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