Nuclear Magnetic Resonance (NMR) Center

Nuclear Magnetic Resonance spectroscopy, or NMR, is invaluable for characterizing molecules we synthesize, and isolate from complex natural extracts. 'NMR' is much more than one method, as it offers a dizzying array of experiments that allow structure determination, characterization of clusters and polymers, binding equilibria, measurement of dynamics and kinetics and elucidation of reactivity. Familiarity with NMR is important for almost all academic and industrial jobs in chemistry.

Our facility is located in rooms 33N (and 29) of the Chemistry-Physics Building, and 315A of the Jacobs Science Building. The facility currently includes 5 NMR spectrometers and 2 EPR spectrometers. In addition, there is a data station for offline processing of NMR data. The facility serves investigators all across campus regardless of college or departmental affiliation, and includes users from the Equine centre and the CAER. Each research group must have an NMR delegate named by the group P.I. and communicated directly to Dr. Miller. The delegate serves as the group's point of contact with NMR to help keep the volumes of correspondence manageable for everyone.

Instrumentation and Options

A. For characterization of small molecules using all routine solution methods and a variety of nuclei, users can choose among:

  1. an automated fast turnaround 400 MHz Bruker spectrometer that executes all standard experiments with 1H 1-dimentional (1d) spectra returned within 3 hours most days.

  2. an automated 500 MHz JEOL spectrometer that executes all standard experiments. Turnaround times vary more on this instrument because its priority is service to undergraduate instruction. However it is also deployed to address samples needing greater resolution or unusual solvents. Target turnaround is ≤24 hours on 1H 1ds.

  3. a 400 MHz Varian/Agilent spectrometer is available for hands-on use with the probe quadruply-tuned for 1H, 19F, 31P and 13C (users may not retune the probe).

    • Reservations must be made on FACES.

For standard run-times for different experiments, please see this document. Any requests involving more than 4 hours for a sample may be scheduled overnight or even on the weekend in order to not delay progress on all other samples. (It may occasionally be necessary to limit each user to 8 hours of instrument time per 24 hours.)

Longer runs are scheduled on the weekends. To be considered for weekend time we NEED an email from your group's delegate (not the sample originator unless the originator is the delegate). The email should be sent to Ms. O. Oladele and must say how many samples will be submitted for the weekend and how much instrument time is requested for each. For samples being submitted on Saturday, 5 pm is the cut-off for sample drop-off, and please submit the web form on Saturday before 5, not Friday.

B. Diffusion measurements and high-resolution high-sensitivity needs can be met on our 600 MHz Varian/Agilent spectrometer. An additional robotic 500 MHz high-resolution spectrometer serves our large undergraduate courses.

C. 'Unusual' experiments and verrrry long acquisitions can be performed on the Agilent MR400, once construction has ceased its series of unannounced irrigations in CP 29, so it becomes safe to remove the plastic coverings and plug in electronics again.

D. Electron Paramagnetic Resonance (EPR) can be performed easily at room temperature on our old but user-friendly EPR in CP 33. This instrument is ideal for free radicals.  Studies of coupled radicals and transition metal ions that need low-temperature wide-scan EPR can be performed on the older EPR in CP 29 once that room becomes accessible again.

Short list of Instruments:

  • 400 MHz Bruker Avance NEO (equipped with a Smart Probe) acquired in 2018
  • 400 MHz Varian 400-MR (equipped with a ATB Probe) acquired in 2008
  • 400 MHz Varian Inova (equipped with a 4Nuc Probe) acquired in 1999
  • 500 MHz JEOL ECZr (equipped with a Royal Probe) acquired in 2016
  • 600 MHz Varian Inova (equipped with a BioProbe) acquired in 2000
  • EMX user-friendly RT EPR (acquired used in 2020, purchase ≈2010)
  • EMX wide-scan EPR from 3.6 K to 300 K (prehistoric, likely 1970s but updated in 2015)

Who's Who in the NMR Lab

The NMR Center is Directed by Dr. Anne-Frances Miller and day to day operations of the NMR facility are executed by Graduate Assistant, Ms. O. Oladele.

Dr. Miller can be reached by email at afm@uky.edu. When on campus, likely locations are rooms CP 33 (office) or CP 390 (lab) in the Chemistry/Physics Building. Dr. Miller supervises NMR centre operations and provides advanced instruction.

Ms. Oladele is the current NMR Center T.A. She runs samples for undergraduate lab courses, advanced courses requiring NMR spectroscopy, and NMR research samples - Please email Ms. O. Oladele whenever you have special sample needs.

