MSc Chemistry / Course details

Molecular spectroscopy, chromatography and mass spectrometry are fundamental to chemical analysis and are important tools in all areas of chemistry. In this module, further principles and applications of some of the most common techniques will be presented, building upon ideas and concepts developed in the first year. The primary objective of the module is to present an integrated, coherent discussion of chemical identification using chromatography and a combination of spectra, as practiced in modern synthetic and analytical chemistry laboratories. To put these skills in practice in a chemical laboratory environment working under relevant COSHH and risk assessment protocols.

The unit aims to:
• Explore further aspects of the theory of molecular spectroscopy, mass spectrometry and chromatography, as applied in analytical chemistry labs to small molecules.
• Further practice the interpretation of spectra and chromatograms, and the integration of data from multiple methods to identify unknown molecules.
• Practice multispectral interpretation in a supportive workshop setting in order to develop analytical chemistry skills for practical labs and projects.
• Plan, safety assess, undertake and report practical chemistry, including multi-step synthesis, anaerobic reactions, measurement and analysis of the outcome of experiments using relevant separation and spectroscopic methods.
 

Overarching ILOs:
At the end of this module, students should be able to:

1) Explain the principles of operation of NMR and IR spectroscopy, mass spectrometry and 
   chromatography, and describe the chemical information that can be provided by each method;
2) Describe and explain the ways in which NMR and IR spectroscopy, mass spectrometry and 
   chromatography are used by practical chemists for quantitative and qualitative analysis;
3) Apply knowledge of each of the methods to unseen examples, both as isolated techniques 
   and in conjunction, to determine elements of chemical composition;
4) Apply knowledge of each of the methods to devise a suitable analytical strategy for unseen 
   examples, by selecting appropriate methods for quantitative and qualitative chemical analysis.

The module will include the modern theory and practice of:

• Mass Spectrometry (MS)
o Basic operating principles, including methods of generating ions
o Interpretation of mass spectra, with respect to the ionisation method
o High resolution mass spectrometry for determination of molecular formula

• Infrared Spectroscopy (IR) and Raman Spectroscopy 
o Introduction to Raman spectroscopy (theory and practice), and comparison to infrared 
  absorption spectra
o Identification of functional groups in vibrational spectra

• Nuclear Magnetic Resonance (NMR) Spectroscopy
o Nuclear spin and nuclear magnetism
o Fundamentals of NMR measurements and instrumentation
o NMR parameters, including the chemical shift, scalar coupling, relaxation times, and the 
  nuclear Overhauser effect
o Interpretation of one-dimensional NMR spectra, including dynamic effects
o Multiple pulse NMR methods, including relaxation time measurement
o Measurement and interpretation of two dimensional NMR (2D-NMR) spectra

• High Performance Liquid Chromatography (HPLC) and Gas Chromatography (GC)
o Theory of chromatography, from partition equilibrium to the van Deemter equation
o HPLC and GC instrumentation and integration of chromatography with mass spectrometry 
  (e.g. GC-MS, LC-MS)
 

• Accessing and using databases of spectral information
• Systematic approaches to problem-solving using a range of data sources
• Analytical Skills
 

Core text

Ian Fleming and Dudley Williams, Spectroscopy Methods in Organic Chemistry, Springer, 7th Edition 2019.

Essential reading (parts of)

D. C. Harris, Quantitative Chemical Analysis, 8th or 9th Edn., W. H. Freeman, 2010 or 2015. 
P.J. Hore, Nuclear Magnetic Resonance (Oxford Chemistry Primer Series), 2nd Edn., Oxford University Press, 2015.
J. A. Iggo, K. Luzyanin, NMR Spectroscopy in Inorganic Chemistry (Oxford Chemistry Primer Series), 2nd Edn., Oxford University Press, 2020.
J. McCullagh, N. Oldham, Mass Spectrometry (Oxford Chemistry Primer Series), Oxford University Press, 2019.
S. Duckett, B. Gilbert, M. Cockett, Foundations of Molecular Structure Determination (Oxford Chemistry Primer Series), 2nd Edn., Oxford University Press, 2015
Laurence M. Harwood, Tim D. Claridge, Introduction to Organic Spectroscopy (Oxford Chemistry Primer Series), 1st Edn., Oxford University Press, 1996.
Roger G. Linington, Philip G. Williams, John B. MacMillan Problems in Organic Structure Determination A Practical Approach to NMR Spectroscopy, Taylor and Francis, 2015
Mark Weller, Nigel A. Young, Characterisation methods in inorganic chemistry, 2017 (electronic access uncertain) 
Robert M. Silverstein, Francis X. Webster, David J. Kiemle, David L. Bryce, Spectrometric Identification of Organic Compounds, Wiley-Blackwell, 8th Edition 2015.
Donald L Pavia, Gary M Lampman, George S Kriz, James R Vyvyan, Introduction to Spectroscopy, 2014 5th edition (No current electronic access)

Recommended reading (some of)

T.D.W. Claridge, High-Resolution NMR Techniques in Organic Chemistry, 2nd Edn., Elsevier, 2016.
Malcolm Levitt, Spin Dynamics: basics of nuclear magnetic resonance, 2nd edition, 2008.
James Keeler, Understanding NMR Spectroscopy, 2nd edition, 2010 
Harald Günther, NMR Spectroscopy: Basic Principles, Concepts and Applications in Chemistry, 3rd Edition, Wiley, ISBN: 978-3-527-33000-3 (available as ebook)
David W. H. Rankin; Norbert W. Mitzel; Carole A. Morrison, Structural methods in molecular inorganic chemistry, 2013
J. M. Brown, Molecular Spectroscopy (Oxford Chemistry Primer Series), Oxford University Press, 1998.
Organic structures from spectra, L. D. Field, Sternhell, S.; Kalman, J. R. 5th Edn., Wiley, 2013
J. Throck Watson, O. David Sparkman, Introduction to Mass Spectrometry – Instrumentation, Applications and Strategies for Data interpretation, Wiley and Sons, 4th Edition.
Mass Spectrometry Instrumentation Interpretation and Applications Edited by Rolf Ekman, Jerzy Silberring, Ann Westman-Brinkmalm and Agnieszka Kraj. Wiley and Sons 2009. 
Mynard C. Hamming , Norman G. Foster, Interpretation of Mass Spectra of Organic Compounds. Academic Press 1972
Infrared and Raman spectra of inorganic and coordination compounds, Kazuo Nakamoto, 6th edition 2007
Peter J. Larkin, Infrared and Raman Spectroscopy, 2nd edition Elsevier. 
Infrared and Raman spectroscopy Edited by Bernhard Schrader, 1995.
Norman B. Colthup, Lawrence H. Daly, Stephen E. Wiberley, Introduction to Infrared and Raman spectroscopy, Academic Press 1990.
J. Michael Hollas, Modern Spectroscopy, 4th Edition 2003.
An Introduction to spectroscopic methods Edited by F. Scheinmann 1973
Structural methods in inorganic chemistry, E. Ebsworth; David W. H. Rankin; Stephen Cradock, 1991 (No current electronic access)
D.L. Andrews, Encyclopaedia of Applied Spectroscopy, Wiley, 2009 (No current electronic access)
C. N. Banwell, Elaine M. McCash, Fundamentals of molecular spectroscopy, 1994 (No current electronic access)