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.
- Type edhead on a Topspin command line. The dialog window appears:
- 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
- To quit this dialog
- click Exit
- 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
"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) |
"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) |
Step 3. Insert your sample, load shims, and lock
Before operating the SampleCase - please, review these guidelines: SampleCase training
- Turn off lock and rotation:
- ro off
- lock off
For regular NMR tubes shorter than 9 inches: use SampleCase
For J. Young tubes and other tubes longer than 9 inches: bypass SampleCase
Follow the Manual Insertion guidelines with these modifications:
After the sample is inserted
- Type lock and select your lock solvent
Step 4. Create a new experiment
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
Step 6. Shimming
Step 7. Adjust Parameters