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Page 4 of
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PREPARING
YOUR SAMPLE |
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Place
your sample in an NMR tube.
NMR spectra are,
as a rule, run in thin-walled glass tubes that are either 5-mm or 10-mm
in diameter. Though these look something like test tubes, they are not
the same. If your spectrometer can be set up for either of these two
sizes, make certain that you use the correct diameter. You can damage
the instrument by trying to load the wrong size.
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Select
a clean, dry NMR tube of the appropriate size and type. If your sample
is air- or light-sensitive, you may need to use a special tube. |
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Method
A: Using a spatula (for a solid sample) or pipet (for a liquid), place
a few milligrams of your sample into an NMR tube. If necessary, tap the
end of the tube to make most of the sample fall to the bottom. If you
need to know the exact concentration of your sample, weigh the tube as
you fill it. You should not usually fill the tube any higher than about
0.25" (0.2 cm) with a liquid or dry powder. |
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Using
a pipet, slowly drip the selected deuterated solvent until the liquid
level reaches a height of 1-2" (3-5 cm). Add a few drops of a chemical-shift
reference, if required. Place a plastic cap snugly on the tube. If your
sample does not dissolve immediately, mix the contents by inverting the
tube several times. |
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Method B:
Using a spatula (for a solid sample) or pipet (for a liquid), place a
few milligrams of your sample into a small glass vial. Add about 2 mL
of the appropriate deuterated solvent, and place the cap snugly onto the
vial. Shake. Pipet the resulting solution into an NMR tube, and cap. |
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Is
your solution clear and free of particles and other separated phases?
If not, then ask for help.
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