Proton observe and F19 CW or CPD decoupling
(This experiment is available on B400b)
(A) In ICONNMR way.
1. Set up a first experiment: F19CPD.
2. Set up a second experiment: PROTON. Set ns = 5000 so that the experiment will keep the sample in the magnet and let you have time to look at the F19CPD spectrum.
Do not yet set up the third experiment: PROTONF19CWDEC.
3. Submit the first two experiments.
4. Start the run.
5. Wait until the F19CPD experiment finishes.
6. Display the F19CPD spectrum.
7. Get the ‘o1p’ value (the exact shift in ppm’s) of the interesting peaks.
8. Set up a third experiment, PROTONF19CWDEC, and set o2p = the value of ‘o1p’ obtained from the last step.
9. Similarly set up more PROTONF19CWDEC experiments if there are more peaks of interest.
10. Submit these PROTONF19CWDEC experiments.
11. Read in the PROTON experiment currently running (click “FID”). Click “halt” (not “stop”!). The PROTON will be stopped and PROTONF19CWDEC will automatically start.
12. Compare PROTON and PROTONF19CWDEC spectra with multi-spectra display and see the difference. Only the H1 splitting due to the coupling of the irradiated F19 should collapse.
(B) In TOPSPIN way:
(B) In TOPSPIN way:
Make sure that the solvent is consistent in all the experiments. After lock and shimming finishes, run the following three experiments:
(1) Get F19 chemical shift for decoupling
Exp 10 1
‘rpar F19CPD all’ ‘getprosol’ ‘ii’ ‘rga’ ‘zg em ft’ phase.
Use “Set RF from cursor” to determine o1p of the F19 peaks.
Write down the O1p values for all the peaks interested.
(2) Get H1 spectrum with no F19 decoupling
Exp 20 1
‘rpar PROTON all’ ‘getprosol’ ‘ii’.
Change PulseProg ‘zg30’ to ‘zg’
‘rga’ ‘zg em ft’ phase.
write down the ‘rg’ value.
(3) Get H1 spectrum with F19 CW decoupling
Exp 30 1
‘rpar PROTONF19CWDec all’, ‘getprosol’, ‘ii’.
Set o2p = the value of ‘o1p’ obtained from the step (1).
Set ‘rg’ = the value obtained in step (2).
‘zg em ft’ phase.
Compare the H1 spectrum to one without F19 decoupling (step 2).
Only the H1 splitting due to the coupling of the irradiated F19 should collapse.