Syllabus - M. Sc. Second Year - Analytical Chemistry

Syllabus for M. Sc. II Year Analytical Chemistry

Semester III:

Paper Code Subject

ACH-381 Principles of analytical chemistry

ACH-382 Spectrochemical methods of Analysis

Elective Group – A

OCH-353 Organic Spectroscopy

ACH-384(A) Chromatographic methods of analysis

Elective Group – B

ACH-383(B) Environmental Chemical Analysis and Control

ACH-384(B) Recent Advances in Analytical Chemistry

Elective Group – C

ACH-383(C) Organic Industrial Analysis

ACH-384(C) Chemical Analysis in Agro and Food Industries

ACH-385 Laboratory Course – 5 (Related to Two Compulsory Papers)

ACH-386 Laboratory Course – 6 (Related to Two Compulsory Papers)

ACH-387 Seminar

ACH-381: Principles of Analytical Chemistry ( 60 Lectures ) Credits 4

1. Errors, Statistics and Sampling

Accuracy and precision, Error, types of error, systematic and random errors, minimisation

of errors, mean and standard deviations, reliability of results, confidence interval,

comparison of results, student T test, F test, Comparison of two samples (Paired T test),

correlation and regression, correlation coefficient and liner regression, Sampling , the basis

of sampling, sampling procedure, sampling statistics.

2. Acid Base Equilibria and Buffer Solutions

Acid-base theories, Definition of pH and pH scale (Sorenson and operational definitions),

and its significance, Hammett acidity function, pH at elevated temperatures, pH for aqueous

solutions of very weak acid and base, pH for salts of weak acid and weak bases, polyprotic

acids. Buffer solutions, buffer capacity, applications of buffers, Physiological buffers, buffers

for biological and clinical measurements.

3. Theory of Volumetric and Gravimetric Analysis

Introduction, Titrimetric analysis, classifications of reactions in titrimetric analysis,

standard solutions, preparation of standard solutions, primary and secondary standards,

Indicators, theory of indicators, Acid–base titrations in non-aqueous media.

Gravimetric Analysis, Impurities in precipitates, Gravimetric calculations, precipitation

equilibria (Solubility product, common ion effect, stoichiometry), organic precipitation.

4. Complexometric equilibria

Introduction, Titration curves, Types of EDTA titrations, Methods of End Point Detection

(a)Indicators (b) Instrumental methods of End point detection (Spectrophotometric,

Amperometric, Potentiometric, High frequency titrator), Types of Complexometric

Titrations (a) Direct Titration (b) Back Titration (c) Replacement titration (d) Indirect

Titration (e) Applications of Complexometric Titrations

Numerical Problems based on the topics mentioned above.

Books Recommended:

1. D. A. Skoog and D. M. West, Fundamental of Analytical Chemistry, 7th Edition (1996),

Saunders College Publishing, Philadelphia, Holt, London.

2. R. L. Pecsok, L. D. Shields, T. Cairns and L.C. McWilliam, Modern Methods of Chemical

Analysis, (1976), John Wiley & Sons, New York.

3. D. A. Skoog, Principles of Instrumental Analysis, 5th Edition (1998), Saunders College of

Publishing, Philadelphia, London.

4. H. A. Strobel, Chemical Instrumentation: A Schematic Approach, 2nd Edition (1973),

Addison Wesley, Reading, Mass.

5. Analytical chemistry, G. D. Christian, Sixth Edition, Wiley publications

ACH-382: Spectrochemical Methods of Analysis

1. Molecular spectrophotometry

Introduction, Lambert, Beer’s law, deviations, quantitative analysis, Theory of

spectrometry and colorimetry, classification of methods of colour measurements or

comparison, standard curve method, balancing method/ calibration graph method,

derivative spectrometry and applications.

2. Atomic Absorption and flame emission spectrometry.

Flame spectrometry: introduction, elementary theory, instrumentation, type of burners,

interferences, type of interferences, background correction method and applications.

AAS: Principle, instrumentation, production of atoms and ions, burners, detectors, HCL,

TGL, EDL, advantage and disadvantage of AAS, standard addition method, internal standard

method.

3. Atomic emission spectrometry

Introduction, equipment, qualitative and quantitative analysis with AAS, plasma emission

spectrometry, direct current plasma, inductively coupled plasma, ICP-AES, high energy

sources (plasma, arc, and spark), sample introduction and measurements.

4. Molecular fluorescence and X-ray fluorescence

Introduction, theory, fluorescence, Instrumentation and applications.


