Year of entry: 2022
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Course unit details:
Analytical Chemistry and Laboratory Techniques
|Unit level||FHEQ level 7 – master's degree or fourth year of an integrated master's degree|
|Teaching period(s)||Full year|
|Offered by||Department of Chemistry|
|Available as a free choice unit?||No|
Molecular spectroscopy, chromatography and mass spectrometry are fundamental to chemical analysis and are important tools in determining the outcome of chemical reactions. In this module, principles and applications of some of the most common techniques will be presented. The primary objective of the module is to present an integrated, coherent discussion of chemical identification using chromatography and a combination of spectra, and to practice this in a modern synthetic chemical laboratory environment working under relevant COSHH and risk assessment protocols.
The unit aims to:
- Explore aspects of the theory of molecular spectroscopy, mass spectrometry and chromatography, as applied in analytical chemistry labs to small molecules.
- Practice the interpretation of spectra and chromatograms, and to integrate 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.
- Undertake laboratory preparation of some organic and organometallic systems, including multi-step synthesis, anhydrous techniques and analyse the outcome of these experiments by relevant spectroscopic methods.
On successful completion of the course students should be able to:
Knowledge and Understanding
- Describe the physical processes employed in chromatography, in terms of adsorption, desorption, the van Deemter A,B and C terms, sample injection, gas flow, liquid flow and eluate detection
- Discuss the nature of chromatographic columns, including normal and reverse phases, and outline procedures for choosing columns and solvent systems
- Identify the main components of commercial GC and HPLC instrumentation, and describe the coupling of mass spectrometric detection to GC and LC methods
- Explain the toxic risk of low concentrations of trace elements
- Identify the advantages and disadvantages of argon plasmas as an optical emission and mass spectrometry source
- Discuss the main sources of signal interference in ICP-OES and ICP-MS and their minimisation
- Describe the basic operating principles of a mass spectrometer and interpret simple mass spectra (parent ions, major fragments) for small molecules
- Describe the basis of Raman scattering and its use as a spectroscopic tool
- Interpret simple pure-compound infrared and Raman spectra on the basis of group modes and fingerprint spectra, and correlate these with other spectroscopic data
- Explain the physical principles of NMR measurements
- Explain the appearance and structure of one- and two-dimensional NMR spectra
- Interpret simple NMR spectra of pure compounds
- Apply 1D and 2D NMR methods to determine molecular structure
- Interpret given sets of multispectral data in a systematic fashion
- Connect theory and practice to find appropriate methods, to collect data and make choices about the appropriate manipulation of that data.
- Undertake independent safety assessments of experiments, and carry out practical work efficiently and professionally.
- Be capable of interpreting and manipulating analytical data from multiple sources and using it to draw conclusions.
- Be able to critically analyse outcomes, research and contextualise your findings and report to a high technical standard.
- Apply relevant analytical methods to identify and characterise molecules
- Perform calculations and data analysis to derive qualitative and quantitative information about molecules
Transferable skills and personal qualities
- Accessing and using databases of spectral information
- Systematic approaches to problem-solving using a range of data sources
- Working in small groups
- Planning experiments
- Time management
- Reporting Skills
- Analytical Skills
|Practical skills assessment||20%|
Oral and written feedback will be given through workshops, tutorials and laboratory write-up feedback. There will also be formative self-assessment exercises on Blackboard, and using software packages (WINTORG and TORGANAL) on the university computer clusters. One experimental write-up is used for formative feedback only.
Feedback on the exam performance will also be provided in line with Departmental policy.
The following textbooks are recommended reading and reference materials.
General (including MS and Chromatography)
- D. C. Harris, Quantitative Chemical Analysis, 8th or 9th Edn., W. H. Freeman, 2010 or 2015.
- D. L. Andrews, Encyclopaedia of Applied Spectroscopy, Wiley, 2009.
- D. H. Williams, I. Fleming, Spectroscopic Methods in Organic Chemistry, 6th Edn., McGraw-Hill, 2007.
- T. D. W. Claridge, High-Resolution NMR Techniques in Organic Chemistry, 2nd Edn., Elsevier, 2016.
- P.J. Hore, Nuclear Magnetic Resonance (Oxford Chemistry Primer Series), 2nd Edn., Oxford University Press, 2015.
- J. W. Akitt, B. E. Mann, NMR and Chemistry: An introduction to modern NMR spectroscopy, 4th Edn., CRC Press, 2000.
- C. E. Housecroft and A. G. Sharp, Inorganic Chemistry, 4th edition.
|Scheduled activity hours|
|Assessment written exam||2|
|Practical classes & workshops||2|
|Independent study hours|
|Alan Brisdon||Unit coordinator|