The Figure below shows, in steps, how to correctly measure your sample using the depth gauge before putting it inside the magnet.
Sample Volume:
- 5 mm tube: 500-600 µL
- 3 mm tube: 180-200 µL
- 1.7 mm tube: 50-60 µL
Solids and bubbles are NOT welcome.
- Insert the sample [if using Sample Case (ASRC: 600 and 800 MHz): sx number (sx 2)].
- Press LIFT to eject (command ej) and inject (ij) directly. Obs: if using sample jet (ASRC: 700 MHz) — use Manual Mode on Firefox.
- Create your own folder (command new).
- Choose the solvent deuterium signal with the lock command.
- Tune and match the probehead (atma or atmm if required).
- Optimize the shim procedure: type topshim gui (check page 41 for more options).
- I usually use the options below for regular tubes (5, 3, and 1.7 mm tube), and when solvent suppression is required.
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- Or with parameters checked to shigemi (when using this type of tube).
Obs: If you regularly run one sample type, you can save your shim using the command wsh. Then, read the shim value every time you run this sample using the command rsh.
- Calibrate the pulse (pulsecal): AU-program to determine the 90° 1H-pulse in F1
Obs: pulsecal, works fine in samples that have a very strong singlet peak, but fails otherwise. It is therefore a very good alternative to the above for biological samples in 90:10% H2O:D2O. It is not recommended for samples in other solvents.