TYBSc Analytical Chemistry 6 Units Syllabus Mumbai University by munotes
Page 1
T.Y.B.Sc. CHEMISTRY (6 UNITS)
Choice Based Credit System
SEMESTER V
ANALYTICAL CHEMISTRY
COURSE CODE: USCH504 CREDITS: 02 LECTURES: 60
UNIT I :INTRODUCTION TO QUALITY CONCEPTS,CHEMICAL
CALCULATIONS AND SAMPLING (3 & 6 UNITS)
1.1 Quality in Analytical Chemistry 05 L
1.1.1 Concepts of Quality, Quality C ontrol and Quality Assurance
1.1.2 Importance of Quality concepts in Industry
1.1.3 Chemical Standard s and Certified Reference Materials ; Importance
in chemical analysis
Quality of material: Various grades of laboratory reagents
1.2 Chemical Calculations (Numerical s and word problems are expected) 04 L
1.2.1 Inter conversion of various concentration units.
(Conversion of concentration from one unit to another unit with
example s)
1.2.2 Percent composition of element s in chemical compounds
1.3 Sampling 06 L
1.3.1 Purpose, significance and difficulties encountered in sampling
1.3.2 Sampling of solids: Sample size – bulk ratio, size to weight ratio,
multistage and sequential sampling, size reduction methods,
sampling of compact solids, equipments and methods of sampling
of compact solids, sampling of particulate solids, methods and
equipments used for sampling of particulate solids .
1.3.3 Sampling of liquids: Homogeneous and heterogeneous, Static and
flowing liquids .
1.3.4 Sampling of gases: Ambient and stack sampling: Apparatus and
Page 2
methods for sampling of gases .
1.3.5 Collection, preservation and dissolution of the sample .
UNIT II : CLASSICAL METHODS OF ANALYSIS (TITRIMETRY) (3 & 6 UNITS)
2.1 Redox Titrations (Numerical and word Problems are e xpected) 08 L
2.1.1 Introduction
2.1.2 Construction of the titration curves and calculation of E system in
aqueous medium in case of :
(1) One electron system
(2) Multielectron system
2.1.3 Theory of redox indicators, Criteria for selection of an indicator
Use of diphenyl amine and ferroin as redox indicators
2.2 Complexometric Titrations 07 L
2.2.1 Introduction, construction of titration curve
2.2.2 Use of EDTA as titrant and its standardisation , absolute and
conditional formation constants of metal EDTA complexes,
Selectivity of EDTA as a titrant.
Factors enhancing selectivity with examples .
Advantages and limitations of EDTA as a titrant .
2.2.3 Types of EDTA titrations.
2.2.4 Metallochromic indicators, theory, examples and applications
UNIT III: OPTICAL METHODS (6 UNITS)
3.1 Atomic Spectroscopy: Flame Emission spectroscopy(FES) and
Atomic Absorption Spectroscopy(AAS) 07 L
3.1.1 Introduction, Energy level diagrams, Atomic spectra, Absorption
and Emission Spectra
3.1.2 Flame Photometry – Principle, Instrumentation (Flame atomizers,
types of Burners, Wavelength selectors, Detectors)
3.1.3 Atomic Absorption Spectroscopy – Principle, Instrumentation
(Sour ce, Chopper, Flame and Electrothermal Atomiser)
3.1.4 Quantification methods of FES and AAS – Calibration curve
method, Standard addition method and Internal standard method.
Page 3
3.1.5 Comparison between FES and AAS
3.1.6 Applications, Advantages and Limitations
3.2 Molecular Fluorescence and Phosphorescence Spectroscopy 04L
3.2.1 Introduction and Principle
3.2.2 Relationship of Fluorescence intensity with concentration
3.2.3 Factors affecting Fluorescence and Phosphorescence
3.2.4 Instrumentation and applications
3.2.5 Comparison of Fluorimetry and Phosphorimetry
3.2.6 Comparison with Absorption methods
3.3 Turbidimetry and Nephelometry 04 L
3.3.1 Introduction and Principle
3.3.2 Factors affecting scattering of Radiation:
Concentration, particle size, wavelength, refractive index
3.3.3 Instrumentation and Applications
UNIT IV: METHODS OF SEPARATION – I (6 UNITS)
4.1 Solvent Extraction 06 L
4.1.1 Factors a ffecting extraction: Chelation, Ion pair formation and
Solvation
4.1.2 Graph of percent extraction versus pH.
Concept of [pH] 1/2 and its significance (derivation not expected)
4.1.3 Craig’s counter current extraction: Principle, apparatus and
applications
4.1.4 Solid phase extraction: Principle, process and applications with
special reference to water and industrial effluent analysis.
