VERSION: 22 AUGUST 2013

FRNSC 831/ CHEM 525/ BMMB 525 Forensic Chemistry II/ Analytical Separations

Welcome to a course that goes by many names: FRNSC 831, CHEM 525, and BMMB 525. These courses are specifically known as Forensic Chemistry II, or Analytical Separations, depending on which department you are coming in from. I’ll be the instructor for this course (Frank Dorman).

Our Course Goals: Many scientists in various analytical settings across the globe use gas and liquid chromatographic separations, as well as others, as the critical step in the identification and quantification of trace organic compounds. Unfortunately most of these practicing chromatographers view the techniques that they use as little more than “black boxes” and really do not understand how these techniques truly operate. The goal of this course is two-fold: First, to gain a solid fundamental understanding of modern separation science and the more common techniques employed in analytical laboratory settings. Second, you should be able to use this understanding to teach others, and act as an “expert” in your area of science, both to other chromatographers, and also to non-scientists.

________________________________________________________________________ Contact Information:

Frank L. Dorman, 107 Whitmore Laboratory, [email protected], 863-6805 Office Hours: By appointment and made through Missy Thomas, [email protected] You may also check at my research labs in 347, 344a, 320 and 434 Davey Labs

Learning Philosophy:

Learning is not effective if it is passive. Both the instructor and the students need to actively participate in the course, and this requires communication in both directions. I have planned to cover a large amount of material, both in a formalized lecture, and also suggested outside readings. Please plan to be engaged and “pull” for more information and clarification. You should also feel invited to push the course and the instructor into additional or different areas of interest as long as they fit into the general theme of this course. A percentage of your final grade will be from a subjective assessment of your level of participation throughout the course. Let’s all become more knowledgeable as separations scientists together!

Exams and Grading:

Exams will consist of three equally weighted exams as scheduled below. Exam material will be taken from text, lecture, and outside literature cited, not just concepts covered in the lectures alone. In addition to the three exams, there will be a presentation from each student during the term. The presentation will be a literature review on a current technique or topic that is to be presented to the class as instructional.

Exam #1 27% Exam #2 27% Exam #3 27% Student presentation 14% Participation factor 5% Total 100% Exam Policy:

Other than unexpected illnesses, all requests for a makeup exam must be made by email to Dr. Dorman no later than two weeks prior to the scheduled exam. If an unexpected illness keeps a student from attending the exam, an email must be sent to Dr. Dorman prior to the class period in order for the student to be allowed to take a makeup exam. NOTE: Makeup exams may be harder than the scheduled exam, so plan accordingly and stay healthy! J

The exams will be a combination of short answer and multiple choice/True and False. Students should practice both verbalizing and writing out their understanding of the course material. Using each approach will help in their preparation for the exams. The exams will be open-resource, take-home format and will be designed to evaluate the student’s ability to apply the material covered in the course, and not merely to determine if the student is able to regurgitate the information. In this regard, it is likely that the exams will require extension of the course material, and may also require problem solving not directly covered as examples in the lecture itself. In other words, reference materials will likely need to be consulted in addition to the lecture notes and text itself.

The Student Presentation:

Each student will be given a currently relevant topic in the area of analytical separations. Each student will prepare to cover a 25-minute lecture period (2 students per period) where you should plan for 20 minutes of formalized lecture, with some time for questions. Your goal is to teach the class about your topic. You may use any medium available (blackboard, overhead, PowerPoint, handouts, etc…) the delivery of the content will not count as much as the content itself. Keep in mind that the level of this

presentation is to analytical chemistry-focused graduate students, and should be rigorous. The grades will, in-part, be determined from peer evaluation. Each presenter will also provide an exam question to the instructor, prior to their presentation, which is intended to gauge the other students understanding of the topic for possible inclusion on an upcoming exam. Presentations will occur throughout the term, typically at the

beginning of lecture periods. Topics are to be determined by each student in consultation with the instructor, but a list of possibilities will be distributed. There is an advantage to choosing you topic early, and the choice of topic does impact when will be appropriate for you to give the presentation. These will, therefore, be scheduled as the topics are chosen, and as we move through the term.

This semester, we will meet:

Monday, Wednesday and Friday 1:25PM – 2:15PM, 205 Ferguson Bldg Required Text:

C. F. Poole, The Essence of Chromatography. Elsevier, Amsterdam, 2003. ISBN:0444501991

Additional resources, Citations given in the course are expected to be read and understood. These are all available through the PSU library system, Angel and as handouts during the course, depending on the reference.

Learning Objectives: Achieved through lectures, recitation sessions and your hard work, and assessed through exams, Presentations and class participation

PLEASE READ THE LEARNING OBJECTIVES

Ø General Concepts in Column Chromatography

Family tree of chromatographic methods, principles of retention and band broadening, resolution, separation speed, and column design

Ø Sample Preparation Concepts

Goals of the sample prep process, gas, liquid and solid sample techniques, solvent extraction, concentration, sample dilution, solvent-less methods and method development

Ø Column in Gas Chromatography

Evolution of column design, mobile phase properties, stationary phase properties and selection, retention mechanisms, column preparation and evaluation, and method development

Ø Instrumental Aspects of Gas Chromatography

Pneumatic systems, thermal zones, sample inlets, multidimensional chromatography, comprehensive chromatography, and detectors

Preparation and properties of column packings, column preparation and evaluation, retention mechanisms, and method development

Ø Instrumental Aspects of Liquid Chromatography

Solvent delivery systems, sample inlets, temperature control, coupled column systems, detectors, and indirect detection

Ø Other Separation Techniques

TLC, SFC, Electrophoresis, other hyphenated techniques Ø Special Topics

To be determined through class input, time available, and possible outside experts.

