Measuring 1H NMR spectra of samples in water (or mixtures of H2O and D2O) usually requires some form of solvent suppression of which selective presaturation is the most common method. In this technique, a long low power selective pulse is applied before the high power excitation pulse (or composite pulse). If too little power is used for presaturation, the water signal will not be sufficiently suppressed. If too much power is used, one loses intensity of signals close to the water resonance and foregoes the quantitative nature of the NMR data. The question then arises as to how much power is required for presaturation. The figure below shows the 300 MHz 1H NMR spectra of a plant extract in H2O/D2O measured as a function of presaturation power. The data were acquired on a Bruker AVANCE II console with the Bruker zgcppr pulse sequence using a two second presaturation pulse. The power levels are reported in dB and Hz.
One can see that at higher presaturation powers, one loses intensity for peaks near the water signal. In this case, where the nearest resonance of interest is 52 Hz from the water signal, one can obtain unattenuated signals with a presaturation field strength of 27 Hz. This corresponds to 58 dB on this instrument.
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More government support needed for research
Lethbridge Herald
Kay and his U of T colleagues have made advances in the field of biomolecular nuclear magnetic resonance (NMR) spectroscopy. They've developed ways to visualize protein molecules and how they can form abnormal structures that can lead to disease.
More government support needed for research - Lethbridge Herald
nmrlearner
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10-20-2017 01:48 PM
[Question from NMRWiki Q&A forum] Predicting aquisition time needed depending on sample concentration
Predicting aquisition time needed depending on sample concentration
Hi ,
is there a way of predicting aquisition time needed depending on sample concentration in order to get a decent spectrum for a 2D experiment for example?
Check if somebody has answered this question on NMRWiki QA forum
nmrlearner
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12-18-2014 11:22 PM
[Question from NMRWiki Q&A forum] 195Pt experiment setup help needed
195Pt experiment setup help needed
We just bought a new console (with Topspin 3.2)for our Bruker 400 and noticed that not all experiments that we previously used to run are setup on the new version. For instance, 195Pt experiment is not working. The message that appeared when we tried it was: "Cannot perform getprosol. The following files are not found. Observe pulses for 195Pt. DE and Trim pulses for 195Pt". Could any one help with the step-by-step procedure for setting up this experiment? Perhaps the probe file is not populated with pulses for 195Pt. We would greatly appreciate...
nmrlearner
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03-19-2014 10:43 PM
[U. of Ottawa NMR Facility Blog] Double Presaturation
Double Presaturation
Presaturation is a common method of reducing the water signal in the 1H NMR spectra of aqueous samples. Sometimes, a sample may contain more than one undesirable resonance which a user may want to presaturate. In such a case, one must presaturate at multiple frequencies simultaneously. On a two-channel Bruker spectrometer, two signals can be presaturated. This is accomplished by using both Signal Generation Units (SGUs). One of the undesirable signals is put on-resonance and is presaturated with the signal from SGU1 after which the hard pulse is given (also through...
nmrlearner
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03-16-2012 07:24 AM
[U. of Ottawa NMR Facility Blog] Watergate vs Presaturation
Watergate vs Presaturation
Biochemists and protein chemists are often interested in observing the NH protons in their samples. Since the NH protons usually undergo slow chemical exchange with water, it is desirable to run the samples in H2O rather than D2O so the NH protons will not exchange with the deuterium in the solvent which would make them invisible in the 1H NMR spectrum. In practice, a mixture of 10% D2O and 90% H2O is used as a solvent so that a deuterium lock can be established and used while running the spectrum. The very high concentration of water compared to the very low...
nmrlearner
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08-21-2010 08:15 PM
[U. of Ottawa NMR Facility Blog] Presaturation
Presaturation
One of the simplest and widely used ways to eliminate a strong water signal is to use presaturation. In this technique, the transmitter is set to the water resonance. a very long (seconds) low power (mW) pulse is given. The excitation profile of this pulse is very narrow due to its length and it saturates the water resonance at the transmitter frequency. A non-selective hard 90° pulse (with a wide excitation profile) is then given to place all remaining spins in the transverse plane for detection. An example of this is shown in the figure below. The top trace is a standard...
nmrlearner
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08-21-2010 08:15 PM
HELP!!!!! Probe Needed
I need a 300 MHz long bore broadband 1H carbon probe. Does anyone have one laying around they dont need anymore??????