4.1.5 Comparison of solid phase extraction and solvent extraction.
4.2 High Performance Liquid chromatography (HPLC) 06L
4.2.1 Introduction and Principle
Instrumentation - components with their significance : Solvent
Reservoir, Degassing system, Pumps -(reciprocating pumps,
screw driven - syringe type pumps, pneumatic pumps ,
advantages and disadvantages of each pump), Pre column ,
Sample injection system, HPLC Columns, Detectors(UV –
Visible detector, Refractive index detector)
4.2.2 Qualitative and Quantitative Applications of HPLC
Page 4
4.3 High Performance Thin Layer Chromatography (HPTLC) 03 L
4.3.1 Introduction and Principle
Stationary phase, Sample application and mobile phase
4.3.2 Detectors
a) Scanning densitometer - Components.
Types of densitometer - Single beam and Double beam
b) Fluorometric Detector
4.3.3 Advantages, disadvantages and applications
4.3.4 Comparison of TLC and HPTLC
REFERENCES
1. 3000 solved problems in Chemistry, David E.
Goldberg,PhD.,Schaums Outline Unit/s: (1.2)
2. A guide to Quality in Analytical Chemistry: An aid to
accreditation, CITAC and EURACHEM, (2002), Unit/s (1.1)
3. A premier sampling solids, liquids and gases, Smith Patricia I,
American statistical association and the society for industrial
and applied mat hematics, (2001) Unit/s (1.3)
4. Analytical Chemistry, Gary.D Christan, 5th edition Unit/s (4.1,4.2,4 .3)
5. Analytical Chemistry Skoog, West ,Holler,7th Edition: Unit/s (2.1)
6. Analytical Chromatography, Gurdeep R Chatwal, Himalaya
publication Unit/s (4.1,4.2,4.3)
7. Basic Concepts of Analytical Chemistry, by S M Khopkar,
new Age International (p) Limited Unit/s (4.1,4.2,4.3)
8. Chemical methods of separation, J A Dean, Van Nostrand
Reinhold, 1969 Unit/s (4.1,4.2,4 .3)
9. Fundamentals of Analytical Chemistry by Skoog and West ,
8th Edition Unit/s (4.1,4.2,4.3)
10. Handbook of quality assurance for the analytical chemistry
laboratory, 2ndEdn., James P. DuxVanNostr and Reinhold,
1990 Unit/s (1.1)
11. High Performance Thin Layer Chromatography by Dr P.D.
Sethi, CBS Publisher and Distribution Unit/s (4.1,4.2,4.3)
Page 5
12. High Performance Thin Layer Chromatography in Food
analysis, by Prem kumar, CBS Publisher and distributer Unit/s (4.1,4.2,4.3)
13. Instrumental methods of Analysis, by Dr Supriya S Mahajan,
Popular Prakashan Ltd Unit/s (4.1,4.2,4.3)
14. Instrumental methods Of Analysis, by Willard Merritt Dean,
7thEdition, CBS Publisher and distribution Pvt Ltd Unit/s (3.1,3.2,3.3)
15. Instrumental Methods of Chemical Analysis by B.K. Sharma
Goel Publishing Hou se Unit/s (4.1,4.2,4.3)
16. Principles of Instrumental Analysis , 5th Edition, By Skoog,
Holler, Nieman Unit/s
(4.1,4.2,4.3) (3.1,3.2,3.3)
17. Quality con trol and Quality assurance in An alytical Chemical
Laboratory, Piotr Konieczka and Jacek Namiesnik, CRC press
(2018) Unit/s (1.1)
18. Quality in the Analytical Chemistry Laboratory, Elizabeth
Prichard, Neil T. Crosby, Florence Elizabeth Prichard, John
Wiley and Sons, 1995 Unit/s (1.1)
19. Solvent extraction and ion exchange, J Marcus and A. S.
Kertes Wiley INC 1 969 Unit/s (4.1,4.2,4.3)
20. . Thin Layer Chromatography, A LAB. Handbook, Egon Stahl,
Springer International Student Edition Unit/s (4.1,4.2,4.3)
PRACTICALS
SEMESTER V
ANALYTICAL CHEMISTRY
COURSE CODE: USCHP13 CREDITS: 02
1. Spectrophot ometric estimation of fluoride
2 Estimation of magnesium content in Talcum powder by complexometry, using s tandardized
solution of EDTA
3 Determination of COD of water sample.
4 To determine potassium content of a Fertilizer by Flame Photometry (Calibration curve
method).
5 To determine the amount of persulphate in the given sample solution by back titration with
standard Fe (II) ammonium sulphate solution.
6 To determine the amount of sulphate in given water sample turbidimetrically.
Note: Calculation of percent error is expected for all the
experiments.
Page 6
REFERENCES
1. Vogel’s Textbook of Quantitative Chemical Analysis, 5thEdn., G. H. Jeffery, J Bassett, J
Memdham and R C Denney, ELBS with Longmann (1989).
