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Bruker 800: Room-temperature probes (TXI and BBO)

 

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Basic Workflow with room-temperature probes

Updated 3/24/2023

When the cryogenic probe is out for repair, the instrument is equipped with two conventional probes: a triple resonance inverse probe, TXI, and a broadband probe for direct detection of X nucleus, BBO. The TXI probe is used for all proton-detected experiments such as HSQC, HMBC, NOESY, ROESY, COSY, and others. The BBO is used for carbon 1D experiments.

 

Step 1: Determine what probe is installed

    The best practice is to contact us ahead of the time to make sure the spectrometer has the right probe for you.

      1. Type edhead on a Topspin command line. The dialog window appears:



      2. The "Current probe:" message and a highlighted line in a table indicates the installed probe:

        5 mm BBO... - is a BBO probe for carbon detection

        5 mm CPTCI... - is a cryogenic probe for proton and carbon detection

        5 mm PATXI ... - is a TXI probe for proton detection

      3. To quit this dialog

        1. click Exit

        2. a window with spectrometer wiring appears: click Close

    If you see that the probe is a wrong type for your experiments, please, contact NMR staff to change the probe.

Step 2. Set the sample temperature

Step 3. Insert your sample, load shims, and lock

Before operating the SampleCase - please, review these guidelines:  SampleCase training

 

  1. Turn off lock and rotation:
    • ro off
    • lock off

For regular NMR tubes shorter than 9 inches: use SampleCase

        1. Place your sample in the SampleCase changer carousel
        2. Insert your sample in the magnet: 
          sx N  (N - position number in the carousel)

For J. Young tubes and other tubes longer than 9 inches: bypass SampleCase

      Follow the Manual Insertion guidelines with these modifications:

          • find the blue gas valve on top of the magnet near the bore (opposite side to the rail)
          • If the current probe is TXI:
            • increase gas flow to 670 LPH for eject and insertion
            • reduce gas flow to 400 LPH after you inserted
          • Do NOT turn off VTU after you finished working with the SampleCase

           

After the sample is inserted

      1. Load a shim set:
        1. type rsh
        2. select BBO or TXI
        3. click Read

      2. Type lock and select your lock solvent

       

Step 4. Create a new experiment

      1. Copy an experiment you want to run from a previous experiment, setup file, or a parameter set.

      2. REQUIRED: type getprosol on a Topspin command line.

        NOTE: This step is required because you must adjust all pulses and powers to the requirements of the probe. The getprosol reads the current probe parameter table and updates parameters in your newly created experiment.
        If parameters were NOT adjusted, you may damage the probe!


      NOTE: If your experiment uses a non-Bruker pulse program, which someone wrote, you must contact NMR staff to set it up properly for the current probe!

     

     

Step 5. Tuning

      1. You must be inside the experiment that you intend to run!
        Type atma and watch for wobble curves and final message "ATMA ... finished.. OK" in a status bar.

 

Step 6. Shimming

      1. Start rotation to help achieve better shimming. Type ro on

      2. If you use

        1. a normal 5 mm tube: type topshim

        2. a Shigemi tube: type topshim shigemi

          NOTE: You may want to save your shigemi-specific shimset to help you shim quicker in your future runs. Type wsh and give a new file name like [your_initials]_[probe]_shigemi. For example, I will use EK_TXI_shigemi name for the shimset I optimized for a shigemi tube with the TXI probe. Next time, I will load this shim set instead of a standard TXI in when loading initial shims.

      3. If you will continue with 1D experiments, leave the sample spinning. Otherwise, turn off the rotation: ro off


Step 7. Adjust Parameters

      1. Adjust parameters of your experiment as needed.

      2. Perform receiver gain adjustement:
        • type rga

      3. Check experiment time:
        • type expt

          NOTE: Make sure your spectrometer booking is sufficiently long to accommodate duration of the experiment! Extend your booking as needed. if possible. If - not (for example, a maintenance period is scheduled right after you), contact the NMR staff to see if more time may be negotiated.

      4. At this point, the spectrometer and the experiment are ready for acquisition.
        • type zg

 

 

 

 

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