Research samples

Standard research samples are collected at 10 am and 5 pm every weekday. Data are collected based on the parameters requested in the online sample submission form. Samples associated with short time requests are run before those for which lengthy data collection as been requested. This is in order to return quick spectra to people as fast as possible. To assess how long individual standard experiments take, please refer to this very handy reference sheet.

Long runs are typically run over the weekends, but standard research samples can also be submitted Saturday until 5 pm. If any member of a research group wants to submit a Saturday sample(s), (s)he needs to communicate with the group's NMR delegate so that the delegate sends a heads-up email to Ms. Oladele before noon on the preceding Friday. Because weekend time is deployed for long runs, it is not possible to add any new experiments once the queue has been set up. The weekend samples and their corresponding sample submission forms (online) can be submitted until 5 pm Sat, but NMR delegates must email Ms. Oladele by Friday at noon if any member of the research group will be submitting request(s) for weekend experiments.

Outside Users

The NMR centre is open for all members of the UK community. We also offer several different options for researchers outside the university to use our facilities. For more information, please contact Dr. Miller.

Training

Until a user-access door is completed for the JSB instruments, there is no mandatory training. Instead, samples are submitted to the NMR centre, experiments are set up by NMR centre staff/volunteers and data are emailed directly to sample originators. The originators need to fill out our online sample submission form. For access to the NMR center and the sample submission system, please email Dr. Miller. Please allow at least 3 full days notice on all such requests, however a one week notice is appreciated.

Hands-On Instrument Time

While most research samples run under automation on the versatile new Bruker 400 MHz or the similarly modern JEOL 500 MHz, we can still provide hands-on use on the (vintage) Varian 400 MHz spectrometer. Because this privilege is shared by users located in buildings all across campus and CAER, users must reserve the instrument in advance using the FACES Scheduling System. This enables all users to know before they leave their building, that they will be able to use the instrument. Please use the group name UKNMR along with your username and password. To make arrangements for special long-block use please contact Dr. Miller.

Learning More

CHE 555, taught by Prof. Miller, introduces users to the 15 of the most useful NMR experiments.

In addition, users wishing to collect 2D spectra and execute advanced experiments are always welcome to contact  Ms. O. Oladele and/or Dr. Miller.

The NMR centre also maintains a modest but perfectly serviceable X-band electron paramagnetic resonance spectrometer (EPR) and a second EPR that is less user-friendly but has expanded capabilities.

Free NMR Processing Software

There are several free NMR processing software options for academic users. Users are encouraged to use these applications to process their data on their personal and/or lab computers. Additionally, users may use a copy of Mnova located on the processing computer in the NMR Center. The NMR centre offers skill sessions to help users become competent with both Topspin (Bruker or Varian data only) and Mnova.

Obtaining Topspin, (for Bruker data)

Bruker (Windows, Mac, or Linux). Once you download this software you will need to obtain an academic license. Once you have the license you can insert that into the pop-up window seen when starting the software. Follow the steps to activate. Note, this does NOT work well on the Google Chrome browser.

To launch Topspin in the 64-bit Mac operating systems (10.15 and later), use the steps document in this how-to sheet.

To open Varian files in the Bruker TopSpin program, type vconv into the command bar (bottom of the screen). Select the desired folder (the folder should have the extension .fid) in the pop-up directory window (please note that you are selecting the folder NOT the files within the folder). Then click VNMR data conversion. A new pop-up window will open. Type 10 next to EXPNO then click OK. Your file should open. 

JEOL (Windows or older Macs). This software has not yet adapted to Apple's 64-bit operating systems, but JEOL is working on it. In order to obtain this software you must register with JEOL (please do so with your uky.edu email address). Once registered follow the instructions. For instrument type select (ECZR). Please note that in order to download the JEOL DELTA software a review of your newly registered account is necessary. Thus, it may take 1-3 day before the software can be downloaded.

NMR References 

There are a plethora of options for users looking for NMR references. Indeed, the University of Wisconsin - Madison maintains a website with common 1H, 13C, 19F,  31P, and 77Se chemical shifts. Information about common H-H and C-H coupling constants can also be found on their website.

Common Chemical Shifts of Trace Impurities by Fulmer et al. is also a great resource. Organometallics (2010) 29:9, 2176-2179.

Additionally, the website NMRDB.org has a helpful NMR predictor which can be used for 1H and 13C as well as the 2D techniques COSY and HSQC/HMBC. 

For those researchers working on NMR of lignin and lignin model compounds a database completed by John and Sally Ralph (University of Wisconsin - Madison and United States Forest Products Laboratory, respectively) can be found here.

The Biological Magnetic Resonance Data Bank (BMRB) is a useful resource for those researchers working on proteins, peptides, nucleic acids, and other biomolecules. 

If you have other NMR references you would like added to this website, or if you find errors, please contact Dr. Miller.