Details of ID4201 (Spring 2014)

Level: 4 Type: Theory Credits: 3.0

Course CodeCourse NameInstructor(s)
ID4201 Physical methods of Structure Elucidation Arindam Mukherjee,
Chilla Malla Reddy,
Swadhin Kumar Mandal

Preamble
This course provides a comprehensive idea about the different spectroscopic methods of structure elucidation. Since spectroscopy is applicable to chemistry, physics, biology as well as earth science, hence this is considered as an ID course.

Syllabus


  • Mass spectroscopy: Introducing Mass Spectrometry; Ionization methods; Mass analyzers; Identifying the molecular ion; The nitrogen rule; Exchangeable hydrogen; Fragmentation pathways; analysis based on ion-molecule chemistry; acidity, basicity, and energy considerations; scope and limitations of different types of mass spectrometry with examples; Mass Spectrometry (LCMS, GCMS) as analytical detector; interpreting mass spectral data for different compounds and understanding fragmentation pattern.

  • Mossbauer spectroscopy: Introduction to Nuclear fluorescence, Lamb-Mossbauer effect, Doppler shift in Mossbauer Spectroscopy, sources in Mossbauer Spectroscopy, Mossbauer Spectroscopy of $^ 57 $Fe; chemical shift, quadrupole and hyperfine splitting in Mossbauer Spectroscopy. Examples of few iron compounds to probe chemical environment and oxidation states- including iron fluorides and mononuclear $^ 57 $Fe complexes.

  • NMR spectroscopy: Review of principles; spins and lattice; master equations and approach to equilibrium; pulses; vector diagrams; spin echo; brief intro on density matrices; product operator formalism; an intro to 2D. 1H NMR analysis, 13C NMR analysis, 31P NMR spectra of specially transition metal compounds, dynamic NMR spectroscopy, 2D NMR analysis.

  • X-ray crystallography: Basic Theory, Introduction, history, periodicity in crystals, geometric principles of diffraction, Miller indices of the atomic planes in a crystal, Bragg's law, the reciprocal lattice, Bragg's law in reciprocal space, atomic scattering factor, Ewald sphere, number of measurable reflections, the generalized unit cell, asymmetric unit, unit-cell dimensions, crystal faces, unit-cell symmetry, symmetry operations, space groups, phase problem,A quick look at some important terms and definitions: Friedels law, structure factor, systematic absences, twinning, disorder, crystal nucleation and growth.

    The Demonstration of the Method in the XRD Laboratory Flow chart of the single crystal XRD method, brief introduction to the XRD instrument, safety, types of diffraction techniques, X-ray sources, crystal mounting, detectors, centering, unit cell determination, data collection, absorption correction, integration, structure solution and refinement, presenting and interpreting the results (with brief introduction on ORTEP, CIF, CSD, IUCr Journals etc.)


References


  1. The Basics of Crystallography and Diffraction by C. Hammond, Oxford University Press, USA, (2001).

  2. Crystal Structure Determination by William Clegg, Oxford University Press, USA, (1998).

  3. Mossbauer Spectroscopy and Transition Metal Chemistry by P. Gutlich, R. Link, A. Trautwein, Springer, (2013).

  4. Introduction to Mass Spectrometry: Instrumentation, Applications and Strategies for Data Interpretation 0004 Edition by O. David Sparkman, John Wiley & Sons, (2007).

  5. Mass Spectrometry by P. Sethi, Campus Books International, (2011).

  6. Organic Spectroscopy, 3rd Edition by W. Kemp, Macmillan, (2011).

  7. NMR: The toolkit by Peter Hore, J. A. Jones, P. J. Hore, Oxford University Press, (2000).



Course Credit Options

Sl. No.ProgrammeSemester NoCourse Choice
1 IP 2 Elective
2 IP 4 Elective
3 MR 2 Not Allowed
4 MR 4 Not Allowed
5 MS 8 Elective
6 RS 1 Elective
7 RS 2 Elective