Advanced Mass Spectrometry

CHM 5938 (3) [Core Analytical Course]

Department of Chemistry

Florida International University

 

Instructor: Dr. Piero R. Gardinali       Office:        CP-328  (305) 348-6354

                                                          Lab:             CP-348  (305)348-6249  

                                                          e-mail:          gardinal@fiu.edu

Office Hours; Tuesdays 2:00- 4:00 PM

 

Class Meets:  Monday and Wednesday 17:00 - 18:15  OE-102

 

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)

 

MIDTERM EXAM               October 10^th 2005 17:00-18:15 PM OE-102

 

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

 

Facilities tours, Demonstrations, Student presentations, Assigned experiments-research

 

Required text (s): None

 

 

Suggested reading material:

 

Books

 

Edmond De Hoffmann and Vincent Stroobant , Mass Spectrometry : Principles and Applications ; 2^nd Edition(2001). John Wiley & Sons; New York, USA. ISBN: 0471485667

QD96.M3 H6413 2001

 

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

QD96.M3 R67 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%        October 10^th 2005 17:00-18:15 OE-102

Final Exam                                             30%        December 14^th 15:30 – 18:15 OE-102

Paper/Presentation*                            15%        TBA

Assignments                                        15%        3 Times a semester

Paper Review                                        10%        1 time during the semester

 

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

 

 

 

Presentation: A 10 minute presentation on a “NOVEL” mass spectrometry topic is required.  Alternatively, a term paper (10 pages double space) on a  “NOVEL” mass spectrometry topic could be selected. 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.

 

Assignments are due a week from the day they are provided, at the beginning of the class period. No late submissions!

 

Once a semester, for the first 5 minutes of class, you will be asked to present a review of a research article that I will assign. You are required to provide a summary and a constructive critique on the topic to your classmates to start discussion on the topic.

 

IMPORTANT DATES:

 

NO-CLASSES                       September 5 (Memorial Day),

November 14 and 16 (SETAC);

 

DROP                                     November 3

 

LAST DAY OF CLASS       December 8

 

TERM PAPER DUE             December 7

 

FINAL EXAM                      December 14, 2005. OE-102 15:30 – 18:15.