analysis, Vol. III -I. M. Kolthoff and R. Welcher, Interscience Public, New

York,1969 6. Vogel's textbook of Inorganic Quantitative Analysis - J. Bassett et al. ELBS ,2005 7. Quality Assurance and Quality Management in Pharmaceutical Industry, Prof. Y.

Anjaneyulu, R.Marayya ,Pharma Book syndicate,2002. 8. Separation methods , J.A.Dean

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10


(Chemistry)

Model Paper

SRPCH–124/ SRFCH–124: Advanced Topics in Analytical Chemistry



(5 X 20 = 100)

1. What are the factors influencing the characteristic of analysis

2. Write about student T-test and Q-test and their significance.

3. a) Write about application of Complex metric Titrations.

b) What are the factors influencing the stability of complexes.

4. What are Precipitation Titration and determine chloride in a sample using Volhard

Method.

5. What is formal potential. Explain the various factors affecting formal potential

6. Explain the basic principle of solvent extraction. Discuss the various methods of

solvent extraction.

7. Write about a) Retention time

b) Retardation factor and Retention volume.

8. a) Write about quality assurance and quality management system

b) GLP.

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11


SRPCH–125/ SRFCH–125: Advanced topics in Environmental Chemistry Air Pollution: Composition of Atmosphere, Air quality standards, Types of air pollution,

Effect of air Pollutants on man & environment, Chemical & Photochemical reactions in

atmosphere; Ozone chemistry, Nitrogen oxides, Sulphur Dioxide, PAN sampling of air,

Analysis of The following pollutants: Carbon monoxide, Oxides of nitrogen, Oxides of

Sulphur, Particulate matter, Analysis of hydrogen sulphide and analysis of hydro carbons.

Water Pollution: Water Physical and chemical properties, Water pollution; Sources,

Eutrophication and Water and quality standards. Types of Pollutants, Sampling and

preservation of water and waste water, Analysis of the following in the Drinking water;

Hardness, Alkalinity, DO, BOD, COD, Chlorides ammonia, Nitrate and Nitrite, Sulphate;

Phosphate, Metals like – Fe2+, Mn2+ ,Pb2+ , Ni2+ and Cr(VI) and Organics – Phenol.

Thermal pollution: important sources of surplus heat, damages caused by heat discharges

on aquatic life, Ecological effects of heated waters on aquatic system and control of

thermal pollution.

Radio active Pollutants: Radioactivity and radiations, Damages caused to a biological

system by radiation, sources of radiation on environment, hazards associated with radio

active pollution, Global accumulation of nuclear waste, types of nuclear waste and

Disposal of Radio active waste.

Soil Pollution: Composition of soil, Inorganic and Organic components in soil, Micro and

Macro Nutrients in soil, Sources of soil pollution, Pollutants in soil, Sampling of soil,

Analysis of soil – C.E.C, Organic carbon, Chlorides and alkali and alkaline earth metals

like Na +, K+ and Ca2+.

Chemical Toxiology: Bio chemical effects of the following, Calcium , Lead, Mercury,

Arsenic, Cyanide, Pesticides, Carbon monoxide, Nitrogen oxide and Sulphur dioxide.

Books:

1. Environmental Chemistry – S.K. Banerjee.

2. Environmental Chemistry – O.P. Tyagi

3. Environmental pollution control engineering – S.P. Mahajan.

4. A Text book of Environmental chemistry and pollution control by S.S. Dara.

5. Principles of Instrumental analysis – Skoog, West and Nieman.

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12


(Chemistry)

Model Paper

SRPCH–125/ SRFCH–125: Advanced Topics in Environmental Chemistry



(5 X 20 = 100)

1. Describe the structure of atmosphere. What are air quality standards? Write a note

on the Classification of air pollutants. Discuss the photochemistry of ozone in the

atmosphere.

2. What is Biological oxygen demand? Differentiate between biological oxygen

demand and Chemical oxygen demand. Describe modified Wink levis method for

the determination of dissolved oxygen in water.

3. Write a note on thermal pollution, its effect on aquatic life and control of thermal

pollution.

4. Write a note on Radio active pollution, types of radioactive waste, hazards

associated with radio active pollution and disposal of radio active waste.

