Course Name : Instrumental Techniques

Code (Credit) : CUTM 2510 (4-2-0)

Course Objectives

• This subject deals with the application of instrumental methods in qualitative and quantitative analysis of samples and provide insight to select instrumentation appropriate to the assessment need.
• This subject is designed to impart fundamental knowledge of the principles and instrumentation of spectroscopic and chromatographic techniques such that  principles central to analytical chemistry are reinforced; an insight into the key methodologies used is gained and critical thinking for interpreting analytical data is developed, 
• This also emphasizes theoretical and practical knowledge of modern analytical instruments that are used for forensic sample testing.

Learning Objectives

• Students will develop the ability to apply calibration curves, internal standards and the method of standard addition as needed for various measurement problems.
• Can use sample data obtained from spectrochemical techniques to calculate unknown concentrations or obtain structural information where applicable.
• Able to describe the various chromatography within this course and analyze a given chromatogram

Course Syllabus

UNIT- I - Spectroscopic Methods:
 Electromagnetic radiations
 General properties of electromagnetic radiations: Wave and Quantum mechanical properties Interaction of EMR with matter
 Electronic spectra and molecular structure
 Internal standards and standard addition calibration methods
 Ultraviolet and visible spectroscopy: Instrumentation and Applications.

UNIT- II - Molecular and Atomic Spectroscopy:
 Infrared Spectroscopy: Molecular vibration, Theory of IR absorption, IR Sources and Instrumentation, FT-IR Applications.
 Raman Spectroscopy: Theory of Raman & FT-Raman spectroscopy, Instrumentation, Applications.
 Instrumentation and Applications of Flame emission spectrometry, Atomic absorption spectrometry and Atomic Fluorescence Spectrometry

UNIT- III - Emerging and Hyphenate Spectroscopy:
 Mass Spectroscopy: Theory, Instrumentation and Applications.
 Inductively coupled plasma-Mass Spectroscopy: Theory, Instrumentation and Applications.
 X-Ray Spectroscopy: Theory, Types, Instrumentation, Applications and Applications.
 Nuclear Magnetic Resonance Spectroscopy: Theory, Instrumentation and Applications.

UNIT- IV - Separation and Detection Techniques
 Introduction to Chromatography: Partition, Adsorption, Ion exchange, Size Exclusion Chromatography, their principle and types of chromatography. Forensic applications of Chromatography.
 Gas Chromatography: Principle, instrumentation and applications. Gas-liquid and gas-solid chromatography, GC – MS, GC – MS – MS (Tandem).
 Gas Chromatography – Head Space: Principle, instrumentation and applications.
 High Performance Liquid Chromatography: Principle, instrumentation and applications, LC
– MS, LC – MS – MS (Tandem)

UNIT- V
General Principles of Biological / Biochemical Analysis
 pH and Buffers, Physiological solution
Centrifugation Techniques
 Basic principle of sedimentation, various types of centrifuges, Density Gradient Centrifugation, Preparative Centrifugation, analysis of sub-cellular fractions, Ultra centrifuge- Refrigerated Centrifuges.
Microscopy
 Basic principles of microscopy, Simple and Compound microscope
 Study of different types of microscopes: Comparison microscope, Phase contrast microscope, Stereoscopic microscope, Polarizing microscope, Fluorescence microscopy, IR microscopy, Scanning Electron Microscope (SEM), Transmission Electron Microscope (TEM)

Practicals
1. Experiments on UV absorption of drug/dyes/Chemicals.
2. Experiments on IR spectroscopy of Paints / Drugs / Organic compounds.
3. Comparison of polythene films by IR spectrophotometry.
4. Identification of drugs / solvents by Gas Chromatography and Gas Chromatography – Mass Spectrometry (GC-MS).
5. Identification and Estimation of Volatile Substances by chemical and Gas Chromatography
– Head Space technique (GC-HS).

