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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
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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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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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GITAM UNIVERSITY (Syllabus for M.Phil / pre-Ph.D degrees, w.e.f. 2008-2009 admitted batch)
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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GITAM UNIVERSITY Pre-Ph.D/M.Phil Examinations
(Chemistry)
Model Paper
SRPCH–122/ SRFCH–122: Advanced Topics in Organic Chemistry
Max. Marks: 100 Time: 3hrs
----------------------------------------------------------------------------------------- Answer any FIVE of the following:
(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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GITAM UNIVERSITY (Syllabus for M.Phil / pre-Ph.D degrees, w.e.f. 2008-2009 admitted batch)
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
GITAM UNIVERSITY Pre-Ph.D/M.Phil Examinations
(Chemistry)
Model Paper
SRPCH–123/ SRFCH–123: Advanced Topics in Physical Chemistry
Max. Marks: 100 Time: 3hrs
----------------------------------------------------------------------------------------- Answer any FIVE of the following:
(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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GITAM UNIVERSITY (Syllabus for M.Phil / pre-Ph.D degrees, w.e.f. 2008-2009 admitted batch)
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
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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
GITAM UNIVERSITY Pre-Ph.D/M.Phil Examinations
(Chemistry)
Model Paper
SRPCH–124/ SRFCH–124: Advanced Topics in Analytical Chemistry
Max. Marks: 100 Time: 3hrs
----------------------------------------------------------------------------------------- Answer any FIVE of the following:
(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
GITAM UNIVERSITY (Syllabus for M.Phil / pre-Ph.D degrees, w.e.f. 2008-2009 admitted batch)
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
GITAM UNIVERSITY Pre-Ph.D/M.Phil Examinations
(Chemistry)
Model Paper
SRPCH–125/ SRFCH–125: Advanced Topics in Environmental Chemistry
Max. Marks: 100 Time: 3hrs
----------------------------------------------------------------------------------------- Answer any FIVE of the following:
(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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GITAM UNIVERSITY (Syllabus for M.Phil / pre-Ph.D degrees, w.e.f. 2008-2009 admitted batch)
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
GITAM UNIVERSITY Pre-Ph.D/M.Phil Examinations
(Chemistry)
Model Paper
SRPCH–131/ SRFCH–131: Research Methodology - Inorganic Materials
Max. Marks: 100 Time: 3hrs
----------------------------------------------------------------------------------------- Answer any FIVE of the following:
(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
GITAM UNIVERSITY (Syllabus for M.Phil / pre-Ph.D degrees, w.e.f. 2008-2009 admitted batch)
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
GITAM UNIVERSITY Pre-Ph.D/M.Phil Examinations
(Chemistry)
Model Paper
SRPCH–132/ SRFCH–132: Research Methodology – Separation Techniques and
Spectroscopic Methods
Max. Marks: 100 Time: 3hrs
----------------------------------------------------------------------------------------- Answer any FIVE of the following:
(5 X 20 = 100)
1. Describe the writing procedure of a research paper and thesis.
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
GITAM UNIVERSITY (Syllabus for M.Phil / pre-Ph.D degrees, w.e.f. 2008-2009 admitted batch)
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
GITAM UNIVERSITY Pre-Ph.D/M.Phil Examinations
(Chemistry)
Model Paper
SRPCH–133/ SRFCH–133: Research Methodology - General Laboratory
Techniques and Numerical methods of Analysis
Max. Marks: 100 Time: 3hrs
----------------------------------------------------------------------------------------- Answer any FIVE of the following:
(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
GITAM UNIVERSITY (Syllabus for M.Phil / pre-Ph.D degrees, w.e.f. 2008-2009 admitted batch)
SRPCH–134/ SRFCH–134: Research Methodology – Modern Methods of Analysis
In
Environmental Analytical Chemistry
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 :
1. Research Methodology, S. Rajasekar, Bharathidasan University, Tamilnadu, India
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
GITAM UNIVERSITY Pre-Ph.D/M.Phil Examinations
(Chemistry)
Model paper
SRPCH–134/ SRFCH–134: Research Methodology – Modern Methods of Analysis
In
Environmental Analytical Chemistry
Max. Marks: 100 Time: 3hrs
----------------------------------------------------------------------------------------- Answer any FIVE of the following:
(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
GITAM UNIVERSITY (Syllabus for M.Phil / pre-Ph.D degrees, w.e.f. 2008-2009 admitted batch)
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
GITAM UNIVERSITY Pre-Ph.D/M.Phil Examinations
(Chemistry)
Model Paper
SRPCH–135/ SRFCH–135: Research Methodology - Chemical Kinetics
Max. Marks: 100 Time: 3hrs
----------------------------------------------------------------------------------------- Answer any FIVE of the following:
(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
GITAM UNIVERSITY (Syllabus for M.Phil / pre-Ph.D degrees, w.e.f. 2008-2009 admitted batch)
SRPCH–136/ SRFCH–136: Research Methodology – Modern Methods of Analysis
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.
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:
1. Research Methodology, S. Rajasekar, Bharathidasan University, Tamilnadu, India
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
GITAM UNIVERSITY Pre-Ph.D/M.Phil Examinations
(Chemistry)
Model Paper
SRPCH–136/ SRFCH–136: Research Methodology - Modern Methods of
Analysis
Max. Marks: 100 Time: 3hrs
----------------------------------------------------------------------------------------- Answer any FIVE of the following:
(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
GITAM UNIVERSITY (Syllabus for M.Phil / pre-Ph.D degrees, w.e.f. 2008-2009 admitted batch)
SRPCH–137/ SRFCH–137: Research Methodology - Extraction Techniques
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.
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
GITAM UNIVERSITY Pre-Ph.D/M.Phil Examinations
(Chemistry)
Model Paper
SRPCH–137/ SRFCH–137: Research Methodology - Extraction Techniques
Max. Marks: 100 Time: 3hrs
----------------------------------------------------------------------------------------- Answer any FIVE of the following:
(5 X 20 = 100)
1. Describe the writing procedure of a research paper and thesis.
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
GITAM UNIVERSITY (Syllabus for M.Phil / pre-Ph.D degrees, w.e.f. 2008-2009 admitted batch)
SRPCH–138/ SRFCH–138: Research Methodology – Separation Techniques
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.
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:
1. Research Methodology, S. Rajasekar, Bharathidasan University, Tamilnadu, India
2. MN Sastry – Separation Techniques – Himalaya publications
3. A.I. Vogel. A text book of quantitative analysis – ELBS.
28
GITAM UNIVERSITY Pre-Ph.D/M.Phil Examinations
(Chemistry)
Model Paper
SRPCH–138/ SRFCH–138: Research Methodology – Separation Techniques
Max. Marks: 100 Time: 3hrs
----------------------------------------------------------------------------------------- Answer any FIVE of the following:
(5 X 20 = 100)
1. Describe the writing procedure of a research paper and thesis.
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
GITAM UNIVERSITY (Syllabus for M.Phil / pre-Ph.D degrees, w.e.f. 2008-2009 admitted batch)
SRPCH–139/ SRFCH–139– Research methodology- Drug analysis
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.
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:
1. Research Methodology, S. Rajasekar, Bharathidasan University, Tamilnadu, India
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
**********
GITAM UNIVERSITY Pre-Ph.D/M.Phil Examinations
(Chemistry)
Model Paper
SRPCH–139/ SRFCH–139– Research methodology- Drug analysis
Max. Marks: 100 Time: 3hrs
----------------------------------------------------------------------------------------- Answer any FIVE of the following:
(5 X 20 = 100)
1. Describe the writing procedure of a research paper and thesis.
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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