5. Describe the methods of sampling of soil. Explain the various types of Nutrients in

soil. What are the sources of soil pollution

6. Write short notes on the determination of the following in soil.

a) Organic carbon b) Calion exchange capacity

c) Chlorides d) Alkali metal with reference to Na+ & K+

7. Write the biochemical effect of Cadmium & Mercury

8. Write a note on the biochemical effects of CN- and Pb2+.

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13


SRPCH–131/ SRFCH–131: Research Methodology - Inorganic Materials

Research Methods:

Meaning of Research, Objectives and importance of Research, Types of Research – basic

and applied, Research Methods versus Methodology, Selection of research topic and

problem, Literature survey, Reference collection, Research design, Investigation of

problem, Art of writing a research paper and thesis, Outlines of research report, Layout of a

research report.

Biomaterials & Nanomaterials:

Introduction to Inorganic structures of Life, Polymorphs of calcium carbonate- calcite,

aragonite, vaterite; Mollusk shell formation. Calcium phosphate – bone and teeth;

biominerasls - silica, iron oxides. Introduction to quantum dots, nanoparticles, nanowires

and nanotubes. Carbon nanotubes. Magnetic nanoparticles for Magnetic Resonance

Imaging (MRI) and drug delivery; Molecular Nanostructures – Single-Molecule Magnets

(SMM).

Synthesis of Inorganic Materials:

Synthesis of solid state materials using ceramic and carbothermal reduction methods.

Synthesis of solids from gas phase using chemical vapour deposition (CVD) technique.

Hydrothermal synthesis for preparation of solids from solution. Sol-gel processing of

silicate materials. Preparation of Nanoparticles and Nanocrystalline materials.

Characterisation of Inorganic Materials:

X-ray diffraction (XRD)

Introduction to crystal systems, Basic components of an X-ray diffractometer, The powder

technique - Debye-Scherer method, application and interpretation of Powder X-ray

diffraction data, Collection of crystallographic data and major programs involved in the

analysis of single crystal structure. Flow chart of SHELXTL program for typical X-ray

structure solution. Electron Microscopy

Characterisation of materials using Scanning Electron Microscopy (SEM), Transmission

Electron Microscopy (TEM), Scanning Probe Microscopy (SPM), Atomic Force

Microscopy (AFM).

Books and articles:

1. Research Methodology, S. Rajasekar, Bharathidasan University, Tamilnadu, India

2. Biomineraliszation: Principles and concepts in Bioinorganic Materials Chemistry’

Stephen Mann, 2001, Oxford University Press.

3. Nanochemistry: A chemical approach to Nanomaterials, Ozin Geoffrey A.

4. Review article ‘Soft chemical approaches to inorganic nanostructures’ C.N.R. Rao

et. al., Pure Appl. Chem., 2006, 78, 1619-1650.

5. Synthesis of Inorganic materials, Ulrich Schubert & Nicola Hüsing, Wiley-VCH,

2000.

6. Review articles from reputed National and International Journals.

14


(Chemistry)

Model Paper

SRPCH–131/ SRFCH–131: Research Methodology - Inorganic Materials



(5 X 20 = 100)

1. Describe the writing procedure of a research paper and thesis.

2. Write short notes on the following research methods:

a) Selection of Research topic

b) Literature survey

3. Describe biomineralization of calcium phosphate in bone and teeth.

4. Explain the application of magnetic nanoparticles as Magentic Resonance Imaging

(MRI) contrast agents.

5. Describe Chemical Vapour Deposition (CVD) method for synthesis of materials.

6. Explain sol-gel processing of silicate materials.

7. Describe the interpretation of powder X-ray diffraction data.

8. Describe the morphology of CaCO3 crystals using Scanning Electronic microscopic

(SEM).

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15


SRPCH–132/ SRFCH–132: Research Methodology – Separation Techniques and

Spectroscopic Methods

1. Research Methods: Meaning of Research, Objectives and importance of Research,

Types of Research – basic and applied, Research Methods versus Methodology,

Selection of research topic and problem, Literature survey, Research design,

Investigation of problem, Art of writing a research paper and thesis, Outlines of

research report, Layout of a research report.

2. Extraction procedures of Natural products, Applications of TLC, Adsorption

chromatography, Flash chromatography, GLC, HPLC techniques for the isolation and

separation of organic compounds.

