Nuclear Magnetic Resonance (NMR) Center

Nuclear Magnetic Resonance (NMR) spectroscopy, is invaluable for characterizing molecules we synthesize or isolate from natural sources. NMR spectroscopy is more than one method offering many experiments that allow structure determination, characterization of clusters and polymers, binding equilibria, measurement of molecular dynamics and kinetics and insights on chemical reactivity. Familiarity with NMR is important for professional activity in the molecular sciences.

Our facility is located in rooms 33N (and 29) of the Chemistry-Physics Building and 315A of the Jacobs Science Building. The facility includes two NMR spectrometers and one EPR spectrometer. The facility serves investigators all across campus regardless of college or departmental affiliation, and includes users from the equine center and the CAER. 

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 three 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.

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

Longer runs are scheduled on the weekends. To be considered for weekend time, please communicate with Arthur Cammers. 

B. Electron Paramagnetic Resonance (EPR) can be performed at room temperature on the user-friendly EPR in CP 33. This instrument is ideal for free radicals. To discuss EPR experiments communicate with Anne-Frances Miller.

Short list of Instruments:

  • 400 MHz Bruker Avance NEO (equipped with a Smart Probe) acquired in 2018.
  • 500 MHz JEOL ECZr (equipped with a Royal Probe) acquired in 2016.
  • 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 Arthur Cammers, and day to day operations of the NMR facility are executed by Justin Holmes. the graduate assistant.

Cammers can be reached by email at a.cammers@uky.edu CP 027 (office) supervises NMR center operations, consults with users and teaches undergraduate spectroscopy.

Justin Holmes is the current NMR Center R.A. He runs samples for undergraduate lab courses, advanced courses requiring NMR spectroscopy and NMR research samples.

Research samples

Standard research samples are collected at 10 a.m. and 5 p.m. 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 procedure  helps 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.

Outside Users

The NMR center 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 Arthur Cammers. 

Sample Runs, Training, Hands-On Instrument Time

We require training for UKY community users who wish to run the 400 MHz Bruker in real time. Otherwise, samples are submitted to the NMR center in Chem / Phys 033. Experiments are set up by NMR center staff/volunteers and data are emailed directly to the submitter. The originators need to fill out our online sample submission form. For access to the NMR center and the sample submission system, please email Arthur Cammers. Please allow at least two days' notice on all such requests.

Learning More

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

NMR Processing Software

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 center offers consultation 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. Follow the steps indicated by Bruker to activate. 

You may have legacy NMR in your research group's archives and these will likely be in the Varian format. 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. 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 one to three day before the software can be downloaded. 

NMR References 

Many options exist  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 Arthur Cammers.