Department of Chemistry

DEPARTMENT OF

Chemistry

site header

NMR

  • Samples in the NMR Lab
  • Molecule Structure in the NMR Lab
  • NMR Equipment
  • Large Liquid Nitrogen Containers in the NMR Lab
  • Françoise Sauriol in the NMR Lab

Location

Department of Chemistry
Chernoff Hall Room 108A
90 Bader Lane
Queen's University
Kingston, Ontario, Canada K7L 3N6
Office: 613-533-2260
Lab: 613-533-6000 ext.77761
Fax: 613-533-6669

Hours

Monday to Friday
10:00 a.m. to 6:00 p.m.

The NMR lab is equipped with six Bruker NMR spectrometers ranging from 300 to 700 MHz. The Avance-300 and 400 run Topspin-1.3 software, while the NEO-500 and 700 MHz spectrometers run Topspin-4.  The auto-400 and 600 MHz spectrometers use XWINNMR software. The spectrometers are operated by students who have received adequate training. The spectrometers are reserved online through the Faces scheduling website. There are a few additional NMR programs located on extra computers in the NMR lab: ACD prediction software (H and C13, as well as F19, N15 and P31), Mestrec-Nova processing, and Topspin (version 1.3, 2.0 and 3.5) processing software. TOPSPIN NMR processing is available freely for academic users. Also available on these computers is the ACD-NMR processing and Spinworks.

Contact Information

Photo: Francoise Sauriol

Dr. Françoise Sauriol
NMR Manager
Email: Francoise.Sauriol@chem.queensu.ca
Website: NMR Website
 

Instrumentation
  • AVANCE-300 – TXI probe, used for routine 1H, 13C, 31P and 15N NMR – 1D and 2D
  • AVANCE-400 - Solution NMR for all nuclei including 19F –1D or 2D; equipped for variable temperature: BBFO probe with auto tuning and matching
  • NEO-500 - Solution (BBFO probe with auto tuning and matching) equipped for variable temperature
  • Auto-400 - Solution NMR for all nuclei–1D or 2D (except Fluorine) – Automatic sample changer – for 60 samples – Automatic Tuning and Matching
  • AVANCE-600 - 3 channel instrument for Solution NMR for all nuclei (except Fluorine). Also Solid CP-MAS probe for nuclei - 1D, 2D or 3D-NMR - equipped for variable temperature; also equipped with a MAS probe for wideline NMR & semi-solid material.
  • NEO-700 - 3 channel instrument equipped with 4 probes for solid state with MAS and a solution probe. The solution probe is a BBO with auto tuning/matching. In terms of solid, we have a 1.3 mm H/F/BB (max speed 67 kHz), a 2.3 mm tri-gamma probe (max speed 37 KHz) a 3.2 mm low gamma nuclei, and a 4 mm BB probe (15 KHz max spinning). This instrument is equiped with a BCU-II unit that can provide temperature down to 233K.
Training
  • We provide basic NMR training (3 hours) to learn how to set up 1D, 2D experiments on the Bruker Avance spectrometers. The basic training includes the manipulation of the Auto-400 (Icon-NMR program). The maximum number of students attending the basic session is limited to three. We also show participants how to back up data files and how to manipulate other NMR programs (i.e. prediction software, the NMR database, etc.).
  • The users that followed the basic training and submit the safety sheet to the main office signed by the user and their supervisor can have their swipe card activated, which admits them into the NMR lab after hours. The safety form can be picked up at the main office.
  • The training for using the 400/500 spectrometers is much shorter (30 min to 1 hr). The training consists of learning manual shimming, variable temperature, and auto tuning of the probe. This training is open to everyone (who has received the basic training). This training is offered on an individual basis and is arranged by email. The user is strongly encouraged to bring his or her own sample for the training.
  • The training on the 600 is 3 hrs long and is only open to graduate students, Post-docs and researchers with a background in NMR. The user must bring meaningful sample(s) from their research and during the training we perform 2D NMR experiments like HSQC, NOESY, etc. and learn how to quickly calibrate proton pulse, measure relaxation time and do probe tuning. This training is offered on an individual basis and is arranged by email.
  • The training on the 700 is 1-2 hrs and consists of running different experiments on the solution with the student sample. There is also a training for solid probes, like the 4 mm BB probe; this training is for students that are recommended by his or her supervisor. Not all probes are multi-users as some probes need to be open to replace some capacitors to reach different frequencies.
 