3. 1H, 13C NMR, Pulse Fourier transform techniques, double resonance, relaxation

mechanisms and applications.

4. Applications of 2D NMR Spectra and correlated 2D NMR Spectra.

5. Applications of U.V, I.R. and Mass Spectroscopy, chemical ionization, FAB, field

ionization and field Desorption techniques.

Reference Books:

1. Research Methodology, S. Rajasekar, Bharathidasan University, Tamilnadu,

India

2. Elucidation of Organic Structures by Physical and Chemical Methods. Eds.K.W.

Bentley and G.W. Kirby, Vol.IV, Part I, Wiley Interscience, New York, 1972

3. Instrumental Methods of Chemical Analysis. B.K.Sharma, Goel Publishing

House, Meerut (UP), 1986-87

4. Spectrometric Identification of Organic Compounds.R.M.Silverstein, G.C.

Bassler and T.C.Morrill, IVth Edition. John Wiley and Sons, New York, 1981.

5. Research Methodology, S. Rajasekar, Bharathidasan University, Tamilnadu,

India

6. The Organic Chem. Lab survival manual, A student’s guide to techniques by

James.W. Zubrick: John Wiley & Sons.

7. Spectroscopic methods in organic chemistry Vth edition by Dudley.H.Williams

and Ian Fleming; Tata McGraw-Hill.

8. Introduction to spectroscopy by Donald.L.Pavia, Gary M Lampman and George

S. Kriz ;Thomson Publication.

9. Organic spectroscopy by William Kemp; ELBS

10. Organic spectroscopy by Jag Mohan ; Narosa Publications

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16


(Chemistry)

Model Paper

SRPCH–132/ SRFCH–132: Research Methodology – Separation Techniques and

Spectroscopic Methods



(5 X 20 = 100)


2. Write the principles and various applications of HPLC techniques.

3. a) Write a note on Fingerprint region and functional group region in IR

Spectroscopy.

b) Write a short note on the following

i) FT NMR ii) Double resonance technique in NMR

4. Discuss the application of IR spectra for the identification of

a) Ester group b) Cyanide group c) Hydroxyl group d) Carbonyl group

5. An organic compound ‘A’ exhibits only a singlet at δ2.17 in the ‘H NMR and

prominent peaks at m/z 58 [m+],43 (base peak),39,27 and 15 in the mass spectrum.

When the compound ‘A’ is treated with benzaldehyde and dil. Ethanolic Sodium

Hydroxide, it yields ‘B’. The IR spectrum of ‘B’ exhibits bands at 3025, 1665,

1630,1600,1495,763 and 705 cm-1. The 1H NMR spectrum of ‘B’ displays

δ7.82(d,j18,1H), δ7.6(m,5H), δ7.05(d,j18 1H) Deduce the structures of ‘A’ and ‘B’

6. Discuss the theory of C13 NMR spectroscopy and its applications with suitable

examples.

7. Write a short note on COSY and HETCOR technique in NMR spectroscopy

8. a) The mass spectrum of ethyl benzene represented as :

m/e (RA) : 65, 91 (100%), 105, 106.What do the term m/e convey?

What is the molecular ion for this compound? What are the possible structures

for the ion located at m/e 91

b) Write the fragmentation pattern for benzyl alcohol and p-nitro acetophenone

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17


SRPCH–133/ SRFCH–133: Research Methodology - General Laboratory

Techniques and Numerical methods of Analysis

1. Handling and Safety in Chemical Laboratory : Classification of Hazardous

materials; Safety aspects in the Design of chemical laboratory; Safe Handling of

Glassware; Safety in storage and Handling of Materials, Precautions for Especially

Hazardous Laboratory Operations; Emergency Procedures.

2. Basic Laboratory Practices : Basic Laboratory operations – Handling, Purification,

usage and recycling of solvents, storage of Hazardous chemicals.

Sampling – Sampling techniques, solid sampling, liquid sampling and gas

sampling.

3 Calibration & Validation: Room and Equipment Validation: Importance and

process of room and equipment validation. Process Validation: Importance, type of

process validation, validation of dissolution, mixing, granulation, tablet

compression, tablet coating, capsule filling, injection vial filling process. Analytical

Method Validation: Importance, specificity, limit of detection, limit of

quantification, linearity, precision, accuracy, robustness and system suitability.

