Hi Shawn,
Welp - I can try to cobble an answer together (with caveats ) ; )
We have a similar 2-channel probe (Agilent HFX) that works well for 1H/19F
HOESY experiments. However, ( - CAVEAT - ) there is a 3-channel console
behind the probe. Note that HFX probe only has a single high-band RF input
connector (labelled PROTON) even though it is a dedicated 'HFX' probe that
can be dual-tuned to H and F. I'm not sure if this jives with what you have ; ).
If you do have the above gear, then there are a few steps that we take to set
everything up :
1.
As mentioned, we require a (minimum) three-channel spectrometer that is rigged
up to be CH1: high band, CH2: low band, CH3: high band. In this case, there are
two separate high-band RF pathways providing RF to / from the probe (i.e.
transmitter / amplifier / pre-amplifier, etc.). CH1 is set up to transmit H1,
while CH3 is set to transmit F19. CH2 can be any X-nucleus as usual (usually C13)
and is connected in the usual manner at the probe / RFFE.
2.
We feed the CH1 and CH3 high-band RF probe outputs (i.e. from the RFFE) into the
input ports of an RF splitter/combiner. The two inputs are combined to a single
output channel at the splitter / combiner and the CH1 and CH3 directional couplers
are then attached in series to the output of the splitter / combiner. An output
cable from the final directional coupler is then fed into the high-band (PROTON)
input connector at the probe.
3.
The probe (if autotunable) should have an additional tune rod for FLUORINE;
this should be hooked up to one of the motors at the Protune box so that
the probe can be dual-tuned to H1 and F19 in automation.
4.
The software does require some adjustment as well:
In this case, we adjust the VJ probefile such that the probestyle is 'hfx'
and then set probeConnect to 'H1 X F19'. This puts H1 and F19 on CH1 and CH3,
respectively. VJ should recognize this set-up for tuning purposes (i.e. the
tune pop-up GUI should then have a new 'H and F' button that can be clicked for
dual tuning to H and F). When done correctly, the 'Channels' GUI under the
Acquisition tab should show H1 as CH1 and F19 as CH3.
(Note that this presumes you also have separate tune calibration files for this
tuning arrangement. The tune calibration files will be different from the usual
dual resonance tune calibration file and may be on the original CDs / DVDs go
with the probe; admittedly it has been a while since I last looked at / for these.)
5.
pw90 calibrations are as usual from there ( . . . I typically run nutation
curves manually; expect slightly longer pws to accommodate dual tuning).
I feel like this may not be the 'be-all / end-all' and may be missing something
in the description. FWIW, this is meant to give a general sense of how to think
about setting up rather than an instruction manual; the usual disclaimers apply ; ) ).
(_at_anyone: feel free to jump in if you see something screwy ; ) )
Hope this helps,
Darcy
_________________________________
Darcy C. Burns, Ph.D.
Manager, CSICOMP NMR Facility
NEW BOOK! Optimizing NMR Methods for Structure Elucidation (Burns and Reynolds)
PURCHASE at
https://pubs.rsc.org/en/content/ebook/978-1-78262-539-1
University of Toronto
80 St. George Street
Toronto, ON
M5S 3H6
ph: (416)-978-0448
fax: (416)-978-8775
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Received on Mon Jul 21 2025 - 20:24:53 MST