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In solid-state NMR spectroscopy, magic-angle spinning (MAS) is a technique routinely used to produce better resolution NMR spectra. MAS NMR consists in spinning the sample (usually at a frequency of 1 to 130 kHz ) at the magic angle θ m (ca. 54.74°, where cos 2 θ m =1/3) with respect to the direction of the magnetic field .
A better alternative to the use of potentially hazardous oxidizers is an NMR tube cleaner (right). It is an apparatus which uses a vacuum to flush solvent and/or a detergent solution through the entire length of the NMR tube. In this apparatus, the NMR tube 1 (with the cap 3 fixed to the base of the NMR tube), is placed upside down on the ...
Solid-state 900 MHz (21.1 T [1]) NMR spectrometer at the Canadian National Ultrahigh-field NMR Facility for Solids. Solid-state nuclear magnetic resonance (ssNMR) is a spectroscopy technique used to characterize atomic-level structure and dynamics in solid materials. ssNMR spectra are broader due to nuclear spin interactions which can be categorized as dipolar coupling, chemical shielding ...
The NMR sample is prepared in a thin-walled glass tube – an NMR tube. An NMR spectrometer typically consists of a spinning sample-holder inside a very strong magnet, a radio-frequency emitter, and a receiver with a probe (an antenna assembly) that goes inside the magnet to surround the sample, optionally gradient coils for diffusion ...
Other NMR-active nuclei can also cause these satellites, but carbon is most common culprit in the proton NMR spectra of organic compounds. Sometimes other peaks can be seen around 1 H peaks, known as spinning sidebands and are related to the rate of spin of an NMR tube. These are experimental artifacts from the spectroscopic analysis itself ...
The spin interaction that is usually employed for structural analyses via solid state NMR spectroscopy is the magnetic dipolar interaction. [8] Additional knowledge about other interactions within the studied system like the chemical shift or the electric quadrupole interaction can be helpful as well, and in some cases solely the chemical shift has been employed as e.g. for zeolites. [9]
The effect is detected by NMR spectroscopy, usually using 1 H NMR spectrum, as enhanced absorption or emission signals ("negative peaks"). The effect arises when unpaired electrons (radicals) are generated during a chemical reaction involving heat or light within the NMR tube. The magnetic field in the spectrometer interacts with the magnetic ...
While 1D NMR is more straightforward and ideal for identifying basic structural features, COSY enhances the capabilities of NMR by providing deeper insights into molecular connectivity. The two-dimensional spectrum that results from the COSY experiment shows the frequencies for a single isotope, most commonly hydrogen (1 H) along both axes.
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