4. Data Handling: Accuracy and Precision, significant figures, Determinate and

Indeterminate errors, ways of expressing Accuracy – Absolute and Relative errors,

Propagation of Errors, Control charts, the confidence limit, Tests of Significance –

The F-test, the student T-test, Rejection of a result – the Q-test. Measures of

Dispersion – Range, Arithmetic mean, Mean Deviation, Variance and Standard

deviation.

5. Numerical methods : Linear least – Squares - the correlation coefficient,

Interpolation – Linear and non-linear interpolation – Lagrange interpolation formula

– application to problems in chemistry, Solution of ordinary first order differential

equations – Euilers method – Predict and correct method, - Rungae – Kutta method

– Application to problems in chemistry

Books:

1. Quantitative Analysis, R.A.Day & A.L.Underwood, Prentice -Hall of India,1991

2. Vogel's textbook of Inorganic Quantitative Analysis - J. Bassett et al. ELBS

,2005

3. Quality Assurance and Quality Management in Pharmaceutical Industry,

Prof. Y. Anjaneyulu, R.Marayya ,Pharma Book syndicate,2002

4. Analytical Chemistry - G.D. Christian

18


(Chemistry)

Model Paper

SRPCH–133/ SRFCH–133: Research Methodology - General Laboratory

Techniques and Numerical methods of Analysis



(5 X 20 = 100)

1. Explain the terms Precision and Accuracy. Describe various factors that quantify

the precision and accuracy of analytical determinations.

2. What are determinate and indeterminate errors? Explain their origin taking suitable

examples. How are these errors propagated in arithmetical computations?

3. a) What is interpolation ? Derive Lagrange interpolation formula and explain its

application in chemistry.

4. What are ordinary first order differential equations? Explain indetail the Euler’s

and Predict-Correct method of solving ordinary first order differential equations.

What is its application in chemistry?

5. Explain different sampling techniques for liquids and gases.

6. Discuss the importance and process of room and equipment validation.

7. Write note on Analytical method validation .

8. Write notes on:

a) Classification of Hazardous materials

b) Safety in storage and handling of materials

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19


SRPCH–134/ SRFCH–134: Research Methodology – Modern Methods of Analysis

In


Research Methods: Meaning of Research, Objectives and importance of Research, Types of

Research – basic and applied, Research Methods versus Methodology, Selection of

research topic and problem, Literature survey, Reference collection, Research design,

Investigation of problem, Art of writing a research paper and thesis, Outlines of research

report, Layout of a research report.

Sampling and sample preparation in chemical analysis, Aims of sampling, Stratified and

random sampling, Statistical criterion of good sampling, Sampling of solids and liquids

with particular reference to soils, Sediment and waste water. Statistics in chemical analysis:

Mean deviation, Standard Deviation, Co-efficient of variance, Normal distribution, F Test

and T Test .Method Development and Validation: Accuracy, Precision, Detection limit and

Calibration curves.

Pollutants: their sources, Degradation and fate in the environment:

(a) Organophosphate and Organochlorine pesticides: DDT, BHC, Parathion and Malathion.

(b) Surfactants

(c) Fertilizers

(d) Xenobiotics

(e) Phenols

Instrumental techniques in chemical analysis: Principle and instrumentation of the

following:

Ions elective electrodes: types and working, U.V and Visible spectroscopy, Flame

absorption and Flame emission Spectroscopy, Atomic absorption spectroscopy, XRF, IR

and thermal methods: TGA, DTA and DSC

Fundamental idea of Hyphenated Techniques: Theory and instrumentation of LC-MS, GC

–MS and ICP-MS

Books :


2. Principles of Instrumental analysis – Skoog, West and Nieman.

3. Analytical Chemistry - G.D. Christian

4. Environmental Chemistry – S.K. Banerjee.

5. Environmental Chemistry – O.P. Tyagi

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20


(Chemistry)

Model paper


In




(5 X 20 = 100)

1. What is the importance of the following:

i. Research and its objectives ii. Research Methodology

2. Write in brief about

i. Outlines of research report ii. Research Design

3. What is method development and method validation in chemical analysis?

Discuss the various methods of preparation of calibration curves.

