NMR Training & Access

NMR Training 

As a general rule, we do not accept submitted samples from ISU researchers. If you wish to analyze your samples using NMR, you or someone from your research group must be trained to operate the NMR spectrometers. CIF staff will provide basic methods implementation and data interpretation assistance during training. ISU researchers desiring significant assistance with methods development, sample preparation, or data interpretation assistance should provide journal articles pertaining to the proposed project so we can provide informed advice and implement existing methodology. Extensive assistance may be subject to the hourly staff rate and/or co-authorship on the project should be considered. Most chemistry graduate students pursuing synthetic chemistry research will take Chem 572 as part of their coursework, however, this course is open to graduate students in other departments and provides extensive training on NMR data interpretation. 

To request NMR training: 

1. Establish an account with the Chemistry Department by completing the Chemical Services Authorization Form. The completed form should be scanned in and emailed to the address at the bottom of the form, or you may return the physical form to 1605 Gilman. All internal users, including summer students and visiting scientists, must have a valid ISU Net-ID and ISU email address before receiving training in the facility. 
2. Pass the EH&S fire safety and extinguisher training.  
3. Send an email to Dr. Sarah Cady or Dr. Jeff Purslow to schedule training. Your email should include which instrument you would like to train on first and your availability for the next week or two. Here is an example email:
   1. Email on behalf of a new student in your group: Hi Sarah and/or Jeff, This is Sally Jenkins from the Professor Magneto Group. I am cc'ing my new student, Jane Smith, who needs to schedule NMR training. Jane has accompanied me to the lab a few times and is familiar with the instruments. Jane has completed the Chem Services Authorization Form and emailed it to the office. I would like Jane to be trained on the <pick one of the NMR spectrometers>, and she is available Tuesday afternoons and Wednesday mornings. I would also like Jane to have autosampler training <or some other specific thing that your group does>.  
   2. Email directly from a new student: Hi Sarah and/or Jeff, This is Jane Smith and I am a new student in the Professor Magneto Group. I have completed the Chem Services Authorization Form and emailed it to the office. I would like to train on the <pick one of the NMR spectrometers>, and I am available Tuesday afternoons and Wednesday mornings. My labmate, Sally, says I should also get trained on the autosampler.
4. Initial training will take approximately one hour. After training you will receive an email with a variety of information on how to download the processing software, access the instrument scheduler, reminders about spectrometer schedules, key card access, etc. You will also be added to the cif-nmr-users email list where important announcements and instrument maintenance status updates are shared. 

A slightly different protocol is applied to external users.

Each spectrometer is slightly different and requires a separate training. Initial training on standard experiments takes approximately one hour per instrument. Everyone who wishes to run NMR must get trained - there is no sharing of NMR user accounts. Sharing NMR user accounts may result in suspension of NMR access privileges. After training, users will be authorized to operate the instruments without supervision. It is strongly encouraged that you come to the NMR lab with a member of your research group that has previously been trained on NMR, both prior to your NMR training, and once or twice after you complete training. "See one, do one, teach one," is a great philosophy for learning how to operate instrumentation.   If you require assistance or implementation of additional methodology after initial training, please contact the CIF staff member you trained with. 

EPR Training

Individuals wishing to use the EPR should follow the protocol above for establishing an account with the Chemistry Department. EPR is substantially different from NMR in that it is much less automated, the training will take place over several sessions, the instrumentation setup can vary greatly depending on the sample, and cryogenic EPR is often required for samples, especially paramagnetic metals. Prior to requesting EPR training, please do some research on EPR analysis of samples similar to yours, and send those journal articles along with the training request. For example, Cu(II) is paramagnetic but Cu(I) is not.  What temperature do people analyze Cu(II) using EPR? How do they prepare their samples? Are the materials in a solvent or are they a solid? Unfortunately, almost every EPR project request is unique, unlike standard ¹H solution NMR where the vast majority of people can analyze their samples with the same parameter set. 

Access to Instrumentation

All instruments are available 24 hours a day, 7 days a week. Users must supply their own NMR tubes and solvents. It is advisable to come to the lab with your samples already prepared in NMR tubes, as we only have a small wet lab available in the CIF. All solution NMR instruments except for the AVIII 600 Cryo are run on a first-come first-served basis during portions of the day, with a 10 minute time limit during walk-on time. Currently, the AVIII 600 Cryo is used extensively for biological solution NMR. Time requests for the AVIII 600 Cryo for samples requiring high-sensitivity ¹³C, ¹⁵N etc. should be discussed with Dr. Jeff Purslow. 

Once a user has received training on a particular instrument, the user can register for the Instrument Scheduling System. If it is your first time accessing the scheduler, please email CIF staff after registration to have your account activated. Please only reserve time you plan to use. Users should arrive within 10 minutes of the start of their reservation time or the time will be forfeited. CIF reserves the right to charge users for time reserved but not used. Abusive over-scheduling or scheduling long blocks of time for "personal walk-on hours" may result in loss of NMR reservation privileges or NMR usage privileges. Users should plan on being logged in to the spectrometer computer for most of their reservation time. Users should be present at the end of their reservation time, or leave a note for the next person regarding the preferred steps for stopping any acquisition and ejecting their sample. Do not leave the general NMR lab area if you are running automation during walk-on hours, as the 10 minute time limit still applies and you will need to stop your run if another user enters the lab.  

