i like this post (click again to cancel)
i dont like this post (click again to cancel) remove favorite mark from this question (click again to restore mark)

there are two known mechanisms: friction heating( which may cause several degrees temperature increase) and induced AC current heating( in this paper:Electrical and ionic conductivity effects on magic-angle spinning nuclear magnetic resonance parameters of CuI. which can heat sample over 100 Celsius.) My question is, has any body seen this heating in MAS NMR?

asked Apr 29 '12 at 10:39

Jeffreyyyy's gravatar image


updated Apr 29 '12 at 10:39

3 Answers:
i like this answer (click again to cancel)
i dont like this answer (click again to cancel)

Sample heating is a typical problem in biomolecular solid state NMR. Heating due to spinning depends very much on the spinning speed. For a 3.2 mm rotor at 12 kHz it will be around 10 deg. Fast MAS with tiny rotors of 1.2 mm (~60 kHz ) produces ~ 50 deg of heating. However, a more serious problem is heating during RF irradiation. This might be very severe, and is especially pronounced for samples containing a lot of salt dissolved in your solvent. Usually the problems arise when long high-power decoupling pulses are applied during the sequence (for instance 100 kHz decoupling of protons for 30 ms of acquisition). As I said it might be quite severe, depending on your sample and experiment, but some extra 40-50 deg is not unusual. The best way to deal with it is to compensate heating by extra cooling of the sample. I hope this is helpful.

Update: check out this paper about heating effects in lipid membranes http://www.ncbi.nlm.nih.gov/pubmed/15366061


answered May 06 '12 at 09:07

Alexey%20Potapov's gravatar image

Alexey Potapov

updated May 10 '12 at 14:32

i like this answer (click again to cancel)
i dont like this answer (click again to cancel)

This is also a critical problem for MAS-NMR of paramagnetic species since the spectra are useless without the actual temperature in rotor. For high spinning rates (60kHz),we measured a 47°C difference between our controle unit and our actual temperature on one of our samples. We use NiCp2 as an NMR thermometer to know exactly the temperature inside the rotor.


answered Dec 16 '14 at 13:15

Thiazole's gravatar image


i like this answer (click again to cancel)
i dont like this answer (click again to cancel)

yes, it seems we met the same phenomenon, when there is the nano-tubes in the sample.


answered May 01 '12 at 03:29

Wendy%20Gong's gravatar image

Wendy Gong

Your answer
Please start posting your answer anonymously - your answer will be saved within the current session and published after you log in or create a new account. Please try to give a good answer, for discussions, please use comments and please do remember to vote (login to vote)
toggle preview



Asked: Apr 29 '12 at 10:39

Seen: 3,520 times

Last updated: Dec 16 '14 at 13:15

powered by CNPROG