Tentative Syllabus syllabus_543_2013_19578.doc

Chromatography & Mass Spectrometry, Chem 543/19578

Fall 2013

Instructor: Alena Kubatova, Abbott Hall (301), 777-0348

E-mail:

Lecture: T/Th 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 three 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, all 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

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 / 3 / 30 / 90 / 21
Lab assignments / 2 / 50 / 100 / 23
Midterm Exam / 1 / 100 / 100 / 23
Final Exam / 1 / 100 / 100 / 23
Total / 432 / 100

Deadlines

Sign-up for 1st presentation / 6-Sep
Sign-up for 1st lab / 6-Sep
1st presentation to be presented by / 16-Oct
Submission of the report for 1st lab report / 1-Oct
Midterm Exam / 8-Oct
Sign-up for 2nd presentation / 18-Oct
Sign-up for 2nd lab / 25-Oct
2nd presentation to be presented by / 8-Nov
Sign-up for 3rd presentation / 15-Nov
Submission of the report for 2nd lab report / 3-Dec
3rd presentation to be presented by / 12-Dec
Final exam / 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.

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 individually

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. 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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