CY6129: Advanced Methods in Experimental Physical Chemistry

Course Objective: To introduce the student to a number of state−of−the−art advanced research methods in physical chemistry, with regard to both the theoretical foundations and the experimental methods that are necessary to pursue modern experimental research in physical chemistry.

Course Outcomes:

Students should be able to:
Understand and Explain state−of−the−art advanced research methods in physical chemistry
Use and interpret experimental data from sophisticated equipment used in physical chemistry research

Thermal Properties of Chemical Systems: Principle, experimental measurement technique and applications of Differential scanning calorimetry (DSC), Differential thermal analysis (DTA), Thermomechanical analysis (TMA), Thermogravimetric analysis (TGA) and Simultaneous thermal analysis – STA (TGA/DSC). Thermal conductivity: Heat flow meter, Guarded hot plate method, Laser Flash (LFA) and Xenon Flash (XFA) techniques for thermal conductivity and thermal diffusivity measurements.

Transport Properties: Viscosity, glass capillary viscometer, rolling-ball viscometer and rotational viscometer; Rheology, Rheometers to characterize the rheological properties of materials, fluids, melts and solutions.

Electrochemical Methods: Voltammetry of reversible systems (Cyclic Voltammetry and Rotating Disk Voltammetry, Effect of Mass Transport); Mechanism of Electrode Processes (Steady-state Voltammetry, Chronoamperometry, and Chronopotentiometry); Electron-transfer kinetics (Current-overpotential curves, electron-transfer rates from voltammetry, Faradaic impedence).
X-ray diffraction and Rietveld analysis (Phase identification by X-ray diffraction, determination of crystal structure, quantitative phase analysis and small angle scattering). Scattering Methods, Particle Size Analysis (light scattering, intrinsic viscosity, x-ray and neutron scattering), gel permeation chromatography and relationship with particle size; zeta potential.

Examination of morphology of condensed phase using advanced microscopy (Kelvin Probe Microscopy, Environmental SEM, Cryo-TEM, Energy Dispersive X-ray Analysis).

Fluorescence spectroscopy, steady-state and time resolved spectroscopy, fluorescence and confocal imaging. Cavity ring-down spectroscopy, Applications of excimer lasers: reaction dynamics, photodissociation processes, and energies of dissociation; Transition State Spectroscopy and Femtosecond Chemistry, Time−integrated observation of Transition States of chemical reactions, Fast and Ultra−fast laser spectroscopy, Time−resolved spectroscopic observation of

Transition States. Techniques in kinetics of radical reactions in gas phase such as Laser induced fluorescence method.

Experimental Data Analysis, Correlation and Predictive Tools. Inspecting, cleansing, transforming, and modeling the experimental data, data integration. Empirical and semi-empirical formulas, correlations, group contribution methods and computational models for the prediction of experimental data.

Any three out of the six methods/modules (thermal, transport, electrochemical, x-ray diffraction, morphology, spectroscopy) shall be taught along with experimental data analysis-prediction of experimental data.

Suggested Reading Materials: Relevant Chapters from the following Books

Experiments in physical chemistry. Joseph W. Nibler, Carl W. Garland, Keith J. Stine, Judy E. Kim, McGraw-Hill Education, Boston, 2014.

Introduction to Thermal Analysis: Techniques and applications. Michael E. Brown, Springer Netherlands, 2001.

Principles and Applications of Thermal Analysis. Paul Gabbott, John Wiley & Sons, 2008.
Electrochemistry, 2nd Edition (Reprint 2010) by Philip H. Rieger, Chapman and Hall.

Elements of X-ray Diffraction, 3rd Edition. B. D. Cullity and S. R. Stock, Pearson, 2001.

Scanning and Transmission Electron Microscopy: An Introduction. Stanley
L. Flegler, John W. Heckman, Karen L . Klomparens, Oxford University Press, 1993.

Methods in Physical Chemistry. Rolf Schaffer and Peter C. Schmidt. Wiley-VCH, 2012.
Fundamentals of Analytical Chemistry. Douglas A. Skoog, Donald M. West, F. James Holler, Stanley R. Crouch, Cengage Learning, Edition 9, 2013.

Principles of Fluorescence Spectroscopy, J R Lakowicz, Springer, Edition 3, 2006.

Laser Spectroscopy. Basic concepts and Instrumentation. W. Demtroder. Third
edition 2004, Springer international edition.