Academic Integrity:

Academic integrity is an essential component of your education. The following is a quote from the “PSU Faculty Senate Policies for Students” - Academic integrity “is the pursuit of scholarly activity free from fraud and deception and is an educational objective of this institution. Academic dishonesty includes, but is not limited to, cheating, plagiarizing, fabricating of information or citations, facilitating acts of academic dishonesty by others, having unauthorized possession of examinations, submitting work of another person or work previously used without informing the instructor, or tampering with the academic work of other students.” All University and Eberly College of Science policies regarding academic integrity/academic dishonesty apply to this course and the students enrolled in this course. Refer to the following URL for further details on the academic integrity policies of the Eberly College of Science:

http://science.psu.edu/current-students/Integrity/Policy.html

Matters of academic dishonesty will be turned over to the University disciplinary system and may result in a failing grade for the course.

Disability Policy:

Penn State welcomes students with disabilities into the University's educational

programs. If you have a disability-related need for reasonable academic adjustments in this course, contact the Office for Disability Services (ODS) at 814-863-1807 (V/TTY). For further information regarding ODS, please visit the Office for Disability Services Web site at http://equity.psu.edu/ods/.

In order to receive consideration for course accommodations, you must contact ODS and provide documentation (see the documentation guidelines at

http://equity.psu.edu/ods/guidelines/documentation-guidelines). If the documentation supports the need for academic adjustments, ODS will provide a letter identifying appropriate academic adjustments. Please share this letter and discuss the adjustments with your instructor as early in the course as possible. You must contact ODS and request academic adjustment letters at the beginning of each semester.

Mutual Respect and Cooperation:

The Eberly College of Science Code of Mutual Respect and Cooperation

( http://science.psu.edu/climate/code-of-mutual-respect-and-cooperation/Code-of-Mutual-Respect%20final.pdf/view) embodies the values that we hope our faculty, staff, and students possess and will endorse to make The Eberly College of Science a place where every individual feels respected and valued, as well as challenged and rewarded.

How to be Successful in this Course:

Be prepared for class by studying/ reviewing the lecture material, and by reading the assigned chapters of the text book and the assigned journal articles. Come to every class, ask questions, and schedule one-on-one meetings with Dr. Dorman if you’re struggling with the course material. Make sure you understand the material, as the exams will NOT be a series of multiple choice questions designed to test recall only.

Tentative Agenda, subject to change

DATE

TOPIC

26 AUG 13

Fundamentals of Separations Phase Distributions

28 AUG 13 Fundamentals of Separations _{Phase Distributions} 30 AUG 13

Fundamentals of Separations Distribution Ratio/equilibrium/thermo

2 SEP 13 LABOR DAY - No Class

4 SEP 13 Distribution Ratio/equilibrium/thermo Fundamentals of Separations

6 SEP 13 Fundamentals of Separations Extraction 9 SEP 13 Fundamentals of Separations Extraction 11 SEP 13 Fundamentals of Separations Counter Current Extraction

13 SEP 13 Fundamentals of Separations Mass Transport/Diffusion

16 SEP 13

Fundamentals of Separations Peak Shapes and measurements

18 SEP 13 Fundamentals of Separations

Mass Transport/Diffusion 20 SEP 13 Fundamentals of Separations Mass Transport/Diffusion 23 SEP 13 Column Chromatography Pressure and Flow

25 SEP 13 NEAFS Conference – Lecture TBD

27 SEP 13

30 SEP 13

Column Chromatography Pressure and Flow

2 OCT 13

Column Chromatography Pressure and Flow

4 OCT 13 Column Chromatography Resolution 7 OCT 13 Column Chromatography Resolution

EXAM 1 Distributed

9 OCT 13 Gas Chromatography General Instrumentation 11 OCT 13 Gas Chromatography Injectors/Inlet Systems

EXAM 1 Due

14 OCT 13

Gas Chromatography Columns

16 OCT 13 Gas Chromatography _{Non-MS Detectors} 18 OCT 13 Gas Chromatography _Applications

21 OCT 13 Gas Chromatography

Applications

23 OCT 13 Liquid Chromatography _{General Instrumentation} 25 OCT 13 Liquid Chromatography _Injectors

28 OCT 13 Liquid Chromatography _Columns

30 OCT 13 Liquid Chromatography _{Non-MS Detectors} 1 NOV 13 Liquid Chromatography _Applications 4 NOV 13 Mass Spectrometers as Detectors _{GC Ion sources}

6 NOV 13 Mass Spectrometers as Detectors

HPLC Ion Sources

8 NOV 13 Mass Spectrometers as Detectors _{Mass Analyzer Types} 11 NOV 13 _{Chromatographic Modeling} Method Development

EXAM 2 Distributed

EXAM 2 Due

18 NOV 13 Electrophoretic Separations

20 NOV 13 Electrophoretic Separations

22 NOV 13 Chiral Separations

25 NOV 13 THANKSGIVING BREAK

27 NOV 13 THANKSGIVING BREAK

29 NOV 13 THANKSGIVING BREAK

2 DEC 13 Comprehensive and Multidimensional Chromatography 4 DEC 13 Comprehensive and Multidimensional Chromatography

6 DEC 13 Special Topics

9 DEC 13

_{EXAM 3 Distributed}

11 DEC 13 Special Topics