Books Recommended:

1. G. H. Morrison and H. Freiser, Solvent Extraction in Analytical Chemistry, 1st Edition

(1958), John Wiley, New York.

2. B. L. Karger, L. R. Snyder and C. Howarth, An Introduction to Separation Science, 2nd

Edition (1973), John Wiley, New York.

3. E. W. Berg, Chemical Methods of Separation, 1st Edition (1963), McGraw Hill, New York.

4. D. G. Peters, J. M. Hayes and C. M. Hieftj, Chemical Separation and Measurements, 2nd

Edition (1974), Saunders Holt, London.

5. J. D. Seader and E. J. Henley, Separation Process Principles, 1st Edition (1998), John

Wiley & Sons. Inc., New York.

Elective courses

ACH-383(A): Organoanalytical Chemistry

1. Hyphenated Techniques

Advanced techniques of analysis: UV-Visible, IR, 1H & 13C-NMR, Mass spectrometry, GC-MS,

HPLC-MS, HPTLC-MS and their applications.

2. Pharmaceutical Analysis

Introduction to drugs, their classification, sources of impurities in pharmaceutical raw

materials such as chemical, atmospheric and microbial contaminants etc. Limit tests, limit

tests for impurities like, Pb, As, Fe, moisture, chlorides, sulfates, Boron, free halogen,

selenium etc. Analysis of some commonly used drugs likes sulfa drugs, antihistamines,

barbiturates, vitamins (A, B6, C , E, K) etc.

3. Analysis of dyes and paints

Types of dyes, and their analysis. Composition and analysis of paints, determination of

volatile and non-volatile constituents, flash points, separation of pigments, estimation of

binders and thinners


Books Recommended:

1. F. J. Welcher: Standard methods of Chemical analysis, 6th Ed. Vol. I and II (D. Van

Nostard Comp.)

2. I. M. Kolthoff: Treatise on Analytical Chemistry Vol. I & II.

3. F. D. Snell: Encyclopedia of industrial Chemical Analysis Vol. 1 to 20 (John Wiley)

4. Riech: Outline of Industrial Chemistry.

5. K. H. Buchel: Chemistry of Pesticides (John Wiley).

6. Indian, Pharmacopoeia, British Pharmacopoeia and U. S. Pharmacopoeia.

7. V. M. Parikh: Absorption spectroscopy of organic molecules (Addision Wesley)

8. Willard, Merrite, Dean and Settle: Instrumental methods of analysis (CBS)

9. D. H. Williams and J. Fleming: Specroscopic methods in organic chemistry (Mc Graw

Hill)

10. Silverstein : Spectroscopic Identification of organic compounds (John Wiley)

11. Jackmann and Sternhill : Applications of NMR spectroscopy of organic Chemistry

(Pergamon Press)

12. J. D. Roberts : Nuclear Magnetic Resonance ( Mc Graw Hill)

13. K. Benjamin : Mass Spectrometry

14. Nichollas: Aids to the Analysis of foods and Drugs.

15. A. H. Beckett and J. B. Stanlake; Practical Pharmaceutical Chemistry Vol. I & II (CBS

publishers)

16. S. Ranganna:Handbook of analysis and quality control for fruits and vegetable products

(McGraw Hill)

17. Ramalu: Analysis of pesticides

ACH-384(A): Chromatographic methods of analysis

1. Introduction to Chromatographic methods

Principles of analytical separation: Plate theory, rate theory, Craig concept of counter

current distribution, process optimisation, Retention analysis; Resolution (Fundamental

equation). Distillation: Fractional distillation, Molecular distillation.

2. Conventional column chromatography

Introduction, stationary phase, mobile phase, polarity of solvents, retention time, curve

width, column adsorption equilibrium, gravity column chromatography, flash column

chromatography, advantages and limitations of column chromatography.

3. Gas Chromatography

Introduction, instrumentation, types of column (packed, open tubular etc.), types of

detector (TCD, ID, FID, ECD, element selective detectors), programme temperature gas

chromatography, applications of GC for quantitative analysis. Internal standard method

and standard addition method.

4. High performance liquid chromatography

Introduction, Types of liquid chromatography, high performance liquid chromatography

and instrumentation, derivatization, quantitative analysis, thin layer chromatography, high

performance thin layer chromatography,

5. Supercritical fluid chromatography

Introduction, SFC Advantages, Supercritical Fluids, Instrumentation, Supercritical Mobile

Phase, Injectors, Ovens and Pumps, Columns, Detectors, SFC for the separation of polymers

and of pesticides.

