Applied Basic NMR Techniques Skills Course

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:

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:

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

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 A-

80-85 B+

75-80 B

70-75 B-

65-70 C+

60-65 C

55-60 D

<55 F

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

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

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

Applied Basic NMR Techniques Chemistry 534 Summer 2008 Syllabus