Instrument Manuals

DO NOT ATTEMPT THESE EXPERIMENTS WITHOUT SPECIFIC TRAINING BY NMR STAFF
Although NMR experiments, in principle, are the same elsewhere, these specific instructions pertain only to methods in this facility.

If there are any issues when running your experiments, please contact one of the NMR staff immediately.  Do not attempt to troubleshoot!


Basic Instructions & Protocols

Bruker Topspin 1.3– These one page instructions will help the beginner user obtain a simple proton experiment on the DPX 250 and DPX 400.

Bruker ICON-NMR – AVIII 400 and AVIII 600 automation instructions.

Bruker Topspin 3.5– This is a quick overview to be used as a reference for obtaining a simple proton experiment ‘manually’ or in ICON-NMR on the AVIII 600.

Useful commands – This is a short list of commands used for these Bruker instruments.

File Path Description– Refer to this if you need help finding your NMR data.


Advanced 1D NMR Experiments

Selective NMR experiments – All selective NMR experiments should be obtained on the DPX 400 or the AVIII 400.

T1(H) relaxation – This is the inversion recovery T1(H) experiment which can be run on the AVIII 600 or the DPX 400

Solvent Suppression – 600 MHz ONLY – for protonated solvents with multiple proton signals use these instructions (also can be found in Bruker’s Advanced User manual).  No instruction needed for suppressing a single peak in a protonated solvent. – use the ‘WaterSup’ parameter set on the AVIII in automation.

Homonuclear decoupling – In this experiment, a proton signal of interest is saturated which effectively makes this proton invisible to the others in the molecule.

Variable temperature experiments – Warning! Trained users only!! Permanent damage to the NMR may occur if you do not follow the procedure learned in training.  These sheets only serve as guides.  All settings must be returned as stated 20 minutes prior to releasing the instrument for others.

  • – high – Maximum temp allowed is +100ºC
  • – midrange – Using the BCU on the 600 MHz, the temperature can be reduced to -20ºC
  • low – Directions are for the DPX400 MHz  in Evans Lab using the ‘evaporator’ which can reach to -90ºC.
  • very low – Directions are for DPX400 MHz in Evans Lab using the ‘exchanger’ which can reach to -120ºC.  These directions are also similar to the procedure for cooling from -20ºC to -120ºC on the 600 MHz in CBEC using the ‘exchanger’.

2D NMR experiments

Basic 2D Instructions – These instructions will help the user set up a COSY experiment and can be modified slightly for the NOESY, HSQC, and HMQC.  For use on the DPX 400, AVIII 400 and AVIII 600.  Some of these experiments can be run in automation on the AVIII.

DOSY – Instructions for obtaining a DOSY data set and measuring the diffision coefficient on the AVIII 600.

Leave a Reply

Your email address will not be published.