6. Electrochromatography

Introduction, paper electrophoresis, gel electrophoresis, size exclusion chromatography (gel

filtration chromatography), Electrophoretic Mobility, Technique, factors affecting

migration of ions, capillary electrophoresis/capillary zone electrophoresis and

applications, Gradient Electrochromatography.

7. a) Ion chromatography: Basic principles, separator column, suppressor columns,

detectors, applications.

b) Ion exchange chromatography: Introduction, ion exchange equilibria, types of ion

exchange resins (strongly acidic, strongly basic, weakly acidic, weakly basic),

instrumentation, ion exchange capacity.

Numerical problems on the topics mentioned above.

Books Recommended:

1. D. A. Skoog and D. M. West, Fundamental of Analytical Chemistry, International

Edition, 7th Edition (1996), Saunders College Publishing, Philadelphia, Holt, London.

2. R. L. Pecsok, L.D. Shields, T. Cairns and L.C. McWilliam, Modern Methods of Chemical

Analysis, 2nd

(1976), John Wiley & Sons, New York.

3. L. R. Shyder and C. H. Harvath, An introduction to separation science, Wiley

Interscience.

4. H. H. Willard; L. L. Merit; J. A. Dean & F. A. Settle, Instrumental Methods of Analysis

(CBS).

ACH-383(B): Environmental Chemical Analysis and Control

1. Sampling in analysis

Definition, theory and techniques of sampling , sampling of gas , liquids and solids , Criteria

of Good sampling , Minimization of Variables, transmission and storage of samples , high

pressure ashing techniques (HPAT), particulate matter , its separation in gas stream,

Filtering and gravity separation. Analysis of particulate matter like asbestos, mica, dust and

aerosols etc.

2. Environment its characteristics and Classification

Metallic and non-metallic pollutants Cr, Hg, Pb, Cd, Cu, As etc. Their physiological

manifestation, source, analysis and control of inorganic compounds.

3. Air pollution

Chemistry of Air pollutants, Characterization. Source, methods of analysis of air pollutants;

CO, CO2, NOX, NH3, H2S, SO2, etc. Monitoring Instruments, Potable and Industrial water,

major and minor components, dissolved oxygen (DO) Chemical oxygen demand (COD)

Biochemical oxygen demand (BOD) and their measurements and significance in waste

water treatments, Threshold odour number.

4. Industrial waste Water analysis

Quality of Industrial waste Water analysis for organic and Inorganic constitutents,

Chemistry of odour and its measurements, Radioactive wastes and its control, Seweage and

sludge analysis. Treatment, disposal and source of phenolic residue, Analytical methods,

treatment by using stream. Gas stripping, ion exchange, solvent extraction, oxidation

method and microbiological treatment.

Books Recommended:

1. A. K. De: Standard Methods of Waste and Waste water analysis.

2. S. M. Khopkar, Environmental Chemistry; Environmental pollution analysis.

3. M. S. Creos and Morr, Environmental Chemical Analysis, American publication(1988)

4. A. K. De, Environmental Chemistry, New Age International publishers.Moghe and

5. Ramteke, Water and waste water analysis : (NEERI)

6. A. C. Stern, Air pollution: Engineering control vol.IV(AP)

7. P. N.Cheremisinoff and R.A.Young, Air Pollution controland Design.Hand Book Vol.I&II

(Dekker)

8. R. B.Pohasek, Toxic and Hazardous waste disposal, Vol.I&II (AAS)

9. M. Sitting, Resources Recovery and Recycling, Handbook of industrial Waste.

10. B. K. Sharma, Industrial Chemistry.

11. S. P. Mahajan, Pollution Control in Process Industries.

12. R. A. Horne, Chemistry of our Environment.

ACH-384(B): Recent Advances in Analytical Chemistry

1. Ultra Purity and Ultra trace Analysis:

Ultra purity and ultra trace analysis, laboratory dosing, purification of reagents,

Preconcentration Techniques, Methods of trace analysis such as NAA, XRF,AAS and ICP,

High purity materials for electronic industry, contamination control during analytical

operations.

2. Radio-analytical Chemistry:

Separation methods, Precipitation, solvent extraction and chromatographic methods.

Activation analysis, basic principles, fast neutron activation analysis, radiochemical

methods in activation analysis, Applications if Geo-chemistry, oxygen in metals. Isotope

dilution analysis: Principles and applications. Sub-stoichiometric determination of traces of

metals: Principles, techniques and experimental methods in the determination of As, Pb

and Hg.

3. Advanced Techniques in Analysis:

13C, 15P, 17O MNR Spectroscopy applications.