Reservation and booking rules

Except for the Auto-400, all the other spectrometers are reserved through Faces Scheduling website where our group name is: QCHEM. The spectrometers can be reserved up to 2 days in advance. Longer blocks of time can be reserved on the weekend. On Saturday during the daytime (9am to 6pm), users can reserve time up to 3 hours max on the 400/500 spectrometers. On the 500, a user can reserve a second block of time to conduct longer experiments.

Your name will be activated in Faces to using the spectrometer(s) as soon as you have completed the proper training session.

  • The 300: Weekdays from 8 AM to 6 PM is reserved for short periods (10 min to 30 min max) during the day. Several blocks can be made during the day (but not continuous). Longer periods are available after 6 PM. The overnight period is 8 PM until 8 AM next day.
  • The 400 and 500: Weekdays from 8 AM to 6 PM time is reserved for short blocks (10 min to 60 min max). The maximum amount of time that can be reserved by a user per day is 1 hr. Longer periods are available can be booked after 6 PM. The overnight period is 8 PM until 8 AM next day.
  • The 600: can be reserved up to 3 hour sessions during the day with the possibility of another continuous reservation for longer experiments. The overnight period is 8 PM until 9 AM next day.
  • The 700: can be reserved for solution or solid state usage. Solid state NMR is the priority for this spectrometer. When in that mode, users of solid state NMR can reserve up to 4 full days. For Solution NMR, each user can reserve up to 3 hrs during the day with the possibility of another continuous reservation for longer experiments. The overnight period is 8 PM until 9 AM next day.
 
Data Backup

If you store your files in your supervisor`s directory, your data will be backed up in the NMR lab periodically (every 2 weeks). If you store your data in a different directory that you create yourself, you are responsible for backing up your data.

To find the files that belong to you it is highly recommended that you use a 2 letter code at the beginning of all your file names. You will receive a unique 2 letter code at training time.

In the future, we will have files saved to a server that will be accessible with your e-mail username and password.

 
Service Fees

Internal users (Chemistry):

  • AV-300: $4.00/hour
  • AV-400, 500, 600: $5.00/hour
  • NEO-700: $7.00/hour
  • Overnight (8 PM to 8 AM) is charged as a 3 hour period
  • Weekend 50% reduction

External (Other Queen’s departments as well as RMC):

  • All spectrometers, except the 700: $12.00/hour
  • NEO-700: $14.00/hour
  • Overnight (8 PM to 8 AM) is charged as a 3 hour period
  • Weekend 50% reduction

Other educational institutions:

  • All spectrometers: $30.00/hour
  • Overnight (8 PM to 8 AM) is charged as a 3 hour period
  • Weekend 50% reduction

Industry:

  • All spectrometers: $100.00/hour
  • Overnight (8 PM to 8 AM) is charged as a 3 hour period
  • Weekend 50% reduction

Discount for heavy internal users:

  • Internal users spending less than $4000 per year: no discount
  • Internal users spending more than $4000 up to $8000 per year will receive a 50% discount on the amount exceeding $4000
  • Internal users exceeding $8000 per year: a 75% discount applies to the amount in excess of $8000

We offer service NMR spectra for those who do not want to use the spectrometers themselves – this service is done as soon as the spectrometers are available. Priority is given to outside users (industry) who have no internal users affiliated with the department. For users who belong to internal or external departments at Queen’s, a double charge is effective when using NMR service (instead of their own users).

Solid state NMR is available upon request (CP-MAS). To submit a sample, fill in the form in the NMR lab and leave your sample in a properly labeled vial. Your sample will be run within a week at the nominal charge for your group.