Tentative Syllabus
Chromatography & Mass Spectrometry, Chem 443/6936
Fall 2013
Instructor: Alena Kubatova, Abbott Hall (301), 777-0348
E-mail: alena.kubatova@UND.edu
Lecture: T 9:30–10:45 AM
Laboratory periods: by appointment
Office hours: We 1:00–2:00 AH 301, other times by appointment
Chromatography is still considered to be on of the most frequently used analytical techniques.
However, while a number of users increases the quality and understanding of chromatographic
methods declines. This course will cover theory as well as the practical training in
chromatographic techniques including also fundamentals of mass spectrometric detection.
To enhance interaction and active learning there will be two presentation assignments within
this class. Since the analytical chemistry is a practical science requiring hands on experience,
there will also be two lab assignments, in which students will individually perform practical
measurements and demonstrate their understanding. The lab assignments will replace portion
of the lectures corresponding approximately to 22 h in lab.
Topics Covered
Quantitation and Data Processing
Fundamental concepts and theory of chromatography
Gas Chromatography: Injectors, Detectors, Column Selection
Sample preparation
Mass spectrometry
Ionization sources
Mass Analyzers
Basics of EI interpretation
Liquid Chromatography
Hyphenated techniques GC/MS, LC/MS
Required Materials
Safety goggles, a bound laboratory notebook, and a calculator
Safety Requirement
Prior to the lab our students will be required to complete safety training.
Website Support
Required
Blackboard
Chromacademy at http://www.chromacademy.com
Additional Web Support
LC GC North America http://www.lcgcmag.com/lcgc/
GC troubleshooting http://www.chem.agilent.com/cag/cabu/gcreflib.htm
LC troubleshooting http://www.chem.agilent.com/cag/cabu/lcref.htm
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Tentative Syllabus
Textbooks
Required
Undergraduate Instrumental Analysis, 6th Ed. By J.W. Robinson, E.M. Skelly
Frame, G.M. Frame II Publisher Marcell Decker, ISBN 978024753594
Additional Supporting Literature:
The following materials will be used as a reference through out the course in addition to peer
reviewed papers.
1. Practical HPLC method development by L.R. Snyder, J.J. Kirkland, J.L. Glajch,
Wiley Interscience, ISBN 0-471-00703-X
2. Modern Practice of Gas Chromatography R.L. Grob, E.F Barry,
Wiley Interscience, ISBN 0417-22983-0
3. Split and splitless injection for quantitative gas chromatography concepts, processes,
practical guidelines, sources of error, K. Grob, Weinheim, New York : Wiley-VCH, 2001,
4th ed., ISBN 3527298797.
4. Interpretation of mass spectra, F.W. McLafferty, František Tureček, 4th ed, Mill Valley,
Calif. : University Science Books, IBSN 0935702253.
5. Mass spectrometry : principles and applications, Edmond de Hoffmann, Vincent
Stroobant, 2nd ed, Chichester, England ; Hoboken, NJ : J. Wiley, IBSN 0471485659.
6. Mass spectrometry : principles and applications, Edmond de Hoffmann, Vincent
Stroobant, 3rd ed, Chichester, England ; Hoboken, NJ : J. Wiley, IBSN 9780470033104.
7. Sampling and sample preparation for field and laboratory, ed. J. Pawliszyn,
Comprehensive Analytical Chemistry ed. D. Barcelo, Elsevier, ISBN: 0-444-50511-3
Assignments and Grading
The grading will be based on the percentage distribution and points for individual assignments
specified below.
Letter Grades: A (≥90%), B (89-80%), C (79-70%), D (69-55%), F (<55%)
Number of
activities
Points per
assignment
Total points
possible
% Grade
Preparation/participation
14
3
42
10
Article presentations
2
30
60
15
Lab assignments
2
50
100
25
Midterm Exam
1
100
100
25
Final Exam
1
100
100
25
402
100
Total
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Tentative Syllabus
Deadlines
Sign-up for 1st presentation
Sign-up for 1st lab
1st presentation to be presented by
Submission of the report for 1st lab report
Midterm Exam
Sign-up for 2nd presentation
Sign-up for 2nd lab
2nd presentation to be presented by
Submission of the report for 2nd lab report
Final exam
6-Sep
6-Sep
16-Oct
1-Oct
8-Oct
25-Oct
25-Oct
10-Dec
3-Dec
19-Dec, 9 AM
Presentations
Students are expected to signup and present two 15 min PowerPoint presentations. The topics
will be posted in the assignment section on the blackboard. The signup for the first and second
presentation must be completed within first two and four weeks of the semester beginning,
respectively. The date of the presentation will be selected with respect to the lecture material.
The electronic version of presentation, electronic links to papers presented should be submitted
to the instructor by 4 PM a day prior to the day of presentation. Failure to signup, present
within specified dates, and providing electronic materials on time will results in loss of 5
points per incident.
Evaluation of presentation
Presentation should include:
 reference to the paper presented (title page)
 the reason for presentation
 problem/material discussed in the article
 basics of analytical methods used including introduction to these methods even if not
covered in the article
 factors affecting those methods
 conclusive optimal conditions – their advantages and disadvantages
 critical evaluation of the method by student
The presentation should be presented in a clear comprehensive manner so other students can
learn from it. The questions regarding the presentation may appear in the exams.
Each student should show understanding the material covered. The presentation will be posted
on the blackboard in the form of PDF file.
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Tentative Syllabus
Laboratory Assignments
The laboratory assignments will cover two topics:
1) Beyond user - advanced use of GC
2) Optimization of electrospray conditions with high resolution mass spectrometry
The goal of these labs is to develop background in application of chromatographic - mass
spectrometric methods. So, students not only learn to operate instrumentation, but they will be
able to start from ”scratch” that is starting the instruments and performing initial setup. The
labs will mimic research investigation of optimal analytical conditions and should be reported in
the form of paper for peer reviewed publication.
Labs will be performed upon completion of the safety training by students working in pairs.
The lab reports will consist of the MS Word and MS Excel files and must be submitted by
specified deadline through Blackboard. The Blackboard SafeAssign feature must be used for
verification of independent work. Even though the work will be performed in pairs, the reports
must be independent. The detailed instruction for the labs will be available on Blackboard in a
pertinent lab folder.
Separation Methods in Peer Reviewed Journals
Journal of Chromatography A
Analytica Chimica Acta
Journal of Chromatography B
Journal Analytical and Bioanalytical Chemistry
Journal of Chromatographic Science
Chromatographia
Electrophoresis
Trends in Analytical Chemistry
Journal of Liquid Chromatography and Related Techniques
Journal of Supercritical Fluids
LCGC International
Journal of Separation Science
Disability Statement
If you need accommodations in this course because of a disability, if you have emergency
medical information to share, or if you need special arrangements in case the building must be
evacuated, please make an appointment to discuss these issues with your instructor soon as
possible.
Academic Integrity
Students are expected to display academic honesty as defined in the UND Code of Student Life
(http://sos.und.edu/csl/). Academic dishonesty will result in loss of all points for the graded
material on which the transgression occurred. A second violation will result in a failing grade for
the course.
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