4. Discuss the various method of sampling of water and waste water. Write in short

on the preservation of water and waste water samples.

5. Write the degradation path way and fate of the following pollutants in the

Environment

Xylene

Phenols

6. Write the degradation and fate of the following pollutants in the environment:

DDT

Organophosphorus pesticides with reference to Parathion and Malathion.

7. Explain the theory and instrumentation of GC-MS

8. Discuss the various types of interferences of Atomic absorption spectroscopy.

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21


SRPCH–135/ SRFCH–135: Research Methodology - Chemical Kinetics

1. Analysis of Kinetic Data : Calculation of rate constant from concentration methods

when the final value is unknown-propagation of errors – linear least squares regression

– non-linear least squares regressions.

2. Accuracy in rate constant measurements; Measurements of rates – Simplification of

experimental kinetics – kinetic scheme: Model Building – Kinetic Equivalence of rate

terms – Microscopic reversibility and detailed balance.

3. Marcus Theory – Tests for Marcus – Harsh Theory – Single potential Energy surfaces –

Exchange reaction Atom transfer reactions – One and two electron transfer reactions.

Inner and outer sphere mechanisms – extended bridge hypothesis – Bridges

intermediates.

4. Explanation of rates through transfer free energies of reactions and transition state –

Effect of dielectric constant – ion – ion, ion – molecule. Molecule – Molecule reactions

– Weinstein equation – Edward Equation – Swain – Scott Equation.

5. Correlation of rates with Ho, HR acidity functions Mechanism of acid – base catalysis –

Catalysis by transition metal ions and their complexes.

REFERNCE BOOKS:

1. Chemical Kinetics – The study of Reaction Rates in solution by Kenneth A. Connors

(V.Ch.Publishers),

2. Physical Organic Chemistry of Weiberg.

3. Chemical Kinetics by K.J. Laidler.

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22


(Chemistry)

Model Paper

SRPCH–135/ SRFCH–135: Research Methodology - Chemical Kinetics



(5 X 20 = 100)

1. Explain the importance of linear least square and non-linear square regression in

the analysis of kinetic data. Add a note on propagation of errors

2. What does model building mean? Describe microscopic reversibility and detailed

balance in the study of kinetic rate.

3. Giving suitable examples, explain Marcus theory reactions.

4. Write a note on the extended bridge and intermediate bridge hypotheses.

5. Write notes on:

a) Accuracy in rate constant measurements

b) Inner and Outer sphere mechanisms

6. Give in detail the explanation of rates through transfer free energies of reactions

and transition state.

7. Describe the mechanism of acid-base catalysis. Comment on the catalysis by

Transition metal and their complexes .

8. Write notes on:

a) Edward Equation

b) Weinstein equation

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23



Research Methods:





research report.

Spectroscopic Methods: NMR Spectroscopy, Resonance, Origin of Spectra, Chemical

shift, Factors affecting chemical shift, Shielding, Spin-spin splitting, Instrumentation,

Interpretation of NMR Spectra of Organic compounds, Applications.

(a) . X-ray diffraction (XRD)

Introduction to crystal systems, Debye-Scherer method, Powder X-ray diffraction,

determination of single crystal structure (cubic system only)..

(b) Thermal methods :

Differential thermal analysis-principle, instrumentation, difference between TG and DTA,

applications with reference to the clays and minerals.

Hyphenated Techniques: Theory, instrumentation and applications of LC-MS, GC –MS

with special reference to drug analysis..

Polarographic Analysis: Principle of polarography residual current, migration current,

diffusion current, half-wave potential, Ilkovic equation, instrumentation, dropping mercury

electrode (DME), advantages and disadvantages of DME, qualitative and quantitative

analysis of inorganic ions - Cu, Pb Cd, Zn,.anodic stripping Voltametry and its

applications.

Books and articles:


2. ‘Instrumental Methods of Analysis’ Hobart H. Lynne, L. Willard, Merit Jr. and

John A Dean.

3. ‘Vogel Text Book of Quantitative Chemical Analysis’ J. Mendham, RC Denney,

JD Barnes and MJK Thomas, Pearson Education.

