Advanced Analytical Chemistry

SC-504

Semester-V

Contents:

Sr. No Topic Hours

1 Classical approach for aqueous and solid phase extraction 12 Hrs

2 Solvent extractions. 15 Hrs

3 Chromatography. 15 Hrs

4 Mass spectrometry. 6 Hrs

5 Hyphenated techniques. 6 Hrs

6 Electrophoresis. 7 Hrs

7 Atomic Spectroscopy 12 Hrs

8 Atomic Mass Spectroscopy 6 Hrs

No Chapter Hours
Classical approach for aqueous and solid phase extraction:

Aqueous phase extraction: Introduction, Liquid-Liquid extraction (LLE) (Theory of LLE, selection of solvents,

solvent extraction, problems with LLE process), purge and trap for volatile organics in aqueous samples

1 Solid Phase extraction: Introduction, Types of SPE media, SPE formats and apparatus, method for SPE 12 Hrs

operation, solvent selection, factors affecting SPE, selected methods of analysis for SPE, Automation and On-Line

SPE

Solvent extractions:

The distribution coefficient, distribution ratio, relation between KD & D, the percent extracted. Solvent

extraction of metals – ion association complexes, metal chelates, effect of pH and reagent concentration,

extraction process, separation efficiency of metal chelates, analytical separations – multiple counter current

distribution, solid phase extraction, solvent extraction of flow injection analysis. Super critical fluid extraction.

2 Organic reagents in Inorganic analysis:- Theoretical basis for the use of organic reagents in inorganic 15 Hrs

analysis. Extraction of metal ions by the use of organic reagents – acetylacetone, thionyl- trifluoroacetone, tri-n-

octyl phosphine oxide. Applications to extractions of metal ions by chelating agent (Dithiazone, 8-hydroxy

quinoline and cupferron) Determination of salts of organic acids and bases, determination of alkaloids in crude

drugs.

Chromatography:

3 HPTLC: Principle, Technique, advantages over TLC 15 Hrs

Gas Chromatography(GC)– Theory, Data acquisition and processing Applications Derivatization techniques.
 Monitoring of ethylene dibrombide (EDB) residue in Indian Black pepper by GC using electron capture

detector. Analysis of petroleum products. Headspace analysis of tobacco. Preparative gas chromatography

High Performance Liquid Chromatography (HPLC)– Theory, and separation modes, Applications with

respect to separation of enantiomers, Organic and inorganic systems.

Supercritical fluid chromatography (SFC)– Instrumentation of SFC, stationary and mobile phases used in

SFC, Detectors, Advantages of SFC. Technique and applications of SFC.

Size Exclusion Chromatagraphy: Principle of Gel Chromatography, Filtration Chromatography,

Instrumentation, retention behaviour, resolution, selection of gel type – applications.

Ion Exclusion – Principle and applications.

Ultra Performance Liquid Chromatography: Principle, Instrumentation

Mass Spectrometry:

Advanced Mass spectrometry Quadruple analysers, Ion traps. Time of flight mass spectrometry. Mass
4 06 Hrs
Spectrometry/ Mass Spectrometry Tandem Mass Spectrometry. Ion cyclotron resonance spectrometers and Ion

traps for MS/MS. Quantitative mass spectrometry: Introduction, principle, calibration and internal standards.

Hyphenated techniques:

GC-MS: Principle, instrumentation, Interfaces, Mass analyzer, Mass chromatogram, Applications. Analysis of

metabolite of drug Imipramine.

5 GC-FT-IR: Principle, Instrumentation and Applications LC-MS: Principle, Instrumentation, Interfaces and 06 Hrs

Applications.

LC-MS-MS: Principle, Instrumentation, Interfaces and Applications.

ICP-MS: Instrumentation, principles, Quantitative analysis and applications.

Electrophoresis

6 Introduction, Definition 07 Hrs

Paper Electrohoresis: Principle, Experimental Requirements, Technique, Factors governing the migration of
 ions, Applications

Capillary Electrophoresis: Electro osmotic flow, migration in CE, instrumentation, control of separation,

applications

Gel Electrophoresis: Principle, technique, applications

Immuno electrophoresis: Principle, technique, applications

Atomic Spectroscopy:

Theory, sources, burners, atomic emission spectra, atomic absorption spectra, effect of temperature on emission,

absorption and fluorescence, electro thermal atomizers, Instrumentation for FES, radiation sources atomic

absorption methods, instrumentation for AAS, spectral interferences, standard addition and internal standard
7 12 Hrs
method of analysis, comparison of atomic absorption and emission methods, inductively coupled plasma and

direct current plasma emission spectroscopy, Cold vapor technique, Applications of AAS, AES and ICPAES,

analysis of micronutrients like Mo, B, Cu, Zn essential towards the healthy growth of crops, fruits, determination

of these micronutrients from soils, plants and fruits.

Atomic Mass Spectroscopy:

Features of atomic mass spectroscopy, Atomic weight in mass spectroscopy, mass to charge ratio, Types of

8 atomic mass spectroscopy, mass spectrometers, transducer for mass spectroscopy, qudrapole mass analyzer, time 6 Hrs

of flight mass analyzer, Inductively coupled mass spectroscopy (ICPMS), Instrumentation for ICPMS, Atomic

mass spectra and interferences, Applications of ICPMS,

References:
1) Separation Methods - M. N. Sastri, 1st ed., Himalaya Publishers, 1991.
2) Principles of Instrumental Analysis, Skkog, Holler, Nieman, (Sixth Ed.)
3) Analytical Chemistry - Gary D. Christian, 6th ed, John Wiley and sons. Inc., New York, sixth
edition, 1994.
4) Mass spectrometry for Chemists and Biochemists, Robert A.W. Johnstone and Macolm. E.
Rose, 2th ed Cambridge University Press 1996.
5) Structural methods in Inorganic chemistry - E.A.V. Ebsworth, et al ELBS Publications, 1988.
6) Introduction to analytical Gas Chromatography, Raymond PW Scott, 2nd Ed. Marcel Dekker,
Inc. New York,1988.
7) Techniques and practice of Chromatography, Raymond PW Scott, Marcel Dekker, Inc. New
York,1995.
8) Extraction technique in analytical science, John R. Dean, Wiley (2009).
9) Liquid Chromatography-Mass Spectrometry Principles & Applications, WMA Neissen & JV
Greef, Marcel Dekker, Inc. New York,1992.
10) Vogel’s Textbook of Quantitative analysis 6th Ed.
11) Practical HPLC method Development, Snyder, Kirkiand, Glajch, Wiley India Pvt. Ltd.