Training within the CIC NMR Facility consists of two laboratory classes, and other, more informal training sessions. The classes provide students with access to the various instruments in our facility.
Chem 636: Graduate students gain access to the
3 routine instruments (Mercury-300 and Bruker ACs) by taking Chem
636, offered in both the fall and spring sessions.
--Chem 636 and 637 have limited enrollments, and students must obtain
approval prior to registering.
Chem 637 is an advanced laboratory course, offered
only in the 8-week summer session.
--Chem 636 is strongly recommended as a prerequisite to enrolling in Chem
637.
--Completion of Chem 637 provides access to the department's 360 and 500 MHz
spectrometers.
--Enrollment is limited, similar to Chem 636 (see above).
--Chem. 637 is a prerequisite to gaining access to the INOVA-600 spectrometer.
Training is available for both X-ray Crystallography and Mass Spectrometry; see discussions in the X-ray and Mass Spectrometry home pages.
Chem 605 provides detailed training for interpretation of NMR spectra, taught by Prof. Hans Reich each spring semester.
Biochem 800 teaches product operator formalism specifically directed at enabling understanding of complex NMR pulse sequences as applied to biomolecules. Taught by Milo Westler every year in the fall semester.
Biochem 801 is an introductory survey course for NMR techniques applicable to biomolecules. Taught by John Markley every other year (even years) in spring semester.
Routine NMR: Chem 636, Fall and Spring semesters
Access to the Varian Mercury-300 (Hermes) and AC-300s (Homer and Athena)
Instructor:
Chemistry 636, offered in the Fall and Spring semesters, provides the primary introduction to experimental NMR in the facility. The department's interpretation class, Chem 605, is highly recommended as a prior or concurrent course. Chem 636 provides extensive hands-on training for obtaining routine 1H and 13C spectra. The course also provides training for our automated sample changer, which is particularly useful for obtaining 13C, COSY and heterocorrelation 2D spectra of moderate-concentration samples.
Due to lab size limitations, course enrollment is limited to 30 students. Students should therefore obtain instructor permission as early as possible to ensure enrollment. Students attend one 1-hour lecture and one 2-hour lab session per week. Lectures are held Tuesday mornings at 8:50AM in Chem. room 2311. Labs sections are offered T,W,R,F from 4-6 PM, and Thursdays 9-11 AM, but may change depending upon enrollment.
A Bruker AC/AM User Guide and Mercury-300 User Guide are available to assist in the use of the routine spectrometers.
Chem 636, first 7 weeks: Introduction to 1H 1D NMR and Sample Changer
Prerequisite: A basic understanding of chemistry and NMR (e.g., successful completion of undergraduate organic chemistry); instructor approval.
|
Wk |
Lecture |
Lab |
|
1 |
Introduction, FIDs and FTs, phase correction |
Data processing via NUTS* |
|
2 |
Lab safety, instrumentation, locking and shimming |
Introduction to Bruker AC spectrometers: 1D 1H NMR* |
|
3 |
The vector model of NMR, the rotating frame, pulse and phase angles |
1D 1H NMR continued: using the Bruker EP mode* |
|
4 |
The Nyquist theorem, digitization and resolution, zero-filling |
Pulse-width calibration: the vector picture of NMR demonstrated |
|
5 |
Phase cycling and quadrature detection |
The rotating reference frame, spectral artifacts and off-resonance effects |
|
6 |
Signal-to-noise, integration, quantification |
Using Athena's sample changer* |
|
7 |
Lecture Exam No. 1 |
Lab Exam No. 1* |
* These labs are required for undergraduate training.
Chem 636, 2nd 7 weeks: 1D 13C NMR and 1H assignments aids
|
Wk |
Lecture |
Lab |
|
8 |
Practical considerations of 13C NMR |
13C NMR and 1H decoupling |
|
9 |
Signal enhancement via polarization transfer (PT) |
PT and spectral editing: the DEPT experiments |
|
10 |
Nuclear spin relaxation |
Estimating T1 via T1NULL.AU |
|
11 |
X-ray Crystallography lecture |
Lab practice |
|
12 |
Origins of the nuclear Overhauser effect (NOE) |
Comparison of NOE and PT |
|
13 |
Introduction to 2D NMR: 1H,1H COSY |
Manual COSY acquisition |
|
14 |
2D NMR continued |
VT NMR on Phoenix |
|
15 |
Lecture Exam No. 2 |
Lab practice |
|
16 |
Miscellaneous topics |
Lab Exam No. 2 |
Chem. 637: Modern Techniques for Structural Analysis
Access to the Varian UNITY-500 (Narn) and INOVA-500 (Vorlon)
Instructor:
Chem 637 places two completely independent requirements on the student: (i) becoming facile with Varian's VNMR software and the UNITY/INOVA consoles and probes, and (ii) learning experimental techniques directed at modern techniques for structural analysis.
A Varian User Guide is available to assist in the use of the Varian 500 and 600 MHz spectrometers.
Chem 637: This course is offered during the 8-week summer session. Lectures are scheduled each T at 8:50 am for two hours. Each student will be assigned to one 2 h laboratory session per week.
Prerequisite: Completion of Chem. 636; instructor approval.
|
Wk |
Lecture |
Lab |
|
1 |
Introduction to VNMR and Unix |
1H 1D NMR on the UNITY |
|
2 |
13C NMR: PT and NOE |
13C NMR: NOE, quantitative, PT |
|
3 |
1H 1D fundamentals and assignment aids: |
homodec, pw90 calibrations, T1 |
|
4 |
Selective 1D techniques |
NOESY-1D, TOCSY-1D |
|
5 |
Introduction to 2D techniques: COSY spectroscopy |
Student research project |
|
6 |
COSY extended - long-range, double quantum, ... |
Student project continued |
|
7 |
NOE, relaxation and NOESY/ROESY |
Student project continued |
|
8 |
Brief intro/review HMQC/HMBC; Lecture exam |
Lab exam |
Training and Access for the ESR and Solid-State NMR
Training for the Bruker ESR
Instructor: none currently (see or
Training on the ESR is done on a one-on-one or small group basis. Contact or to request training.
An ESR User Guide is available to assist with the use of the Bruker ESP-300.
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