TENTATIVE SYLLABUS CHEM 443
FALL 2015
Chromatography & Mass Spectrometry, Chem 443 9855 (2 credits)
Instructor: Alena Kubatova, Abbott Hall (301), 777-0348
E-mail: alena.kubatova@UND.edu
Lectures: Tuesdays 9:30-10:45 AM
Laboratory periods: Thursdays 9:00 AM -12:00 PM, the lab times are scheduled by appointment, the lab tasks
are scheduled to be completed within a total of ca. 22 h.
Office hours: We 10:00–11:00 AM AH 301, other times by appointment
Chromatographic methods, in particular those coupled with mass spectrometry, are among the most frequently
used analytical techniques. However, while a number of users increases to encompass their broader range, the
understanding of chromatographic methods by these users declines. This course will cover theory as well as the practical
training in chromatographic techniques, also including the essential fundamentals of mass spectrometric detection.
The class is run in a flipped classroom format. That is, students will be expected to prepare using the online
lecture and reading materials as well as some texts available in the library for each ‘lecture session’. They will be
required to bring solved take-home quizzes to lectures, so the answers will be discussed in class. Further, students will
present two presentations. One presentation will be a literature review targeting the analytes and specific
chromatographic method of analysis of the student’s interest (part of the 1st assignment); this presentation will be
preceded by a written document. The second presentation will be a report on the results obtained within the second
lab.
Since 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
of chromatographic methods. The lab assignments will be performed on Thursdays with a lab time expected for
completion of approximately 22 h.
TOPICS COVERED
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Quantitation and data processing
Fundamental concepts and theory of chromatography
Gas chromatography: Injectors, detectors, column selection
Sample preparation
Mass spectrometry
o Ionization sources
o Mass analyzers
o Basics of EI interpretation
Liquid chromatography
Hyphenated techniques, i.e., GC/MS, LC/MS
Ion chromatography, size exclusion chromatography
REQUIRED MATERIALS
A bound laboratory notebook and a calculator
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TENTATIVE SYLLABUS CHEM 443
FALL 2015
SAFETY REQUIREMENT
Prior to any lab work, students will be required to complete the online Chemistry Department Safety training.
Failure to complete the safety training will prevent students from entering the lab, so they cannot complete the
assignments.
WEBSITE SUPPORT
Blackboard: Students are expected to check Blackboard online regularly for announcements and submit all their
work through the blackboard site
Chromacademy: http://www.chromacademy.com This website is essential to follow the required lecture
materials. You will need to register on the Chromacademy website by selecting a tab with free University sponsorship
(do NOT select LITE version on Free membership!!)
Other useful sites:
http://chemwiki.ucdavis.edu/Analytical_Chemistry
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
RECOMMENDED REFERENCE MATERIALS
The following materials will be used as reference throughout the course in addition to pertinent peer reviewed papers.
1. Quantitative Chemical Analysis by Daniel Harris, 8th or 9th edition, Freeman http://bcs.whfreeman.com/qca8e
2. Undergraduate Instrumental Analysis, 6th Ed. By J.W. Robinson, E.M. Skelly Frame, G.M. Frame II Publisher
Marcell Decker, ISBN 978024753594
3. Practical HPLC method development by L.R. Snyder, J.J. Kirkland, J.L. Glajch,
Wiley Interscience, ISBN 0-471-00703-X
4. Modern Practice of Gas Chromatography R.L. Grob, E.F Barry,
Wiley Interscience, ISBN 0417-22983-0
5. 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.
6. Interpretation of mass spectra, F.W. McLafferty, František Tureček, 4th ed, Mill Valley, Calif. : University Science
Books, IBSN 0935702253.
7. Mass spectrometry : principles and applications, Edmond de Hoffmann, Vincent Stroobant, 2nd ed, Chichester,
England ; Hoboken, NJ : J. Wiley, IBSN 0471485659.
8. Mass spectrometry : principles and applications, Edmond de Hoffmann, Vincent Stroobant, 3rd ed, Chichester,
England ; Hoboken, NJ : J. Wiley, IBSN 9780470033104.
9. Sampling and sample preparation for field and laboratory, Ed. J. Pawliszyn, Comprehensive Analytical Chemistry
ed. D. Barcelo, Elsevier, ISBN: 0-444-50511-3
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TENTATIVE SYLLABUS CHEM 443
ASSIGNMENTS
FALL 2015
The assignments will consist of take-home quizzes, and 3 major assignments including two laboratories, which
results will be demonstrated with written papers/ reports and oral presentations.
