NMR Facility Rules

  1. No food or drink in the NMR Facility. Crumbs attract bugs, and spilled drinks can damage computer equipment, furniture, and carpet. The work environment must remain neat and clean for all users.

    2.
  2. No smoking in the NMR Facility. Smoke particles are the right size to enter and damage computer disk drives.

    3.
  3. The exterior doors to the NMR rooms should be kept locked at all times.

    4.
  4. No unauthorized individuals are allowed in the NMR Facility. Guests must be escorted at all times.

    5.
  5. Only routine NMR experiments may be performed. Users must receive permission and instruction before attempting any new or specialized techniques. The NMR Facility Manager must be informed before any non-standard equipment or experimental setup is used. Appropriate safety measures will be discussed and implemented. Users may not work alone when setting-up or performing nonstandard experiments.

    6.
  6. Covers should be placed over the magnet openings when the probe is removed. This keeps out small objects including magnetic dust.

    7.
  7. Each individual is responsible for handling, labeling and storing the samples they bring into the NMR laboratory. Samples that are not labeled will be destroyed.

    8.
  8. Hazardous samples may not be brought into the laboratory without prior discussion of handling and disposal procedures with the NMR Facility Manager.

    9.
  9. NMR spectrometers are equipped with deuterium lock, thus it is advisable to have some deuterium in the sample. Generally samples are prepared in deuterated solvents; however, if a deuterated solvent is not feasible, a lock signal can be created by positioning a capillary tube with deuterated material inside the NMR tube. Deuterated solvents are never isotopically pure, so residual solvent peaks appear in the proton spectrum. This can be minimized by using high grade solvents, especially with dilute samples. Many solvents are hygroscopic and will quickly absorb water from the air if not sealed. It is important that the melting and boiling points of the solvent be taken into consideration if you do not plan to run your experiments at room temperature.

    10.
  10. Paramagnetic or ferromagnetic impurities will lead to signal degradation and/or lock instability. Samples should be filtered through glass wool to remove such particles. Dissolved oxygen has paramagnetic properties and will degrade resolution. Several freeze-pump-thaw cycles or bubbling dry nitrogen gas through the sample will reduce this problem. Use of metal needles or spatulas can leave metallic residues in your sample. Even sweat and oils from your hands can find its way into the solution. As a practical safety precaution it is necessary to wear gloves continuously during sample handling.

    11.
  11. Sample height should be about 3 cm (0.7 ml) in a 5 mm NMR tube. Overfilling can waste solvent and dilute the sample thus decreasing signal strength. Underfilling makes shimming difficult and degrades resolution. For necessarily small samples, use a vortex plug (especially in 10 mm tubes).

    12.
  12. Make sure to eject the standard sample from the magnet before inserting your sample.

    13.
  13. If a sample tube breaks in the magnet contact the NMR Facility Staff immediately. The probe must be removed and cleaned as soon as possible to minimize damage. Use thick-walled or Teflon-lined tubes with corrosive or highly toxic samples. Always test your samples at the intended experiment temperature before inserting them into the magnet.

    14.
  14. Each new user is provided with standard spectra and setup parameters in their directories.

    15.
  15. The NMR data storage system has limited capacity and cannot provide long-term storage. The system will crash when attempting to save files to a disk exceeding 95% capacity. Therefore, users are responsible for checking on their disk usage, deleting unwanted files and backing up important files to a more permanent storage medium. Accounts that are unused for more than a single year will be deleted and the associated data archived.

    16.
  16. After completing your experiments:
    • Shim the TMS signal of the Ethyl Benzene Standard to < 1 Hz.
    • Sign the log book. Include your Name, Date, Time, Solvent, Nuclei, Temperature, and Linewidth of TMS.

  17. Report all defective equipment to the NMR Facility Staff. If the problem is not potentially hazardous and the NMR Staff cannot be located, record the problem in the log book.
The NMR Facility Manager can be reached at shirazi@chem.ucsb.edu