4. Electron Spin Resonance Spectroscopy:

Electron behaviour, ESR spectrometer, Spectra, Hyperfine interaction, free radical and

interpretation of the spectra, Applications in quantitative analysis.


Books Recommended:

1. Garen W. Ewing, Analytical Instrumentation, Handbook, Marcel Dekker Inc. (1997).

2. Mereitt, Dean, Settel, Instrumental methods of Chemical Analysis.

3. M. Zeif and J.W.Mitchell, Contamination Control in trace elemental analysis.

4. Ajuja, Ultrapurity.

5. Minczewski,Chwastowska and Dycozynski, Separation and pre-concentration methods

in Inorganic trace analysis.Ellis Haward.

6. Cali, trace Analysis of semiconductor Materials Pergamon.

7. Overman and Cleark, Radioisotopes techniques MGH.

8. Tolgyessy, Brown and Kyrs, Isotope dilution analysis.

9. Leniham and Thomson, Activation Analysis(AP)

10. Ruzica and Stary, Substopchiometry in Radiochemical Analysis. Pergamon.

11. Ladd and Lee, Radiochemistry.

12. Clerk, Handbook of Radiochemical methods

13. Price, Nuclear radiation detections.

ACH-383(C): Organic Industrial Analysis

1. Analysis of oils, fats, soaps and detergents

Introduction to natural fats and oils, Analysis of oils and fats: Softning point, Congent point,

Titre point, cloud point, Iodine, Saponification, acid, hyroxyl, R-M and Polenske value,

Elaiden test.

Introduction to soaps, analysis of soap (saponifiable, unsaponifiable) and for unsaponified

matter in soaps, Estimation of free alkali and phenol in soap. Classification of detergents (in

Brief): Analysis of active ingredients from detergents (methylene blue and Hyamine-1622

method); Estimation of CMC, Chlorides, total phosphates etc.

2. Analysis of cosmetics

a) Composition of creams and lotions: Determination of water, porpylene glycol non-

volatile matter and ash content. Determination of borates, carbonates sulphate, phosphate,

chloride, titanium and Zinc oxide.

b) Analysis of face powder: Estimation of boric acid, Mg, Ca, Zn, Fe, Al, and Ba.

c) Analysis of ingredients of hair dyes.

3. Food Analysis

Food flavours, food colours, food preservatives, Milk and milk products, fluor staches,

honey, jam, and their major component analysis

4. Analysis of petroleum products

Cloud point, pour point, flash point, vapour pressure, specific gravity and their

determination, Estimation of ‘S’ and ‘Pb’ in petrol


Books Recommended:

1. S. R. Junk and H. M. Pancoast: Hand book of sugars(AVI)

2. B. Bilot and B. V. Well: Perfumary technology (JW)

3. I. M. Kolthoff: Treatise on Analytical Chemistry Vol. I and II

4. D. Pearson: Laboratory techniques in food analysis.

5. S. Ranganna: Handbook of Analysis and Quality control for fruits and vegetable

products, 2nd Ed.(Mc Graw Hill.)

6. Nicholls : Aids to the analysis of foods and drugs.

7. G. J. Mountrey: Poultry product technology (AVI)

8. Karamer Twig: Quality control for food industry (AVI)

9. G. F. Longonan: the analysis of detergents and detergent products (JW)

10. A. Davidsohn & B. M. Mlwidaky : Synthetic detergents (Book center, Mumbai)

11. M. Ash and L. Ash: A formulary of cosmetic preparations. (G. Goodwin)

12. Kurl Bauer, Dorothea Garhe, Horst Surburg: Common fregrance and flavour materials,

(VCH publisher, New York)

13. F. J. Welcher: Standard Methods of Chemical analysis Vol I & II (6th Ed.)

14. S. N. Mahendru: Analysis of food products (Swan Publishers)

ACH-384(C): Chemical Analysis in Agro, and Food Industries.

1. Analysis of soil

Moister, pH, total nitrogen, phosphorous, silica, lime, Magnesia, Manganese, sulfur & alkali

salt, carbon, fertilizers and pesticide analysis.

2. Food analysis:

Food analysis: Solid, liquid and Gas, ultimate and proximate analysis heating values,

grading of cool, liquid fuels, flasks points, aniline point, octane number and carbon residue,

gaseous fuels – producer gas and water gas – calorific value.

Moisture, ash, crude protein, fat, crud fibre, carbohydrate, calcium, potassium, sodium, and

phosphates, food adulteration – common adulteration in food, contamination of food stuffs,

microscopic examination of foods for adulterants, Pesticide analysis in food products,

Extraction and purification of sample, HPLC, gas chromatography for organo–phosphates,

thin layer chromatography for identification of chlorinated pesticides in food products


Books Recommended:

1. Fundamentals of analytical chemistry by D. A. Skuog , D. M. West and F. J. Honer, W. B.

Saunders.