Home to Take Quizzes
Besides the study of the online lectures and reading materials for each ‘lecture session’ as well as some texts
available in the library, students will need to complete take-home quizzes (handwritten), the answers to which will be
discussed in class. Please note that students are expected to be able to present the answers without reading them.
1st Assignment = Literature Review
Task: Peer reviewed literature search on the application of chromatographic-mass spectrometric methods for
analytes relevant to students’ majors followed by oral and written presentations. The details of the assignment are
provided as a separate document.
As the first task, students will be asked to perform a peer reviewed literature search of the chromatographic
and/or mass spectrometric characterization methods addressing the analytes of student’s choice. The papers are
expected to cover the currently used methods in a similar manner as it is done in introductions of papers published in
analytical chemistry peer reviewed journals. This paper may serve as an introduction to the 2nd lab report. To ensure
collaborative learning, this component will be worked out by teams of students where the first two drafts will be
evaluated by the team of classmates and only the final report will be evaluated by the instructor.
The submission deadlines of drafts and final papers is 4 PM Sep 15, 22, 29. The graduate students will have three
days to submit revisions.
Further, this assignment includes an oral Power Point presentation. Students will be expected to work on the
first presentation/paper in collaboration within groups on Blackboard demonstrating work on, at least, two versions. The
electronic versions of presentation, along with the electronic links to the papers presented should be submitted to the
instructor by 4 PM one day prior to the day of presentation.
Laboratory Assignments
The laboratory assignments will cover two topics:
1) The fundamentals of quantitation in chromatography
2) Application of the selected chromatographic / mass spectrometric method to the selected analytes
The goal of these laboratories is to develop strong background in application of chromatographic - mass
spectrometric methods. Every chemist should have the fundamental understanding of quantitation methods. Thus
training in application of quantification in gas chromatography and mass spectrometry is ensured through the first
laboratory assignment.
Within the 1st lab student will evaluate GC-MS analyses performed in different scanning modes using the
internal standard calibration method applied to selected compounds (selected with the instructor’s approval at least 3
weeks prior to the lab), determine their instrumental limits of quantification for each acquisition mode and validate both
methods based on replicate determination of the targeted compounds in an evaluation sample of a defined (known)
composition.
The topic of the second lab will depend on the student’s selection of analytes (which may be the same as those
targeted in the 1st assignment). It is essential that the equipment to perform experiments must be available - students
need to verify this with the instructor. Students are expected to analyze the analytes in the matrix of interest and
validate the method with a verification of their procedure.
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TENTATIVE SYLLABUS CHEM 443
FALL 2015
The lab reports will consist of the MS Word and MS Excel files and must be submitted by the specified deadline
through Blackboard. All file names should start with the initials of the student (details for labeling are provided in the lab
manual).
The second lab will be completed by oral presentation. Students are expected to sign up and present 10 min
PowerPoint presentations reporting the results obtained in the second lab. The electronic version of this presentation,
as well as the electronic links to the papers presented, should be submitted to the instructor by 4 PM a day prior to the
day of presentation. Failure to sign up, present within specified dates, and/or providing electronic materials on time
will results in a loss of 5 points per incident.
Presentations
Students are expected to signup and present two 10 min PowerPoint presentations. 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 (deadline are specified in timeline below), 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:
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references to the papers presented in the ACS format on the pertinent slides
the motivation for presentation
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 for specific target analytes
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 must show understanding the material
covered. The presentation will be posted on the blackboard in the form of PDF file.
