Hsin and AMMRLers,
We've setup adiabatic decoupling for 19F on our spectrometers, and have
posted some notes (which I should simplify) on this at
http://www.chem.wisc.edu/~cic/nmr/Guides/Ba3vug/AV3_19F-adia-dec-setup.pdf.
Not surprisingly, it is _much_ better than standard 19F decoupling.
Charlie
On 4/26/2017 4:35 PM, Hsin Wang wrote:
>
> Dear AMMRLs,
>
> I would like to make a summary to my post “H2-decoupled H1-spectrum on
> Avance III HD”. I have changed the subject title to “X-decoupled” to
> reflect that this is really a question about X-decoupling, including
> the special cases of H2-decoupling and also F19-decoupling which is
> possible with BBFO probe.
>
> I would like to thank Yizhou Liu, Sebastien Kemper, Clemens Anklin,
> Paul Cope, Bob Berno, and Wei Wycoff for their helpful advice.
>
> One condition that is perhaps most important with X-decoupling is that
> it uses more power. Clemens advises to set the acquisition time (AQ)
> between 0.25 and 0.5 seconds. A few others have pointed out that D1
> should be relatively long (low duty cycle) to allow adequate heat
> dissipation.
>
> --
>
> X-decoupling set up, excluding H2 and F19
>
> Two ways were described to me. The way I like better is to rpar
> either “PROP31DEC” or “PROB11DEC”. Then in edasp edit NUC2 to
> nucleus of interest. Make sure the pulse program is zgig. (This is
> also described in TopSpin Help Mannuals > “Pulse Program Catalogue,
> 1D/2D” > “Basic 1D pulse sequences, page 67”).
>
> Another way is rpar the H1-decoupled X-nucleus experiments, such as
> C13IG, N15IG, Si29IG or Sn199IG. The in edasp use the switch f1/f2
> button and change f2 to the nucleus of interest.
>
> It is possible the prosol table may not have that nucleus set up
> properly. One should enter the correct P90 for X observe and decouple,
> go to “square pulses” to enter desired PCPD. The ‘edprosol’ should
> calculate the power level properly.
>
> I had asked specifically about B11-CPD in a glass tube and was told
> that it is not a problem.
>
> --
>
> H2-decoupling of H1 spectrum
>
> I will just quote Clemens here:
>
> for the deuterium decoupling experiment (use “zgig2h” as the pulse
> sequence) you just select 2H as nucleus in F2 and click on default.
> This should correctly route the signal. You do not have to worry about
> the lock. This experiment will lock during the relaxation delay and
> decouple during acquisition all the switching is taken care of by the
> pulse program.
>
> --
>
> F19-decoupling H1 spectrum
>
> I have heretofore not discussed this with anyone. But I noticed there
> is an rpar “PROF19DEC”, which loads the pulse program “zghfigqn”. The
> program indicates QNP-operation (F19 – via X-QNP output of
> switchbox). I should probably verify that this is standard with BBFO
> and Avance III HD. If it is, then it seems straightforward. