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

 

Updated 10/16/2024

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.

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Required workflow:

1. Determine what probe is installed

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2. Set the probe temperature

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3. Insert your sample

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4. Tune

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5. Load shims

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6. Lock and Shim

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7. Create a new experiment

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8. Finish your work

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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. NOTE: currently not functional.

   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.

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Set the probe temperature

1. Set temperature and gas flow values
   
   NOTE: Two conventional probes have different parameters for a normal operation. Likely, the parameters will already be set correctly but it is your responsibility to check them.
   
   
1. Type edte
   
   
2. EDTE screen appears
   
   
   
   
   
3. Check visually if the orange light on the BCU-5 switch is lit (to the right from the workstation table, behind the staircase).
   

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4. Check/set the EDTE parameters
   
   
   • For the BBO probe
     
     
     1. Set Gas flow of 670 L/h. <<<< THIS NEEDS TO BE RE-TESTED BECAUSE OF POSSIBLY POOR GAS CONNECTION DURING CALIBRATION
        
        
     2. Set Target temp. according to the table:
        
        

"Target temp." setting	Actual temperature in a sample
299.6	298.0 K  (24.8 C)
295.2	293.4 K  (20.2 C)
291.2	289.2 K  (16.0 C)






• For the TXI probe 
  • Temperature limits:  -50C to +80C
  • Perform self-tuning after reaching maximum or minimum temperature!
  • NOTE: as of 1/19/24  
    • There is some issue with cooling - possibly blockage or rupture of the gas line in the probe
    • The lowest temperature accessible temperature with a BCU-05 chiller is 280.2 K or 7C at a maximum flow rate of 935 LPH
      
      

"Target temp." setting	Required Gas flow	Actual temperature in a sample
300.0	400	298.2 K (25.0 C)
299.6	400	298.0 K  (24.8 C)
295.2	400	293.4 K  (20.2 C)
291.2	400	289.2 K  (16.0 C)
282.0	670	278.7 K (5.5 C)

• 
  
  
2. To change temperature use 10-degree steps and wait 3 min after each step.
   
   
3. Set gas flow to the value for your target point
   
   
4. If your target temperature is more than 5 degrees from the initial temperature: wait at least 10 min after reaching the target and before proceeding with shimming

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Insert your sample

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

 

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

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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)
   

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For Shigemi NMR tubes

1. Check that your Shigemi tube has 8 mm bottom piece ("Bruker" tube)
   
   
2. Set the tube in a spinner to have the sample volume is centered around horizontal line in the middle of the coils
   
   
   
   NOTE: The bottom of the Shigemi tube does NOT touch the bottom of the depth gauge !
   
   
3. Use SampleCase

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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
  

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Tune

1. Display the experiment that has nuclei that you intend to use: check Procpars:Nucleus section.
   
   
2. Type
   spooler
   qu atma
   qu wobb
   
   Watch spooler window for atma to finish and exit and wobb start.
   
   
3. Double-check the tuning results in wobb window.
   NOTE: wobb will never finish on its own. You must click stop button in the toolbar.

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Load shims

1. Load an appropriate shim set:
   
   
   1. Type rsh
      
      
   2. Select
      
      
      1. for normal tubes: BBO or TXI
         
         
      2. for Shigemi tubes with the TXI probe: TXI_shigemi
         
         
   3. Click Read
      

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Lock and Shim

1. Start rotation to help achieve better shimming. Type ro on
   
   
2. Type lock and select your lock solvent
   
   
3. If you use
   
   
   1. a normal 5 mm tube: type topshim
      
      
   2. a Shigemi tube: type topshim shigemi
      
      
      
4. If you will continue with 1D experiments, leave the sample spinning. For 2D experiments, turn off the rotation: ro off

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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!
   
   

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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Finish your work

Before leaving, you should insert the standard sample and lock:

1. spooler
2. qu lock off
3. qu ro off
4. qu sx 1
5. qu rsh TXI  (or BBO - as appropriate for the current probe)
6. qu lock cdcl3

You must watch the Spooler window for all commands to finish and the lock established before you exit Topspin!

 

 

 

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