Hi, I have question for you who have Bruker instruments! On 300 MHz I worked on selective noesy pulse sequence (selnogp) and it worked perfectly (d20=0.05s, pl14=62dB and p12=90ms). When I tried it to do on 600 MHz, it did not work. Please, help me to understand it! Marijana asked Feb 04 '14 at 02:52 gugica |
In principle it should work as well. Please, check: 1. D8 (mixing time) 2. Edprosol and check shaped pulses and their power 3. Gradient values 4. If probe is tuned and matched 5. This is essential: check that you properly set O1 and SR equals to 0, sometimes when one creates experiment from proton with calibrated scale non-zero SR plus measured center of peak would lead to wrong O1. answered Feb 04 '14 at 22:41 VVK |
Assuming that all of your pulses (both the hard pulses and shaped pulses) and everything else are calibrated properly, it could be that at 600 MHz you are now at the cross-over point between extreme narrowing and spin-diffusion. What is the molecular weight of your compound, and what solvent are you using? The easiest way to set up these experiemnts is with the selective panel, available from the "Spectrometer" menu. This will only work if you have a properly setup prosol table, however. If you are at the cross-over point, a ROESY experiment may work. answered Feb 05 '14 at 11:52 Kirk Marat |
Thank you for your answer! Molecular weight of my compound is 300 and solvent is DMSO! I will check all the pulses and try again! Have a nice day, Marijana answered Feb 12 '14 at 05:05 gugica DMSO is not a good solvent for doing NOE at high field, simply because of the cross-over effect. You can also try raising the temperature to make the DMSO less viscous and hopefully get you back into the extreme narrowing region. - Kirk Marat (Feb 13 '14 at 13:17) |
Do you see the signal from the selected peak and nothing else, or do you see nothing at all? If it's just that the NOE is zero under your conditions on the 600, then you should at least see the inverted peak, with reasonable intensity (you will lose some signal due to relaxation during the selective pulse and mixing time). You could also run the simple selective gradient spin echo pulse program selgpse - just copy the dataset used for the selective noesy and change the pulse program. If that doesn't give a decent signal, then likely there is a problem with the setup of the selective step. answered Feb 13 '14 at 14:58 Pete Gierth |