2. Chromic phenomenon, The Technological application of color chemistry Peter

Bamfield.

Practical Course for semester-III:

ACH-385: Laboratory Course – 5

1. Conductometric titration of (I) strong acid, monobasic weak acid or polybasic weak

acid with strong base (ii) Zinc with EDTA, and (iii) KCl vs AgNO3.

2. Determination of pH and pKa values of a weak acid potentiometrically using

quinhydrone electrode.

3. Determination of phosphoric acid in cola beverages by pH titration.

4. Determination of ferrous ammonium sulfate potentiometrically with standard ceric

sulfate solution (Direct and back titration).

5. Determination of concentration of halide ion(s) in the given solution

potentiometrically.

6. Determination of concentration of Fe ion in ferric salicylate complex

spectrophotometrically.

7. Simultaneous determination of arsenic (III) and antimony (III) by spectrophotometry.

8. Simultaneous determination of chromium and manganese by spectophotmetry.

9. Determination of sulphate and phosphate by spectrophotometry.

10. Spectrophotometric determination of pK value of an indicator.

11. Determination of moisture content in organic compounds using Karl-Fischer method.

12. Determination of glucose from blood serum (enzyme method/folin-Wu-method).

13. Fluorometric determination of riboflavin (vitamin B2).

14. Determination of normality of given HCl and CuSO4 thermometrically

15. Estimation of percentage of each constituent in mixture of CuSO4 and NaCl using TGA.

16. Estimation of carbohydrates by Anthrone method.


1. Separation and estimation of Zn2+ and Cd2+ by Ion exchange chromatography.

2. Separation and estimation of Br- and Cl- by Ion exchange chromatography.

3. Estimation of Zn2+ and Mg2+ by Ion exchange chromatography.

4. Determination of magnesium and calcium in tap water by atomic absorption

spectroscopy.

5. Determination of vanadium in lubricating oil by atomic absorption spectroscopy.

6. Estimation of Na, K and Ca in a mixture using Flame photometer.

7. Separation by column chromatography (1)

8. Separation by column chromatography (2)

9. Molecular weight of polymer by viscosity measurements.

10. Determination of aspirin, phenacetin and caffeine in a given mixture by using HPLC.

11. Quantitative analysis of mixture by gas chromatography.

12. Separation of mixture using liquid chromatography.

13. Estimation of metal ions using atomic absorption spectrometry.

Semester IV:

Paper Code Subject

ACH-481 Electroanalytical techniques in chemical analysis

ACH-482 Applied Analytical Chemistry

Elective Group – A

ACH-483(A) Quality asuurance, quality control, analytical method

devolopment and validation

ACH-484(A) Techniques in Forensic sciences and Pharmaceuticals analysis.

Elective Group – B

ACH-483(B) Analysis of Microbiological and Polymeric materials

ACH-484(B) Clinical and Consumer Product Analysis

Elective Group – C

ACH-483(C) Biosensors and Agrochemicals

ACH-484(C) Clinical and Consumer Product Analysis

ACH-495 Laboratory Course – 7 (Related to Two Compulsory and Elective

Papers)

ACH-486 Research Project

ACH-487 Seminar

Analytical Chemsitry, Semister-IV (Core papers)

ACH-481: Electroanalytical techniques in chemical analysis.

1. Potentiometry

Fundamentals, reference electrode, indicator and ion selective electrodes, Instrumentation

and measurement of cell emf.

2. Voltammetry

Fundamentals, conventional or DC polarography, theoretical principles, complex ions,

quantitative techniques, the effect of oxygen, simple polarography and classical DC

polarography, the three electrode polarograph: potentiostatic control, modified voltametry,

cyclic voltammetry, quantitative applications of polarography.

3. Polarography

Theory, apparatus: derivative polarography, modified polarographic techniques, sinusoidal

AC polarography, pulse polarography, chronopotentometry and their application in

qualitative and quantitative analysis.

4. Coulometry

Introduction: principles, technique, coulometry at constant current and controlled

potential coulometry , applications and stripping analysis. Unit-III: High frequency titration

Introduction: theory and instrumentation, high frequency titrimetry, types of cell.

Advantage of high frequency methods, applications.

5. Electrogravimetry

Introduction, theory, apparatus, cell processes, deposition and separation, electrolytic

separation of metals, metals which can be determined.

