Advanced Mass Spectrometry

CHM 5931 (3) [Core Analytical Course]

Department of Chemistry

Florida International University

Instructor: Dr. Piero R. Gardinali Office: CP-313 (305) 348-6354

Lab: CP-397 (305)348-6235

Class Meets: Tuesday and Thursday 17:00 - 18:15 GC-276

Course Description: The class offers a in depth description of the processes and techniques involved in creating, controlling and measuring elemental or molecular ionic species by mass spectrometry techniques. Topics covered in the course include: Theory of mass spectrometry. Methods of ionization. Instrument Design. Combined Chromatography and Mass Spectrometry. Quantitative aspects of mass spectrometry. Meta-stable ions in mass spectrometry. Recent applications of mass spectrometry techniques (may involve some hands in experiments).

Tentative Class outline:

Introduction to Mass Spectrometry (2 classes)

· The mass spectrum

· Formation of ions

· Multipe Charged Species

· Isotopes

· Metastable Ions

· Elemental composition of Ions

· Apperance of the mass spectrum

Theory of Mass Spectrometry (3 classes)

· Energy States and Ionization

· Formation of Ions

· Theories of fragmentation rates

· Ions lifetimes

· Qualitative Theories

Methods of ionization (3-4 classes)

· Gas-Phase Ionization

· Electron Ionization (EI)

· Chemical Ionization (CI)

· Desorption Chemical Ionization (DCI)

· Negative-ion chemical ionization

· Field Desorption and Ionization

· Field Desorption (FD)

· Field Ionization (FI)

· Particle Bombardment

· Fast Atom Bombardment (FAB)

· Secondary Ion Mass Spectrometry (SIMS)

· Atmospheric Pressure Ionization

· Electrospray Ionization (ESI)

· Atmospheric Pressure Chemical Ionization (APCI)

· Laser Desorption

· Matrix-Assisted Laser Desorption Ionization (MALDI)

Instrumental Design (2-3 classes)

· Inlet systems

· Ion sources

· Mass analyzers (ion separators)

· Detection and recording of spectra

· Complete systems

Combined chromatography and mass spectrometry (3 classes)

· Gas Chromatography/mass spectrometry (GC/MS)

· Liquid chromatography/mass spectrometry (LC/MS)

· Capillary electrophoresis/mass spectrometry (CE/MS)

· Supercritical fluid chromatography/mass spectrometry (SFC/MS)

· Thin-layer chromatography/mass spectrometry (TLC/MS)

· Other applications of mass spectrometry

Quantitative Mass Spectrometry (2 classes)

· Introduction and principles

· Specificity

· Sensitivity and limits of detection

· Calibration and standards

· Selected ion monitoring (SIM)

· Selected reaction monitoring (SRM)

· Isotope dilution

· High-resolution vs. low-resolution

· Accurate mass measurements

· Derivatization

Metastable ions and tandem mass spectrometry (2-3 classes)

· Unimolecular ion dissociation: Metastable ions

· Collision-induced Dissociation (CID)

· Double focusing magnetic sector instruments

· Triple Quadrupole instruments

· Three- and Four-sector instruments

· Hybrid instruments

· Time of flight instruments

· Ion traps

· Fourier transform instruments

· Tandem MS (MSⁿ)

· Applications of MSⁿ

Student presentations - Assigned experiments-reserach

Required text (s): None

Suggested reading material:

Books

Chapman, J.R., Practical organic mass spectrometry: a guide for chemical and biochemical analysis, 2^nd edition (1993) John Wiley & Sons Ltd. England. ISBN 0 471 92753 8 QD272.S6C43 1993.

Johnstone, R.A.W., Mass Spectrometry for chemists and biochemists, 2^nd Edition (1996) Cambridge University Press. USA. ISBN 0 521 42497 6

QD96.M3R67 1996.

Journals

Analytical Chemistry

Organic Mass Spectrometry

International Journal of Mass Spectrometry and Ion Processes

Biological Mass Spectrometry

Mass Spectrometry Reviews

Rapid Communications in Mass Spectrometry

Journal of the American Society for Mass Spectrometry

Grading:

Midterm Exam 30%

Final Exam 30%

Paper/Presentation* 30%

Assignments 10%

*Depending on the number of students in the class a term paper/presentation will be required.

Note on the presentation:

All presentations must be made in Microsoft Power Point or equivalent software (I don't want to endorse anything!) no slides/overheads will be allowed! All final presentations will be compiled and distributed among the students at the end of the class in CD-ROM format.