The current NMR schedules are as follows:

Users requiring high-field NMR access should contact Dr. Jeff Purslow or Dr. Bruce Fulton in the Biological NMR Facility in BBMB to schedule time on the 700 or 800 MHz instruments. The 700 and 800 MHz NMR spectrometers in the BNMRF are both equipped with cryoprobes, feature very high resolution for large molecular weight systems, and provide up to 4x signal enhancement for low concentration samples. 

Access to Labs

Iowa State ID cards are required for after-hours access. The Access Request Form can be filled out after training. Users who have office located outside of Hach Hall can also request external door access via the Access Request Form, or via email to Dr. Sarah Cady. College of LAS policy does not allow us to grant external door access to undergraduates, and you will not have access to Hach in the late evenings or weekends. However, you may request lab access to use the NMR in the early morning or evening hours when the building is open but the lab is locked. 

External users requiring after-hours lab access can request an affiliate ISU card. 

Access to Data

The NMR facility has a site license for MNova NMR processing software. This software is available on shared computers (3 in Hach, 1 in Gilman) or available for download on your personal Windows or Mac computer. The MNova software is very user-friendly, can be used to process both Bruker, Varian/Agilent, or JEOL data, and perform tasks such as peak picking, integration, multiplet analysis and many other high-level features. The shared processing computers also have copies of ACD Labs NMR prediction software available. The processing computers are networked for instantaneous access to data that has been acquired on any of the facility spectrometers. Topspin processing licenses are also available from Bruker for no cost to academic users. 

The CIF contracts with IT Services for space on its networked attached storage drive. After logging out of a spectrometer, any data you acquired will be uploaded to the networked storage, also called the CIF Research Data Cloud. Users will be granted access to The Cloud after their initial training, and a folder will be automatically created after the first file is saved to the new user account. The Cloud can be accessed from on or off campus. Occasional blips in the network may prevent data from being uploaded to the cloud; if you discover a file that is missing, please contact CIF staff so it can be uploaded manually.

Access to both the MNova processing software license and the CIF Data Cloud requires connection to the IASTATE network or connection to the ISU VPN, both of which require a valid Net-ID. If you are leaving ISU but still require access to MNova software or data for completion of your thesis or publications, please click through to this guide. 

Good NMR Practices and Abuse of NMR Privileges

Very rarely do we encounter individuals who do not respect the instrumentation in the facility, the training that is required before using the instruments, the time constraints of other users, or the policies established by facility staff. In these rare instances, CIF may deem it necessary to temporarily suspend NMR access privileges until a conversation can be had with the user's major professor or the Chemistry department chair.

Please remember:

1. If something is not working correctly, please contact CIF staff and explain the problem to the best of your ability. During regular hours, you can find us in the office, or we will put up a note as to our location in Hach or Gilman. After hours, email or text is the best way to contact us. Emailing a photo of the error on the screen will be helpful. We will typically reply to emails after hours, especially if the problem is easy to correct. We may walk you through troubleshooting over text/email when possible.
2. Do not walk away from a broken NMR tube without cleaning it up to the best of your abilities. There is a broken glass bucket and broom/dustpan in the NMR lab for this purpose. If there is glass stuck in a spinner, set the spinner on the shelf above the printer and email us to let us know to clean it out. If a broken NMR tube is in an instrument, please leave a note on the spectrometer keyboard and email CIF staff immediately.
3. Do not abuse walk-on time. During walk-on hours, instrument usage is limited to 10 minutes when others are waiting. If you have several samples to run and there is a line of people waiting to use the instrument, log off the instrument after your 10 minutes and go to the back of the line. Do not leave a spectrometer unattended during walk-on hours if you are using the autosampler software (IconNMR) - you must remain in the vicinity of the NMR lab. Do not plan on running a lengthy or multidimensional experiment during walk-on hours. You will probably be interrupted and have to stop your experiment early.
4. Do not abuse the reservation system. Reserve time as needed, but be courteous and cancel/change reservations if you will not use all of the time. Plan on being logged in for your entire reservation - do not reserve large blocks of time for personal walk-on time. Cancel large blocks of time well in advance of the start of the reservation, if possible. Do not expect to use the instrument beyond the end of your reservation if someone has signed up in the next time slot. If possible, communicate with the next person as soon as possible if you anticipate your experiment may go over your reserved time.
5. Leave the spectrometer in the "standard" configuration for the next user. If you disable the autosampler for a tall tube, be sure to reset it. If you use variable temperature, make sure to return the temperature to 298 K before exiting the software. On the MR400, if you tune to ¹⁹F, tune back to ¹H before removing your sample and exiting the software.
6. Leave notes at the spectrometer to communicate with other users if you are running a long/overnight experiment and do not plan on being present when your reservation time ends.

Above all, please remember to be kind and respectful to all NMR users and facility staff. 

Usage Rates

Users associated with Iowa State University have equal access to the facility and are charged with the same rates. Most spectrometers have a minimum billable rate of 12 minutes. 

The CIF is also open to the users from other academic institutions and industry. This usually involves submitting samples to NMR staff for data collection. External users located in Central Iowa may wish to schedule a training session and run their samples independently. Contact either Dr. Sarah Cady or Dr. Jeff Purslow for details.

The hourly rates for instrument time (user run samples) are listed below. The rate for spectroscopist time is $30.00 per hour. New users are charged the normal instrument hourly rate for initial account set up and training. Samples submitted for analysis by users from outside Iowa State University are billed at 3.0 times the internal rate. The rate for external academic users is 1.5 times the internal rate. 

See also: Internal Rates and External Rates.