Reference Books:
1. D.A.Skoog, F.J.Holler and T.A.Neman, Harcoust Principles of Instrumental Analysis college publishers, Singapore
2. G.D.Christian and J.E.O’Reilly, Instrumental Analysis, Allyn and Bacon, Inc., Boston.
3. F.W.Fifield and D.Kealey, Principles and practice of Analytical Chemistry, International Textbook Company, London.
4. R.P.Bauman, Absorption Spectroscopy, John Wiely, New York.
5. M.Donhrow, Instrumental Methods in Analytical Chemistry; Their Principles and practice Vol.2, optical method, Pitaman, New York.
6. G.G.Guilbanlt, Practical Fluorenscence: Theory, Methods and Practice, Marcel Dekker, New York.
7. S.Udenfriend, Fluorescence Assay in Biology and Medicine, Academic Press, New York.
8. W.J.Price, Spectrochemical Analysis by Atomic Absorption, Hyden, London.
9. R.S.Alger, Electron Paramagnetic Resonance: Techniques and Applications, Interscience, New York.
10. Analytical Chemistry by open Learning, John Wiley & Sons, New York.
11. J.C.Giddings, Dynamics of Chromatography, Marcel Dekker, New York.
12. R.C.Grob, Modern Techniques of Gas Chromatography, Marcel Dekker, New York.
13. J.A.Dean, Chemical Separation Methods, Ban Nostrand Reinhold Co., New York.
14. R.E.Smith, Ion Chromatography Applications, C.R.C. Press, Inc., Boca Raton.
15. R.E.Smith, Supercritical Fluid Technology, C.R.C. Press, Inc., Boca Raton.
16. G.Zweig and J.R.Whitaker, Paper Chromatography and Electrophoresis, Academic Press, New York.
17. Safferstein: Forensic Science Handbook Vol. I, II, III.
18. Lee Honry: An Introduction to Forensic Science
19. Egon Stahl: Thin Layer Chromatography

Session Plan- Theory

Session 1

Electromagnetic radiations

Session 2

General properties of electromagnetic radiations: Wave and Quantum mechanical properties

Session 3

Interaction of EMR with matter

Session 4

Electronic spectra and molecular structure

Session 5

Internal standards and standard addition calibration methods

Session 6

Ultraviolet and visible spectroscopy: Instrumentation and Applications.

Session 7

Infrared Spectroscopy: Molecular vibration, Theory of IR absorption, IR Sources

Session 8

Infrared Spectroscopy: Instrumentation, FT-IR Applications

Session 9

Raman Spectroscopy: Theory of Raman & FT-Raman spectroscopy

Session 10

Raman Spectroscopy: Instrumentation, Applications.

Session 11

Instrumentation and Applications of Flame emission spectrometry

Session 12

Instrumentation and Applications of Atomic absorption spectrometry and Atomic Fluorescence Spectrometry

Session 13

Mass Spectroscopy: Theory, Instrumentation and Applications

Session 14

Inductively coupled plasma-Mass Spectroscopy: Theory, Instrumentation and Applications

Session 15

X-Ray Spectroscopy: Theory, Types, Instrumentation, Applications and Applications

Session 16

Nuclear Magnetic Resonance Spectroscopy: Theory, Instrumentation and Applications.

Session 17

Introduction to Chromatography: Partition, Adsorption, Ion exchange

Session 18

Size Exclusion Chromatography, their principle and types of chromatography

Session 19

Forensic applications of Chromatography

Session 20

Gas Chromatography: Principle, instrumentation and applications. Gas-liquid and gas-solid chromatography

Session 21

GC – MS, GC – MS – MS (Tandem)

Session 22

Gas Chromatography – Head Space: Principle, instrumentation and applications

Session 23

High Performance Liquid Chromatography: Principle, instrumentation and applications

Session 24

LC – MS, LC – MS – MS (Tandem)

Session 25

General Principles of Biological / Biochemical Analysis
pH and Buffers, Physiological solution

Session 26

Basic principle of sedimentation, various types of centrifuges

Session 27

Density Gradient Centrifugation, Preparative Centrifugation

Session 28

analysis of sub-cellular fractions

Session 29

Ultra centrifuge- Refrigerated Centrifuges

Session 30

Basic principles of microscopy, Simple and Compound microscope

Session 31

Study of different types of microscopes: Comparison microscope

Session 32

Phase contrast microscope, Stereoscopic microscope, Polarizing microscope

Session 33

Fluorescence microscopy, IR microscopy

Session 34

Scanning Electron Microscope (SEM)

Session 35

Transmission Electron Microscope (TEM)

Session Plan- Practical

Session 1

Experiments on UV absorption of drug/ dye/ Chemicals

Session 2

Identification of drug/ dye / Chemicals by Thin layer chromatography

Session 3

Comparison of polythene films by IR spectrophotometry.

Session 4

Experiments on IR spectroscopy of Paints / Drugs / Organic compounds

Session 5

Identification of drugs / solvents by Gas Chromatography and Gas Chromatography – Mass Spectrometry (GC-MS).

Session 6

Identification and Estimation of Volatile Substances by chemical and Gas Chromatography – Head Space technique (GC-HS).

Session 7

Identification and separation of dye by Gel Electrophoresis method.