Books Recommended:

1. R.D. Braum, Introduction to Instrumental Analysis.

2. Willard, Deritt, Dean and Settle, Instrumental methods of Analysis.

3. F. J. Welcher, standard Methods of chemical Analysis Vol.3, Part A & B.

4. G.W. Ewing, Instrumental Methods of Analysis 4th and 5th editions.

5. Chatawal and Anand, Instrumental Methods of Analysis.

6. Bassett, Denney-Jeffer and Mendham, Vogel’s Textbook of Quantititative Inorganic

Analysis.

7. Electro-analytical chemistry, edited by H.W.Nurnberg.

8. Kortum and Bockris, A Textbook of Electrochemistry.

9. D.A. Maclines, Principles of Electrochemistry.

10. Stulic, Ion selective electrodes (John Wiley).

ACH-482: Applied Analytical Chemistry

1. Analysis of Minerals and Ores: Bauxite, haematite, dolomite, phosphates, monazite,

pyrites and the chemicals from sea.

2. Analysis of metals and alloys: Foundry materials, analysis of coal, ferroalloys, and

special steels, slags, fluxes, brass and bronze.

3. Analysis of soil and fertilizers: Method of soil analysis, soil fertility its determination,

determination of inorganic constituents of plant materials, Chemical analysis as measure of

soil fertility, analysis of fertilizers.

4. a)Analysis of Pesticide residues: Estimation of Malathion, parathion.

Organomercurials and related pesticides residues in food samples.

b) Types of plastics and their Identifications: Determination of molecular weight of

plastic and determination of metallic impurities in plastics.

c) Explosives: Types and Analysis.

Books Recommended:

1. Hillebrand Lhundel, Bright and Hoffiman, Applied Inorganic Analysis, John Wiley.

2. Snell and Biffen, Commercial Methods of Analysis.

3. P. G. Jeffery, Chemical Methods of Rock Analysis, Pergamon.

4. Buchel, Chemistry of Pesticides. J Wiley.

5. Rieche, Outlines of Industrial Organic Chemistry, ButterWorth.

6. F. A. Henglein, Chemical Technology, Pergamon.

7. Kent, Riegl’s Industrial Chemistry,Rainhold.

8. Chopra and Kanwar,Analytical Agriculture Chemistry, Kalyani Publishers.

9. Aubert and Pintes, Trace Elements in Soils.

10. Bear, Chemistry of Soil.

11. Hauson, Plant Growth Regulators, Noyes.

12. P. G. Jeffery and D.J. Hatchinson, Chemical Methods of Rock Analysis.

13. F. J. Weleher, Standard Methods of Chemical Analysis, A Series of Volumes Robert and

Krigeger Publishing Company.

14. I. M. Kolthoff and PJ Ewing, Treatise o Analytical Chemistry, A series of Volumes.

15. R. D. Reeves and R.R. Brooks, Trace element Analysisof Geological Materials, John Wiley

& Sons NewDehli.

16. W. M. Johnson and J.A.Maxwell,Rock and Mineral Analysis, John Wiley and Sons,

NewYork.

17. W. F. Hildebrand, G H C Landell and HABrighot, Applied Inorganic Analysis, John Wiley

2nd Edition.

18. K. J. Das, Pesticide Analysis(MD).

ACH-483(A): Quality asuurance, quality control, analytical method devolopment and

validation

A) Quality Assurance and Quality Control:

a) Industrial Analysis:

Quality characteristics of chemical analysis, errors occurring at the start, during or by the

end of analysis, interpretation and presentation of results, Shewhart Chart, CUSUM chart

and EWMA chart; Batch and process evaluation, QA schemes, experimental designs for

optimization studies and ruggedness testing, system management;

b) Clinical Analysis:

Introduction, analytical responsibilities, Managerial responsibilities, practical approaches

to QA, characterization of a method, Results and preparation of reports. Internal QC,

Accuracy and external quality assessment, near-patient testing and QC;

c) Water Industry:

Water quality field sampling QA/QC program, QA/QC documentation, QA project plan,

designing a water quality monitoring plan, Site selection, sampling frequency and sample

size, cost considerations, training of field personnel, field trip preparations, Water quality

sampling, toxic chemicals in bottom sampling and biota, bacterial sample collection,

sequential triplicate sampling, sample handling, preservation, storage and transport, chain

of custody, field safety, field audit program, laboratory QC procedures inter- and intra-

laboratory QC, detection limits, reporting of analytical results, data handling and data

management

B) Reference Materials (RMs):

Analytical standards, primary and secondary standards, high purity substances, reference

materials, use of RMs in statistical control schemes and in intercomparisons, role of

certified reference materials (CRMs), production and requirements, obtaining reference

value and certified value.

