Instrumental Methods of Analysis

CHEM F313

Instructors:
Prof. Anupam Bhattacharya & Prof. Jayanty Subbalakshmi (IC)
 Evaluation Scheme: Total 200 marks

A. Theory (150 Marks that is 75%)

Components Duration Weightage Date & Time Remarks

Mid-Sem 1.5 h 30% 21-10-2021 Open Book

Quizzes --- 10% Continuous

18-12-2021
Comprehensive Examination ** 3h 35% Open Book
(Forenoon)
* There will be 4 quizzes, each carrying 5 marks.
** The midsem and comprehensive examination can have objective and descriptive portions.
B. Practical (50 Marks/25% Weightage OB)
There will be ten regular experiments: Each experiment shall carry 5 marks with total of 50 marks.

Text Books:
T1. Gary D. Christian, “Analytical Chemistry”, 6th ed., John Wiley & Sons (Asia) Pvt. Ltd. Singapore (2003).
T2. Kemp W, “Organic Spectroscopy”, 3rd ed., Palgrave, New York (1991).
Reference Books:
R1. Lampman G.M., Pavia D.L., Kriz G.S., and Vyvyan J.R., “Spectroscopy”, 4th Edition, Cengage Learning (2010).
R2. Silverstein R. M., and Webster F. X., “Spectrometric Identification of Organic Compounds”,6th Edition, John Wiley & Sons, New York (1998).
R3. Willard H. H., Merritt L. L., Dean J. A., and Settle F. A. Jr., “Instrumental Methods of Analysis”, 7th Edition. Wadsworth, New York (1989).
R4. Kalsi P. S., “Spectroscopy of Organic Compounds”, 6th Edition, New Age International Publishers, New Delhi (2005).
 Atomic Spectrometric Methods

Atomic Absorption Spectroscopy (AAS)

and
Atomic Emission Spectroscopy (AES)

Purest and simplest form of matter: Atom

Cannot vibrate or rotate. Only electronic transitions happen when energy is absorbed by the atom.
AES: Intensity of the emitted radiation is directly proportional to the concentration

AAS: Absorbance is measured and the concentration is related to the signal by Lambert-Beer law
➢ What is the difference between molecular spectroscopy and atomic spectroscopy?

Molecular spectroscopy is a subject of quantum physics: excitation of molecular

movement, vibration or excitation of electron in higher -orbitals (UV-Vis) is possible in
general surrounding. In atomic spectroscopy its electronic transition in atom.

➢ Term symbols

Representation of energy states

➢ Maxwell-Boltzmann distribution Law

For understanding the population distribution

 Atomic Spectroscopy
➢ Principle – Energy level diagram

➢ Source & Flames

➢ Atomizers

➢ Monochromators (wavelength separators)

➢ Interferences – Spectral, Chemical & Physical

➢ Sensitivity & Detection limit

➢ Internal standard and standard addition calibration

 Atomic Spectroscopy
• Atom consists of nucleus surrounded by electrons
• When energy of right magnitude is applied to an atom, the electrons in the
ground state absorbs energy to shift to higher electronic, state also known as
the excited state.
• Since excited state is less stable, the atom will spontaneously return to the
ground state configuration.
• Energy absorbed initially is emitted back, generally as light.
 Atomic Emission Spectroscopy (AES)
➢ Also known as flame photometry

➢ Atoms can be excited to the higher energy levels by providing thermal energy. Upon
returning to the ground state, an atom would emit it’s characteristic light that can be
used to qualitatively and quantitatively analyze it.

➢ Simple electronic transitions possible; with no vibrational and rotational energy levels
possible. Bandwidth much narrower!

➢ Occur at discreet λ.