I am on Bruker 400 in Stepan Chemistry Hall

YOU CAN DO THE ACTIONS LISTED BELOW ONLY IF YOU WERE DIRECTLY INSTRUCTED BY NMR CENTER STAFF .

Restarting spectrometer

Restarting the sample changer

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First things to do

• Notre Dame NMR Operation and Concepts
• Notre Dame Basic NMR Operation Course

1. Log in

• Log into workstation
• start Topspin software

2. Insert your sample

• Bruker 400 is equipped with an automatic sample changer Bruker SampleCase 24
  Before you use the changer you must read and view SampleCase Training
• Place the sample in the spinner
• Check for a correct depth of insertion with the depth gauge
• Place it in the carousel of the sample changer
• Issue:
  • lock off
  • ro off
  • sx N (N- your sample position)

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  NOTE: If your solvent is toluene-d8 (Tol) and 'atma' fails with an error, follow these instructions: System will not tune when lock solvent is toluene-d8

  Tuning system needs to know what nucleus you are going to work with. Follow these steps:

  • Right-click on the appropriate dataset in the data browser of Topspin
    • If you only need to use proton, any proton-detected experiment is OK
    • if you will use both proton and carbon during you session - join a carbon 1D experiment because it uses both channels and they both will be tuned.

    Automatic Tuning

    • issue
      • qu ro off
      • qu atma
      • qu wobb

      Manual Tuning

      Manual tuning mode allows you to see what channels are tuned, inspect the result of tuning and adjust if necessary

      • issue atmm
      • move the mouse cursor onto the Atma Control window and wait till the cursor stops rotating (during this time the computer talks to the motors in the probe - it is a slow communication)
      • The lowest-gamma nucleus (13C) is automatically selected and a "wobble curve" - the probe response at different frequencies is shown.
      • Select Optimize:Start to start automatic tuning

      

      

      

      1. Click Optimize:Start and let it optimize automatically
      2. (A little faster, applies to Stepan 400) Click 18 times on [>>>] button in Tuning section to bring a resonance closer to the center

      

      

      
      NOTE: The automatic tuning result is completely acceptable for most routine work. However, for best sensitivity you may want to adjust Tuning and Matching manually to make the resonance sharper.

      Probe is now tuned and ready for experiments.

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      Locking

      Next step is to lock spectrometer on your solvent:

      1. Load the default shimset
         • Issue: rsh
         • Find bbfo-latest in the dialog window
         • Click Read button
      2. Issue: lock
      3. Select your solvent in the dialog window

      Wait for the lock system to finish locking (see the status messages)

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      Shimming is required to achieve good resolution in NMR spectra.

      issue topshim in the experiment you intend to run

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      Using Temperature Control

      IMPORTANT NOTE: If you need to use temperature OUTSIDE of 20-40 Deg C range,
      you must be trained on the "Variable Temperature" protocol: contact NMR center staff to schedule training.

      For all Variable Temperature tutorials and instructions see Variable-temperature NMR operation

      The instrument is equipped with manual BCU-1 refrigerated chiller and liquid N2 chiller.