C) Development and validation of Analytical Method:

Analytical method development:

Theory and factors affecting resolution – a reminder of the importance of resolution,

separation factor (selectivity), retention factor (capacity factor) and column efficiency).

Selecting the HPLC separation mode (reversed-phase, normal-phase etc.) Selecting the

most appropriate detector

Gradient/isocratic operation, selecting the column for analysis, Selecting and optimising

the mobile phase, the effect of pH, considering pKa of the analyte

Requirements for a stability-indicating analytical method, Anticipation of likely

degradation products, From experience with compound, From forced degradation (stress

testing) of drug substance, as per ICH guidance, Note findings of stress-testing industry

comparison , Are degradation products likely to be enantiomers or diastereoisomers?,

Calculation of mass balance and its significance

Validation of methods

Introduction to ICH guidelines: ICH Q2(R1), A detailed discussion on the parameters to be

validated, Specificity: peak purity determination (Diode array and MS detectors), Linearity,

Range, Accuracy, Precision, Detection Limit, Quantitation Limit, Robustness

Extent of validation: how much work at each phase of development, Acceptance criteria,

Validation procedures and protocols, Dealing with validation failures

Books Recommended:

1. D. A. Skoog , D. M. West and F.J.Holler, Fundamentals of Analytical Chemistry, 2nd Ed.,

Saunders College Publishing, 1991.

2. R. A. Day and A.L.Underwood, Quantitative Analysis, 6th Ed., Prentice-Hall of India

Pvt.Ltd., 1993.

3. Gas Chromatography, Open Book Learning Series

4. Larry Hargis, Analytical Chemistry. Principles and techniques

5. Encyclopedia of Analytical Chemistry, Vol.

ACH-484(A): Techniques in Forensic sciences and Pharmaceuticals analysis.

a. Forensic Analysis: Overview, Destructive and Nondestructive techniques, Data

interpretation.

b. Blood Analysis: Blood preservation and ageing effects, Analysis of blood components

and exogenic substances, blood stain analysis.

c. DNA Profiling : DNA and its polymorphism, DNA typing procedures-RFLP, PCR, MVR-

PCR, Dot-blot, AMP-FLP, STR, other methods, paternity testing, applications, interpretation

and practical use.

d. Determination of alcohol in body fluids: Legal background, Sampling and sample

preservation, analysis-GC, IR, enzymatic and other methods.

e. Fingerprint analysis: Latent fingerprints; optical, physical, physico-chemical & chemical

detection methods; fingerprints in blood, fingerprint detection sequences.

f. Hair analysis: Structure and composition of hair, morphological examination, Chemical

analysis of hair components and components remaining on or in hair.

g. Systematic Drug Identification: Classification and categories of compounds involved,

analytical strategy-EMIT, FPIA, TLC, LC, GC-MS, etc., requirements for identification,

possibilities & limitations of selected techniques, isotope detection method with

numericals, new drug groups.

h. Materials of interest for Forensic studies: Explosives: Types, analytical methods for

identification of low and high explosives in post-blast debris. Fibres: Fibres encountered at

crime scene, identification of types, dye extraction and analysis, colour matching, analysis

for metals, additives and contaminants-SEM-EDX, XRD,XRF.

Paints, Varnishes and Lacquers: Formulation of paints, types of sample, Sample pre-

treatment prior to analysis, colour measurements, Analysis by SEM, SEM-SPMA, TEM,

TLC/HPTLC, PyrGC, IR, Raman, UV-Vis-Flu, XRF, AES, TG-DTA. Glass: As forensic evidence,

measurement of physical properties, elemental analysis-XRD, NAA, etc., interpretation of

results, casework examples. Arson Residues: nature of arson evidence, chemical evidence,

properties of liquid accelerants, sampling and sample pre-treatment, laboratory

examination of suspect arson evidence, evidential value. Gunshot Residues: Composition

of sources, detection on hands & its limitations, determination of muzzle-to-target distance,

elemental & inorganic analysis, numericals on estimation of energy released by combustion

reactions, etc.

