HSQC-instructions

advertisement
HSQC – 15N-1H
1. Login
a. User – “nmrsu”
b. Password – “topspin”
2. Take cap off of the magnet
3. Bring up the “BSMS Suite”
4. Make sure that the LOCK is OFF.
5. Click “lift”
6. Replace current sample (or H2O/D2O placeholder) and put new sample in the
magnet.
7. Click “lift” to draw the sample into the magnet.
8. Put cap back on the magnet.
9. Set the temperature to what you want it to be (295/298K)
a. Should be there; type “edte” to change
10. Type “lock” to choose the solvent – 10% D2O/90% H2O
11. While the sample equilibrates to the desired temperature, copy your methods.
a. Open up a previous experiment
b. Type “edc” and enter the appropriate information (be sure to make a new
folder)
c. Copy both “trosy….” And “zgpr….”
12. Adjust field and phase (make it symmetrical)
a. Make sure that the lock is off.
13. Lock ON, manual.
14. Match and Tune – type “atmm” or “atma”  (auto)
15. Shim – “topspin gui”
a. 3D – new sample; 20 minutes. 10 minutes for a repeat.
b. “solvent suppression”
c. “1H”
16. Turn off the lock – adjust field and phase.
17. Find your “P1” - zgpr – “zg” GO
18. Do a quick 1D with your P1
a. “efp” to process 1D.
19. Adjust P1, P0, P29(?) in TROSY.
20. “zg” GO
21. “xfb” to process 2D spectra.
22. To process 1D spectra
a. Rser 1
b. Ssb 2
c. Sinm
d. Fp
16- NS 32?
16 – DS 32?
Download