4. Principles of Instrumental Analysis’ Skoog and West.

5. Instrumental methods of chemical analysis – B.K. Sharma, Goel Publishing house,

Meerut

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24


(Chemistry)

Model Paper

SRPCH–136/ SRFCH–136: Research Methodology - Modern Methods of

Analysis



(5 X 20 = 100)

1. What is the importance of

i. Research and its objectives ii. Research Methodology

2. Write in brief about

i. Outlines of research report ii. Research Design

3. Write about

i) TGA and DTA

ii) Factors effecting chemical shift in NMR

iii)Applications of GC

4. Explain the basic Principle and Instrumentation of NMR Spectroscopy.

5. Explain the basic principle of XRD and write about Powdered X-ray diffraction

method

6. Explain the theory and instrumentation of Gas Chromatography

7. Explain the Principle involved in LC-MS and mention its applications. in drug

analysis.

8. What are the factors influencing Polarogram and its applications in trace metal

estimations..

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25


SRPCH–137/ SRFCH–137: Research Methodology - Extraction Techniques






Principles of solvent extraction:Distribution ratio relationship between distribution metal

ion between aqueous and organic layers – percentage extraction – batch extraction –

continuous extraction. Factors playing role in extraction efficiency – change in acid, metal,

extractant concentrations, diluent effect and kinetic factors, synergism and antagonism.

Different extraction mechanism systems – extraction by solvation – extraction by

compound formation – extraction by ion – extraction.

Solid phase extraction :

Principle matrix solid phase dispersion, special SPE phases, Solid phase micro – extraction

(SPME) and stir – bar sorbent extraction (SBSE)

Literature survey on different extraction systems, special extraction systems.

Extraction efficiency of tri – n octyl phosphine oxide (TOPO) and di-2 (ethyl hexyl)

Phosphoric acid (HDEHP).

Ion exchange: Introduction to ion exchange resins. Principles of ion exchange mechanism –

simple systems, separation of inorganic mixtures. Application – separation of lanthanides.

Super fluid Critical extraction :

Principle development of spent fuel reprocessing by super critical fluid extraction – Dye

extraction from fibre by super fluid critical extraction – Design of super – critical fluid

extraction apparatus.

Text Books:

1) Research Methodology, S. Rajasekar, Bharathidasan University, Tamilnadu, India

2) A.I. Vogel, A text book of quantitative analysis.

3) M.N.Sastry, Separation techniques – Himalaya publications.

4) B.K.Sarma, instrumental methods of chemical analysis.

5) Chatwal & Anand, instrumental methods of chemical analysis.

6) Solid phase extraction, E.M. Thurman, M.S. Mills, Wiley publications.

7) Solid phase extraction, Principle, techniques and applications.

8) Super fluid critical extraction, M.B. King, T.R. Bott.

9) Chemical Engineering at super critical Fluid conditions, M.E Paulaitis, Ann Arbor,

Science Publications.

26


(Chemistry)

Model Paper

SRPCH–137/ SRFCH–137: Research Methodology - Extraction Techniques



(5 X 20 = 100)


2. a) What is solid phase extraction explain with examples.

b) Explain the following terms.

i) Solid phase micro extraction ii) Stir bar Sorbent extraction

3. Describe the importance of literature survey in solvent extraction field.

4. Write a detailed account on extraction efficiency of tri – n, octyl phosphine

oxide. (TOPO)

5. a) Describe the principle of ion exchange with suitable examples.

b) Explain the separation of lanthanides using ion exchange.

6. a) Write in detail the ion exchange mechanism of a suitable reaction.

b) Describe the separation of mixtures using ion exchange principle.

7. a) What is super fluid critical extraction?

b) What are the development of spent fuel re-processing by super critical fluid

extraction.

8. a) What is dye extraction?

b) Describe the design of super critical fluid extraction apparatus.

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27


SRPCH–138/ SRFCH–138: Research Methodology – Separation Techniques

Research Methods:





research report.

Chromatography

Classification of chromatographic process

Adsorption chromatography – Theoretical

Basis of separation by adsorption

Column chromatography – applications of column adsorption chromatography

Absorbents and solvents.

Calibration & Validation

High performance liquid chromatography and gas chromatography Theory, Instrumentation

– merits – Demerits Applications of HPCL, GC.