Books Recommended:

1. ‘Forensic Chemistry’ by Suzanne Bell, Pearson Prentice Hall Publishers, 2006

2. Encyclopaedia of Analytical Chemistry, Volume 3, Academic Press, 1995

3. Allan Cury,Irvins Sunshine, Forensic Analysis, Academic Press Publications.

4. E.G.J.Clarics, Isolation and Identification of drugs, Pharmaceutical Press.

5. C.J.Creswell, C.A.Runquist and M.M.Campbell, Spectral Analysis of Organic Compounds.

6. F.J.Welcher, Robert E,Standard Methods of Chemical Analysis, A series of volumes.

7. Hawk’s Physiological Chemistry.

ACH-483(B): Analysis of Microbiological and Polymeric materials

1: Analytical Microbiology

Morphological structure and characteristics nutrition and physiology, classification of

microorganisms, Taxonomy and nomenclature Nutritional requirements Phathoseas and

Spoilage organics Microscopy, Staining techniques, Aspatic Techniques, isolation and use of

differential media, sterilization and disinfection.

2. Applied Microbiology

Air Microbiology with respect contamination control, Food Microbiology, Walia

microbiology, Industrial microbiology with respect to quality control.

3. Analysis of Polymers

Molecular Weight of polymers – Arithmetic, weight average and number average molecular

weights of polymers, Determination of molecular weight of polymers, End-Group Analysis,

Cryoscopy, Light scattering, Viscosity, and gel permeation chromatographic methods,

Thermal Transition in Polymers, Tg and Tm and their relation, DSC, TGA, Spectral methods

of Analysis.

Books Recommended:

1. D. J.Holme and H. Pack, Analytical Biochemistry, Longman.

2. G. Keleti and W H Liederer, Hand book of micro methods for the biological science-

VNR.

3. C. H. Collins, Microbiological Methods, Butterworths.

ACH-484(B): Clinical and Consumer Product Analysis

Clinical analysis:

Enzymatic and Immunochemical Analysis, Mineral metabolism, Electrolyte analysis, Body

fluid analysis, Therapeutic drug monitoring, Scope of Clinical chemistry: Philosophy of

clinical analysis, Practical aspects of analysis: sample types, collection of specimens

(samples) like blood, urine, faeces; Cleaning of glass apparatus; Storage of clinical samples.

General techniques for analysis: Brief principle and applications of following techniques:

colorimetric, spectrophotometric, turbidimetric, fluorimetric, flame photometry,

autoanalysis, paper electrophoresis, gel-electrophoresis, chromatography; Units of

expressing biochemical values.

Protein structure and analysis: Definition of protein and peptides; structure of protein;

types of protein s; Physical and chemical properties of protein; Analysis of proteins: Total

protein, albumin and globulin from serum samples.

Hormone analysis: Introduction; Classification and general characteristics of hormones;

Determination of cortisol from blood and urine samples; determination of oestrogens from

urine samples

Consumer Product Analysis

Consumer products and their chemical speciation (as well as qualitative and quantitative

analysis), Cosmetics – Face powders, hair preparations, Antiperspirants and deodorants,

Perfumes, Toothpastes, Food pigments

Books Recommended:

1. B. M. Mittal and R. N. Saha, Handbook of Cosmetics,Vallabh Prakashan, New Delhi, 1st

edn., 2000.

2. S. Nanda and R. K. Khar, Cosmetic Technology, Birla Publication Pvt. Ltd., 1st edn.,

2006.

ACH-483(C): Biosensors and Agrochemicals

Biosensors

Definition, components and types of Biosensors, Enzyme-based Biosensors, Immobilization

of enzymes, Types of transducers, fabrication of probes for sensors and evaluation of

sensor Performance, Applications of Biosensors

Analysis of Agrochemicals

Introduction, Classification, mechanism of action and synthesis.

Insecticides : DDT, BHC,Aldrin, Endosulfon, Malathion, Parathion.

Herbicides : 2,4-dichloro phenoxy acetic acid, dalapon, paraquat, Banalin, Butacarb .

Fungicides : Boardeaux mixture, Copper oxychloride, Zineb,, Benomyl(Benlte) Analysis of

pesticide residue and toxicological effects.

Books Recommended:

1. Text Book of Polymer Science by F. W. Bilmayer;

2. Polymer Science by Gowarikar

3. Introduction to polymer science and chemistry by M. Chanda, Taylor and Francis Pub.

4. Chemistry of pesticides, N.M. Melnikov, Residue Reviews, Vol.36, Springer Verlag, New

York, 1971.

5. Future for insecticides , R.C. Netealr, J.J.Mckalvery, Jr. John Wiley &Sons, New York,

1976.

6. A. Townshend, Ed., Encyclopedia in Analytical Science, Academic Press (1995)

7. R. L. Na Academic Press, Calcutta.

ACH-484(C): Clinical and Consumer Product Analysis

See ACH-484(B).


ACH-486: Research Project

ACH-487: Seminar

Syllabus - M. Sc. Second Year - Analytical Chemistry

Documents