Summer 2008
Applied Basic NMR Techniques CHEM 534
Applied Basic NMR Techniques – Skills Course
CHEM 534
Summer 2008
July 28-August 8, 2008 from 9 a.m.-12 p.m.
(lectures) and from 1 p.m.-4 p.m. (labs)
Bayer 101 and NMR lab
Instructors:
Dr. Tomislav Pintauer
Office: 347 Mellon Hall
Phone: 412-396-1626
Email: pintauert@duq.edu
Office Hours: Monday 2-3pm
Wednesday 9-10 am
Friday 9-10 am
or by appointment if scheduled in advance
Dr. Rita Mihailescu
Office: 330 Mellon Hall
Phone: 412-396-1430
Email: mihailescum@duq.edu
Office Hours: Monday 4-5 pm
Wednesday 4-5 pm
or by appointment if scheduled in advance
Course Description:
The purpose of this graduate level skills course is to give an
introduction into the application of NMR spectroscopy to those
who use this method to solve problems in the fields of chemistry,
physical chemistry and biochemistry. The importance of NMR stems
from the fact that the extraction of a wealth of information can
be readily achieved by the average chemist with a minimum
knowledge in quantum mechanics or mathematics.
The course will
consist of five lectures per week (9:00 a.m.-12:00 p.m.) which
will include basic principles and theory of NMR, relating
chemical shift and coupling constants to molecular structure,
important one and multi dimensional experiments and discuss their
application in assignment and structure determination problems.
In addition the course involves a laboratory during which
students will get hands on experience in acquiring NMR spectra,
and perform on line processing and practice assignment and
structure elucidation using one- and two dimensional NMR spectra.
The organic, inorganic and organometallic aspects of NMR will be
taught by Dr. Tomislav Pintauer, and the biochemical perspectives
of NMR will be covered by Dr. Rita Mihailescu.
Recommended Text:
We will use “ABCs of FT-NMR” by John Roberts. This book is
published by University Science Books and is available via
amazon.com or barnesandnoble.com
Applied Basic NMR Techniques
Chemistry 534
Summer 2008
Syllabus
1
Summer 2008
Applied Basic NMR Techniques CHEM 534
Other Recommended Texts:
J. W. Akitt and B. E. Mann; "NMR and Chemistry: An Introduction
to Modern NMR Spectroscopy" Stanley Thornes, Cheltenham 2000
Grading:
Class Participation: 10%
Instrument Manipulation: 10%
Assignment 80% (Due August 15, 2008)
Inorganic, Organic and Organometallic Students: Each student is
required to collect a data set for a compound with unknown
structure.
The compound can be provided by the student, or if
not available, it will be provided by the instructor. Data set
collection will include 1H and 13C NMR, as well as 2D COSY.
If
the compound contains other NMR active nuclei such as P, Si or F,
those NMR need to be collected as well.
The final report will
include detailed structural determination of the unknown compound
supported by the NMR measurements. The format of the report will
be provided during lectures. Unknown compound cannot be
commercially available.
Biochemistry Students: Each student is required to collect a data
set for an RNA molecule which will be provided by the instructor.
The predicted secondary structure of the RNA will be provided.
The student will acquire 2D NOESY on this sample, both in H2O
based buffers to obtain information about the imino proton
resonances, as well as in D2O based buffers to obtain information
about the base H8/H6 and ribose H1’/H2’ region. The final report
should contain the assigned imino proton resonances as well as
the “NOE walk” with the corresponding assignments in the H6/H8
region.
Grade Distribution:
90-100 A
85-90 A80-85 B+
75-80 B
70-75 B65-70 C+
60-65 C
55-60 D
<55 F
Applied Basic NMR Techniques
Chemistry 534
Summer 2008
Syllabus
2
Summer 2008
Applied Basic NMR Techniques CHEM 534
Tentative Course Schedule for Organic, Inorganic and
Organometallic Students
Monday, July 28
Lecture: NMR Theory (Dr. Rita Mihailescu)
Tuesday, July 29
Lecture: NMR Theory (Dr. Rita Mihailescu)
Wednesday, July 30
Lecture: NMR Theory (Dr. Rita Mihailescu)
Lecture: Spin-Spin Splitting (Dr. Tomislav Pintauer)
Lab: Basic 1H NMR Spectroscopy of Organic Compounds
Thursday, July 31
Lecture: Chemical Shifts (Dr. Tomislav Pintauer)
Lab: Basic 13C NMR Spectroscopy of Organic Compounds
Friday, August 1
Lecture: Measurements of Rates by NMR (Dr. Tomislav Pintauer)
Lab: COSY and NOESY
Monday, August 4
Lecture: Data Analysis from July 30, July 31 and August 1
Lab: Heteronuclear NMR
Tuesday, August 5
Lab: Low T dynamic NMR
Lab: Low T dynamic NMR
Wednesday, August 6
Lecture: Data Analysis
Lab: Student’s samples
Thursday, August 7
Lecture: Data Analysis
Lab: Student’s samples
Friday, August 8
Lab: Student’s samples
Lab: Student’s samples
Applied Basic NMR Techniques
Chemistry 534
Summer 2008
Syllabus
3
Summer 2008
Applied Basic NMR Techniques CHEM 534
Tentative Course Schedule for Biochemistry Students
Monday, July 28
Lecture: NMR Theory (Dr. Rita Mihailescu)
Tuesday, July 29
Lecture: NMR Theory (Dr. Rita Mihailescu)
Wednesday, July 30
Lecture: NMR Theory (Dr. Rita Mihailescu)
Lecture: Spin-Spin Splitting (Dr. Tomislav Pintauer)
Lab: Basic 1H NMR Spectroscopy of Organic Compounds
Thursday, July 31
Lecture: Chemical Shifts (Dr. Tomislav Pintauer)
Lab: Basic 13C NMR Spectroscopy of Organic Compounds
Friday, August 1
Lecture: Measurements of Rates by NMR (Dr. Tomislav Pintauer)
Lab: COSY and NOESY
Monday, August 4
Lecture: Data Analysis from August 1
Lab: How the spectrometer works: Tuning, shimming and instrument
calibrations
Tuesday, August 5
Lab: Pulse field gradients
Lab: Solvent suppression methods
Wednesday, August 6
Lecture: NMR data processing
Lab: HSQC data analysis
Thursday, August 7
Lecture: RNA structure calculation
Lab: COSY for RNA samples
Friday, August 8
Lab: Student’s samples
Lab: Student’s samples
Applied Basic NMR Techniques
Chemistry 534
Summer 2008
Syllabus
4