Room and Equipment Validation: Importance and process of room and equipment

validation. Process Validation: Importance, type of process validation, validation of

dissolution, mixing, granulation, tablet compression, tablet coating, capsule filling,

injection vial filling process.

Analytical Method Validation: Importance, specificity, limit of detection, limit of

quantification, linearity, precision, accuracy, robustness and system suitability.

Mass spectrometry

Principle – theory Instrumentation – Interpretation of spectra of metal compounds –

identification of compounds of metal compounds from fragmentation pattern advantages of

mass spectrometry.

Studies on pesticide determination – organophosphorous pesticides (manocrohophos,

vamidothion, acephate etc.,) pesticides in vegetables and fruits – determination of

pesticides using LC.MS.

Sampling Techniques and Introduction to statistics

Sampling of gases, liquids and solids

Standard deviation – coefficient of variation

Precision and accuracy – T - test F – test for significance.

Suggested books:


2. MN Sastry – Separation Techniques – Himalaya publications

3. A.I. Vogel. A text book of quantitative analysis – ELBS.

28


(Chemistry)

Model Paper

SRPCH–138/ SRFCH–138: Research Methodology – Separation Techniques



(5 X 20 = 100)


2. Write short notes on

i) Adsorption chromatography

ii) Application of column adsorption chromatography.

3. a) Compare HPCL and GC.

b) Explain briefly the demerits of HPLC.

4. a) Explain the basic principle involved in mass spectrometry.

b) What are the disadvantages of mass spectrometry?

5. a) Explain the interpretation of spectra of metal compounds with reference to mass

spectrometry.

b) What are the advantages of mass spectrometry?

6. a) What are the organ phosphorus pesticides?

b) Write the standard method of determination of monocrotophos pesticide in

vegetable.

7. a) Explain briefly the sampling of gases and liquids.

b) Write briefly the importance of statistical treatment.

c) Write notes on F-test.

8. Write notes on i) Standard deviation ii) T-test iii) Coefficient of variation

iv) Sampling of solids.

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29


SRPCH–139/ SRFCH–139– Research methodology- Drug analysis






Introduction to chemical instrumental analysis:

a) Spectral methods of analysis

b) Chromatographic analysis

c) Titremetric analysis

d) Elemental analysis

Control of the quality of the analytical methods:

a) Introduction, control of errors in analysis, validation of analytical procedures

(Precision, repeatability, intermediate precision, reproducibility, accuracy). Standard

operating procedure for assay of by taking paracetamol as example.

b) Other terms used in reporting of results and control of analytical procedures (system

suitability, analytical blank, calibration, limit of detection, limit of quantification,

linearity, range, robustness, selectivity and sensitivity.

Analytical profiles of the following official durgs including its structural elucidation:

Antipyretic and Analgesics (NSAID): Aspirin, Paracetomol

Antibiotics: Glutamycin, Quinine

Anticancer drugs: Methotrexite, Cyclophosphamide

Antihypertension drugs: Enalapril

Antidiabetic drugs: Gilbenclamide, Metformin

Antiasthmatic drugs: Theophylline, Caffeine.

Application of NMR, Mass, FT-IR, UV-Visible, HPTLC, HPLC, GC, LC-MS, GC-MS in

drug analysis.

Books:


2. Pharmaceutical Analysis by Watson

3. Fundamentals of Analytical Chemistry, Skoog, West, Holler and Crouch

4. A text book of Pharmaceutical Analysis by Kennath A. Connors.

5. Pharmaceutical Analysis by Takeru Higuchi

6. Introduction of Instrumental Analysis by Robert D. Braun.

7. Indian Pharmacopoeia

8. British Pharmacopoeia

30

**********


(Chemistry)

Model Paper

SRPCH–139/ SRFCH–139– Research methodology- Drug analysis



(5 X 20 = 100)


2. Explain the principle of NMR spectroscopy.

3. Describe the methods involved in the quality control of drugs.

4. Explain the procedure involved in the analysis of drug using FTIR.

5. Explain the principle and applications of LC-MS.

6. Describe the analytical profile of a drug of Aspirin.

7. Discuss structure, synthesis and activity relationship of quinine.

8. Discuss structure, synthesis and activity relationship of glutamycin

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