Training Procedure for New Users

1. Complete the Request for NMR User Training form and return it to the NMR Facility staff. You are STRONGLY encouraged NOT to start training until you plan to routinely use the spectrometer for research. You may NOT use the spectrometer before the first training session.

2. Schedule 1 or more training sessions with NMR Facility staff. At least one training session with a NMR Facility staff member MUST FIRST be held, after which you may schedule additional training sessions with the Facility staff and/or you may also be trained by other experienced users.

3. Practice using the spectrometer with research samples between 8am and 5pm weekdays (i.e., when a staff member is present in the Facility). If you plan to practice using the spectrometer after 5pm or on weekends or holidays, you MUST make prior arrangements for a staff member or a designated experienced user to be present in the NMR Facility during your spectroscopy.

4. Collect, process, and plot a 1H spectrum of a typical research sample within 15 minutes:

• Line shape much be symmetrical, spinning sidebands must be no more than 2% of peak height. Write line width at 50% of the peak height and (spinning sideband amplitude)/(peak height) on spectrum. Write ALL lock and shim parameters, lock parameters, lock level, spin speed, and temperature on back of the spectrum.
• Set the number of points so that digital resolution < 0.25 hz/point after zero-filling.
• Set d1 to an appropriate value. Write on the back of the spectrum about how you chose this value.
• Spectral window must have exactly 0.5 ppm between left edge of window and left-most peak and exactly 1.0 ppm between right edge of window and right-most peak.
• Set number of transients and steady state transients. Signal/noise of the resulting spectrum must be a minimum of 10. Write the signal/noise on the spectrum.
• Set line broadening to a good value to improve signal/noise without significantly broadening your peaks.
• Spectrum must be referenced. Indicate which line was used for referencing on spectrum.
• Plot the full spectrum, scale, title, normalized integration of three or more peaks, and peak frequencies on one page.
• Plot ALL parameters with spectrum or on separate sheet.
• Save data.

5. Collect, process, and plot a 13C spectrum of a typical research sample within 30 minutes:

• Line width at half-height must be 5.0 Hz, line shape must be symmetrical, spinning sidebands must be no more than 2% of peak height. Write line width at half-height and (spinning sideband amplitude)/(peak height) on spectrum. Write ALL lock and shim parameters, lock level, spin speed, and temperature on back of spectrum.
• Set the number of points so that digital resolution &al; 1 Hz/point after zero-filling.
• Spectral window must have exactly 5 ppm between left edge of window and left-most peak and exactly 10 ppm between right edge of window and right-most peak.
• Set number of transients and steady state transients. Signal/noise of the resulting spectrum must be a minimum of 5. Write the signal/noise on the spectrum.
• Spectrum must be referenced. Indicate which line was used for referencing on spectrum.
• Plot ALL parameters with spectrum or on separate sheet.
• Save data.

6. Make a list of at least 3 suggestions or questions that you have about the spectrometer or NMR spectroscopy.

7. Review the spectra and your suggestion/question list with a staff member.

8. You're officially trained! Pick up your NMR spectroscopy merit badge, collect more spectra, and publish!