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
13
3
39
1 Assignment Paper/Oral
2
30
60
Lab assignments/reports
2
55
110
2nd Presentation
1
50
30
Midterm Exam
1
120
120
Final Exam
1
250
250
Preparation/participation
st
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TENTATIVE SYLLABUS CHEM 443
Week
Date
Topic
1
25-Aug
Intro to class
2
1-Sep
Data handling and
quantitation
8-Sep
Working with
Scifinder
FALL 2015
Required Preparation
Source
Material
Quant Chem Analysis by
Harris
Calibration: external and internal
standards, limits of detection
Quiz
Assignments
Quiz 1
Selection of the topic for 1st
assignment/approved, sign-up for 1st
presentation
Sign-up for 1st lab/selection of target
analyte
Submission of the 1st lab report (must be
done within 2 weeks of the lab
completion)
3
15-Sep
GC intro
Chromacademy
GC Introduction/Chromatographic
Parameters and Band Broadening
GC Theory of
Instrumentation
Chromatographic Parameters and
Band Broadening
Quiz 2
1st draft of the 1st assignment for review
to the evaluation group
4
22-Sep
GC Injection
GC Theory of
Instrumentation
Sample Introduction
Quiz 3
2nd draft of the 1st assignment for review
by the evaluation group
5
29-Sep
GC column
selection
GC Theory of
Instrumentation
GC columns
Quiz 4
Submission of the final of the 1st
assignment paper
1st assignment oral presentation (send to
the instructor a day before)
1st Presentations
Selection of the topic for the 2nd lab
(provide reference paper) and signup for
the 2nd lab
6
6-Oct
GC detectors
GC Theory of
Instrumentation
GC detectors
Quiz 5
1st Presentations
7
13-Oct
Midterm Exam
Midterm exam
Meet with the instructor to confirm the
approach used in the 2nd lab and schedule
the lab and availability of the equipment
Submission of the 2nd lab report (must be
done within 2 weeks of the lab
completion)
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TENTATIVE SYLLABUS CHEM 443
8
20-Oct
FALL 2015
2D GC
Multidimensional GC
Multidimensional Chromatography
Sample
preparation
Sample Preparation
SPE overview & mechanisms
Quiz 6
1st Presentations
9
27-Oct
GC-MS
MS
Fundamental GC-MS – Introduction
E-learning mod.
Quiz 7
MS
Fundamental LC-MS – Intro, 10 Ways
to Break Your LC-MS.
Quiz 8
1st Presentations
10
3-Nov
LC-MS
2nd presentation to be presented by (send
to the instructor a day before)
2nd Presentations
11
10-Nov
MS instruments &
interpretation
MS
MS interpretation – General
strategies
Quiz 9
LC
Theory of HPLC: Introduction &
Reverse phase
Quiz
10
LC
Theory of HPLC: Normal phase &
Gradient
Quiz
11
2nd Presentations
12
17-Nov
LC Introduction &
Instrumentation
2nd Presentations
13
24-Nov
LC Separation
2nd Presentations
14
1-Dec
LC separation
Instrumentation of HPLC: The mobile
phase
LC
2nd Presentations
15
8-Dec
LC detectors
Theory of HPLC: Ion
chromatography
Ion and size exclusion
chromatography
LC
Instrumentation of HPLC: Detectors
2nd Presentations
15-Dec
Final Exam
Quiz
12
10:15 AM-12:15 PM
6
Quiz
13
Syllabus Chem 443
Tentative Detailed Lecture Outline
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://und.edu/student-affairs/code-of-student-life/index.cfm. Academic dishonesty will result in a 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.
NON-DISCRIMINATION STATEMENT
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with Title IX of the Education Amendments, which prohibits discrimination and harassment based upon sex in an
institution’s education programs and activities. Title IX prohibits sexual harassment, including sexual violence, of
students at UND-sponsored activities and programs whether occurring on-campus or off-campus. Title IX also protects
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protects employees from sexual harassment and discrimination. Prohibited harassment includes acts of verbal,
nonverbal or physical aggression, intimidation or hostility based on sex, even if those acts do not involve conduct of a
sexual nature; sex-based harassment by those of the same sex; and discriminatory sex stereotyping. UND will take
prompt action to investigate and resolve reports of sexual harassment or sexual violence in accordance with Title
IX. UND’s Title IX coordinator is Donna Smith, Director of Equal Employment Opportunity/Affirmative Action, 401
Twamley Hall, 264 Centennial Drive Stop 7097, Grand Forks, ND 58202-7097, 701-777-4171,
donna.smith@und.edu. Retaliation against any person who initiates an inquiry or complaint or participates in the
investigation of a complaint is prohibited. Such conduct will be further cause for disciplinary action.
Brief Information about Reporting
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stalking) or gender-based misconduct is encouraged to report and seek appropriate resources on campus. Please
contact the Title IX Coordinator (Donna Smith, donna.smith@und.edu or 701-777-4171) to discuss your options. To
view the policy and additional resources, please visit: http://und.edu/finance-operations/university-police/sexualviolence-programs.pdf.
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