Separation Science and Mass Spectrometry

Module code: CFS7027-B

Module Aims       

This module will provide you with specialist knowledge in the principles of separation science and mass spectrometry.  This covers: sample preparation, instrumental fundamentals and design, including case studies related to applications in specialist areas and recent advances.

The specialist knowledge is reinforced by the 'hands on' practical component and will include use of the analytical centre instruments, collecting and analysing data, troubleshooting and method development/enhancement.  The practical sessions will also involve following written experimental protocols, working in a small group, and working to deadlines.

Outline Syllabus   

Separation Science:

Module Introduction.  Principles of separation science (chromatography, mobile and stationary phases, differences between HPLC/GC).  Instrumental techniques split into two separate topics: GC & HPLC: GC - Injection (SS, HS, COC, PTV), columns (capillary/packed, stat. phases), mobile phase (He vs N2 vs H2), detection (FID, ECD, NPD, FPD) etc).  HPLC - Apparatus overview, injection, stationary phase, mobile phase, detection.  Sample preparation (solvent extraction, derivatisation methods, pre-concentration, difficult samples, contamination, pure/complex mixtures, degraded).  Method development - how to affect separation, peak shape etc to split to GC & HPLC: GC - stationary/mobile phase consideration, compound volatility, temperature profiling, sample amounts, detection (selectivity and sensitivity).  HPLC - mobile phase (composition, gradients, modifiers, pH), stationary phase (type, particle size, column dimensions, temperature etc all relating to resolution equation), detection (selectivity and sensitivity).  Trouble shooting, peak shapes etc, improving chromatographic resolution.  Other separation methods (ion chromatography, related areas, hyphenated techniques (GC-MS, HPLC-MS, GC-C-IRMS...), high throughput and other techniques (UPLC, fast GC, GCGC).

Mass Spectrometry:

Module introduction.  Principles of mass spectrometry.  Instrument fundamentals.  Ionisation: electron ionisation (EI), chemical ionisation (CI), fast atom bombardment (FAB), electrospray (ESI), matrix assisted laser desorption ionisation (MALDI).  Instrument fundamentals.  Fragmentation and rearrangement (isotope rations, C, CI, Br.., N rule, McLafferty, common fragments), including post-source decay.  Interpretation of data (artefacts and limitations, adducts, contamination, data tools, theoretical rearrangements, example spectra).  MS/MS Chromatography, hyphenated techniques, (GC-MS, LC-MS).  Sample preparation: solvents, derivatisation (TMS, methylation), standards, quantification.  Ohter separation.., MSMS, QTOF.  Recent developments in mass spectrometry.

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