2. Vogel's Textbook of Quantitative Chemical analysis, Sixth edition, J.Mendham et.al
SEMESTER V I
ANALYTICAL CHEMISTRY
COURSE CODE: USCH604 CREDITS: 02 LECTURES: 60
UNIT I : ELECTRO ANALYTICAL TECHNIQUES (3 & 6 UNITS)
1.1 Polarography (Numerical and word problems are expected) 11L
1.1.1 Difference between potentiometry and voltammetry, Polarizable and
non-polarizable electrodes
1.1.2 Basic principle of polarography
H shaped polarographic cell, DME (construction, working,
advantages and limitations)
1.1.3 DC polarogram: Terms involved - Residual current, Diffusion
current, Limiting current, Half -Wave Potential
Role and selection of supporting electrolyte , Interference of oxygen
and its removal , polarographic Maxima and Maxima Suppressors
Qualitative aspects of Polarography: Half wave potential E 1/2,
Factors affecting E 1/2
Quantitative aspects of polarography: Ilkovic equations: various
terms involved in it (No derivation)
1.1.4 Quantification
1) Wave height – Concentration plots ( working
plots/calibration)
2) Internal standard (pilot ion) method
3) Standard addition method
1.1.5 Applications advantages and limitations
1.2
Amperometric Titrations 04L
1.2.1 Principle, Rotating Platinum Electrode(Construction, advantages
and limitations)
1.2.2 Titration curves with example
1.2.3 Advantages and limitations
Page 7
UNIT I I: METHODS OF SEPARATION - II (3 & 6 UNITS)
2.1 Gas Chromatography (Numerical and word p roblems are e xpected ) 09 L
2.1.1 Introduction, Principle , Theory and terms involved
2.1.2 Instrumentation: Block diagram and components, types of c olumns ,
stationary phases in GSC and GLC, Detectors: TCD, FID, ECD
2.1.3 Qualitative, Quantitative analysis and applications
2.1.4 Comparison between GSC and GLC
2.2 Ion Exchange Chromatography 06 L
2.2.1 Introduction, Principle.
2.2.2 Types of Ion Exchangers , Ideal properties of resin
2.2.3 Ion Exchange equilibria and mechanism, selectivity coefficient and
separation factor
Factors affecting separation of ions
2.2.4 Ion exchange capacity and its determination for cation and anion
exchangers.
2.2.5 Applications of Ion Exchange Chromatography with reference to
Preparation of demineralised water, Separation of amino acids
UNIT III:FOOD AND COSMETICS ANALYSIS (6 UNITS)
3.1 Introduction to food chemistry
10 L
3.1.1 Food processing and preservation:
Introduction, need, chemical methods, action of chemicals(sulphur
dioxide, boric acid, sodium benzoate, acetic acid, sodium chloride
and sugar) and pH control
Physical methods (Pasteurization and Irradiation)
3.1.2 Determination of boric acid by titrimetry and sodium benzoate by
HPLC.
3.1.3 Study and analysis of food products and detection of adulterants
1) Milk:
Composition & nutrients, types of milk (fat free, organic and lactose
milk)
Analysis of milk for lactose by Lane Eynon’s Method
Page 8
2) Honey:
Composition
Analysis of reducing sugars in honey by Coles Ferricyanide method
3) Tea:
Composition, types (green tea and mixed tea)
Analysis of Tannin by Lowenthal’s method
4) Coffee:
Constituents and composition, Role of Chicory
Analysis of caffeine by Bailey Andrew method
3.2 Cosmetics 05 L
3.2.1 Introduction and sensory properties
3.2.2 Study of cosmetic products –
1) Face powder:
Composition
Estimation of calcium and magnesium by complexometric titration
2) Lipstick:
Constituents
Ash analysis for water soluble salts: borates, carbonates and zinc
oxide
3) Deodorants and Antiperspirants:
Constituents, properties
Estimation of zinc by gravimetry
UNIT IV :THERMAL METHODS AND ANALYTICAL METHOD VALIDATION
(6 UNITS)
4.1 Thermal Methods 12 L
4.1.1 Introduction to various thermal methods
(TGA, DTA and Thermometric titration)
Page 9
4.1.2 Thermogravimetric Analysis(TGA)
Instrumentation -block diagram,thermobalance (Basic components:
balance, furnace, temperature measurement and control, recorder)
Thermogram (TG curve)forCaC 2O4..H2O and CuSO 4.5H 2O
Factors affecting thermogram -Instrumental factors and Sample
characteristics
Applications :
Determination of drying and ignition temperature range
Determination of percent composition of binary mixtures
(Estimation of Calcium and Magnesium oxalate)
4.1.3 Differential Thermal Analysis (DTA):
Principle , Instrumentation, and Reference material used
Differential thermogram ( DTA curve) CaC 2O4 .H2O and
CuSO 4.5H 2O
Applications
Comparison between TGA and DTA.
