Radiation damping causes broadening in the NMR resonances of very strong signals (such as the 1H signal of pure water) as a result of currents induced in the coil from the strong transverse magnetization. Radiation damping can also produce asymmetry and phase irregularities in the affected resonances. These problems make pulse calibration by the standard nutation curve problematic when very strong signals are used for the calibration. The left-hand panel (black) of the figure below shows the standard 1H nutation curves for 0.1% H2O in D2O (bottom) and 80% H2O in D2O (top). In both cases, single-scan spectra with a recycle delay of 30 sec were collected and plotted horizontally. The pulse was varied from 1 µsec to 24 µsec in steps of 1 µsec. In the case of 0.1% H2O in D2O, the nutation curve is well behaved and one is easily able to read off the 90°, 180°, 270° and 360° pulse durations. In the case of 80% H2O in D2O, where radiation damping is a problem, the nutation curve is not well behaved. There are asymmetry and phase distortion problems which make it impossible to determine the 90° pulse, based on maximum signal height, with any accuracy. Nor is it possible to determine a reliable 180° based on the first minimum. The spectra show very little distortion in the vicinity of the second minimum so the 360° pulse can be used reliably to determine the 90° pulse. The right-hand panel of the figure (red) shows the integrals of the corresponding nutation spectra. The integrals for both samples behave similarly. It is clear that even in the case of severe radiation damping, one is able to determine a well behaved nutation curve from the integrals.
[Question from NMRWiki Q&A forum] 15N 90 degree hard pulse calibration
15N 90 degree hard pulse calibration
Greetings, I want to ask for some advice in matter of 15N hard pulse calibration on Bruker machines. I'm working on Avance DRX 500 with 5mm TBI probe. This calibration is easy to made if 15N urea is avaible, but I don't have opportunity to use this compound. I have in my stable horses as follows:
methylamine hydrochloride (99% 15N) ammonium chloride (99,9% 15N) aniline (15N >99%) sodium nitrite (99% 15N)
I tried to use first two salts in DMSO-d6. Unfortunately I couldn't obtain proton spectrum with multiplet structure that is needed for pulse...
Radiation Damping in Modern NMR Experiments: Progress and Challenges
Radiation Damping in Modern NMR Experiments: Progress and Challenges
Publication year: 2012
Source:Progress in Nuclear Magnetic Resonance Spectroscopy</br>
V.V. Krishnan, Nagarajan Murali</br>
Highlights
? Overview of radiation damping effects in biomolecular NMR experiments. ? Theory and modifications of Bloch Equations. ? Current status, artifacts, control, applications as well as constructive uses of radiation damping.</br>
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06-15-2012 02:10 PM
Measurement of amide hydrogen exchange rates with the use of radiation damping
Measurement of amide hydrogen exchange rates with the use of radiation damping
Abstract A simple method for measuring amide hydrogen exchange rates is presented, which is based on the selective inversion of water magnetization with the use of radiation damping. Simulations show that accurate exchange rates can be measured despite the complications of radiation damping and cross relaxation to the exchange process between amide and water protons. This method cannot eliminate the contributions of the exchange-relayed NOE and direct NOE to the measured exchange rates, but minimize the...
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09-30-2011 08:01 PM
Radiation Damping on Cryoprobes
Radiation Damping on Cryoprobes
Publication year: 2011
Source: Journal of Magnetic Resonance, Available online 9 September 2011</br>
Dmitry*Shishmarev, Gottfried*Otting</br>
Radiation damping on 600 and 800 MHz cryoprobes was investigated. The phase angle ? between a vector 90phase shifted to the precessing magnetization and the rf field induced in the coil was found to depend markedly on whether an FID was being acquired or not. The magnitude of the radiation-damping field was sufficiently strong to restore 95% of the equilibrium water magnetization of a 90% H2O sample in a 5 mm...
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09-12-2011 09:00 PM
[Question from NMRWiki Q&A forum] How to study polymer degradation by gamma and X-Ray radiation?
How to study polymer degradation by gamma and X-Ray radiation?
Hi, I was asked to study polyethylene degradated by gamma and Xrays. I planed to measure relaxations rates, but which one is the most relevant to highlight chain degradation? T1, T2, but on 1H or 13C? By reading some articles, I feel T2 is not very interesting, right? T1rho experiments seems to give good results, I have found 2 sequences in Bruker's library, T1rhoX (CP step then variable length spin lock pulse on 13C channel) and T1rhoH (CP step then variable length spin lock pulse on 1H channel), and there is also the more...