1H Experiments with Fluorine
Decoupling
Measuring
1H spectra with fluorine
decoupling, or19
F spectra with proton decoupling differs from the
conventional heteronuclear decoupling, because the spectrometers have
only one highband amplifier, which has to be shared between the
proton and fluorine pulses. This will be taken care off by setting
homo=’y’. Other than that, the set-up procedure is similar to that of
normal decoupling.
- Collect a proton FID using the standard
parameters and process the data.
- Determine the spectral window you want to
observe. Using the left and right mouse buttons, bracket the
spectral range that you want to observe. Be aware, that peaks
outside your cursors may fold in, meaning they may appear with
strange phases at places in the spectrum, which do not correspond
to their true shifts. Typing
movesw will set the center
frequency and sweep width to correspond to your choice.
- jexp2 join an
other experiment, for example 2, if not used and collect a
standard fluorine experiment.
- Find the peak, which you want to decouple with
and set your cursor on it.
- nl
- movetof
- tof? will give
you the exact offset frequency, write it down.
- jexp1 go back to
your proton spectrum in experiment 1, if that was what you
used.
- dn=’F19’
- dof=enter the
offset, you found as tof in the fluorine experiment
- dm=’nny’ this
allows fluorine decoupling during the acquisition
- dmm=’c’ turns on
"continuos" wave decoupling (see remark below)
- homo=’y’allows
the use of the high band amplifier for both nuclei
- Next you need to find the minimum decoupler
power, that is sufficient for you to collapse the multiplet you
wish to decouple. You do this by
arraying
dpwr (see
PulseWidth / Delays on how to
array). Rough values to test may be between 40 and 49.
Do not go higher than 49 or you will
ruin the probe.
Now you are ready to get your data,
good luck
.
Remark:
You may want to use different decoupling schemes
( SIZE="-1">dmm= ‘w’,
(WALTZ-16), ‘m’,
(MLEV-16), or
‘g’, (GARP)).
For these it is important to set dmf
which corresponds the inverse of the
decoupling pulselenghts. Because of the necessity to share the
amplifier between both nuclei it is not possible for all sweepwidths,
to use all dmf values. We recommend, that you array dmf and optimize
the value for your goal. You may also want to do a fluorine
homonuclear decoupled experimentwith, to see, which fluorine
resonances are effected with your values of choice.
The following table gives you an idea about
possible decoupler settings for the standard sweepwidth (4801 Hz).
Optimize the parameters for your system.
|
decoupler scheme
|
dpwr
|
max dmf that gives decoupling
|
|
C
|
48
|
not used
|
|
W
|
48
|
400
|
|
G
|
48
|
100
|
|
m
|
48
|
400>
|
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Last updated: April 1st, 1998
URL: http://nmr.chem.indiana.edu/NMRguide/1dexpt/HF.html
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The Trustees of Indiana University