4.1.4 Thermometric Titrations – Principle and Instrumentation
Thermometric titrations of :
1) HCl v/s NaOH
2) Boric acid v/s NaOH
3) Mixture of Ca+2 and Mg+2 v/s EDTA
4) Zn+2 with Disodium Tartarate .
4.2 Analytical Method V alidation 03L
4.2.1 Introduction and need for validation of a method
4.2.2 Validation Parameters: Specificity, Selectivity, Precision, Linearity,
Accuracy and Robustness
Note: Concept of sensitivity is to be discussed for all techniques
and instruments mentioned in the syllabus.
REFERENCES
1. An Advance Dairy chemistry, V 3, P. F. Fox, P. L. H. McSweeney
Springer Unit/s (3.1,3 .2)
Page 10
2. Analysis of food and Beverages, George Charalanbous, Academic
press 1978 Unit/s (3.1,3 .2)
3. Analytical Chemistry of Open Learning(ACOL),James W. Dodd &
Kenneth H. Tonge Unit/s (4 .1,4.2)
4. Analytical chemistry David Harvey The ,McGraw Hill Compan ies,
Inc. Unit/s (4.1,4 .2)
5. Analytical Chemistry, Gary.D Christan, 5th edition Unit/s (2.1,2 .2)
6. Analytical chemistry, R. K. Dave. Unit/s (2.1,2 .2)
7. Chemical methods of separation, J A Dean, Van Nostrand Reinhold,
1969 Unit/s (2.1,2 .2)
8. Egyankosh.ac.in/bitstream/123456789/43329/1/Unit -8 Unit/s ( 1.1,1.2,1 .3)
9. Food Analysis, Edited by S. Suzanne Nielsen, Springer Unit/s (3.1,3 .2)
10. Food Analysis: Theory and practice, YeshajahuPomeranz, Clifton E.
Meloan, Springer Unit/s (3.1,3 .2)
11. Formulation and Function of cosmetics, Sa Jellineck Unit/s (3.1,3 .2)
12. Fundamentals of Analytical Chemistry, D .A. Skoog and D. M. West
and F. J. Holler Holt., Saunders 6th Edition (1992) Unit/s (2.1,2 .2)
13. Government of India publications of food drug cosmetic act and rules. Unit/s (3.1,3 .2)
14. Harry’s Cosmetology, Longman scientific co. Unit/s (3.1,3 .2)
15. High Performance Thin Layer Chromatography in Food analysis, by
Prem kumar, CBS Publisher and distributer Unit/s (3.1,3.2)
16. Instrumental methods Of Analysis, by Willard Merritt Dean,
7thEdition, CBS Publisher and distribution Pvt Ltd Unit/s (1.1,1.2,1 .3)
(4.1,4.2,4 .3)
17. Introduction to Polarography and Allied Techniques, By Kamala
Zutshi, New Age International, 2006. Unit/s (1.1,1.2,1 .3)
18. Modern cosmetics, E. Thomessen Wiley Inter science Unit/s (3.1,3 .2)
Page 11
19. Principles of Instrumental Analysis , 5th Edition, By Skoog, Holler,
Nieman Unit/s (4.1,4.2,4 .3)
20. Principles of Polarography by Jaroslav Heyrovský , Jaroslav Kůta, 1st
Edition, Academic Press, eBook ISBN: 978148326478 Unit/s (1.1,1.2,1 .3)
21. Solvent extraction and ion exchange, J Marcus and A. S. Kertes Wiley
INC 1969 Unit/s (2.1,2 .2,)
PRACTICALS
SEMESTER V I
ANALYTICAL CHEMISTRY
COURSE CODE: USCHP14 CREDITS: 02
1 Estimation of Chromium in water sample spectrophotometrically by using Diphenyl
carbazide.
2 Estimation of reduc ing sugar in honey by Willstatter method.
3 Estimation o Mg+2 & Zn+2 by anion exchange resin.
using an anion exchange resin
4 Estimation of acetic acid in Vinegar sample by using Quinhydrone electrode
potentiometrically.
5 Determination of phosphoric acid in cola sample pH metrically.
Note: Calculation of percent error is expected for all the
experiments.
Refer ences:
1. Vogel’s Textbook of Quantitative Chemical Analysis, 5thEdn., G. H. Jeffery, J Bassett, J
Memdham and R C Denney, ELBS with Longmann (1989).
Page 12
2. Vogel's Textbook of Quantitative Chemical analysis, Sixth edition, J.Mendham et.al
3. The chemical analysis of food and food products III edition Morris Jacob
4. The chemical analysis of food by David Pearson and Henry Edward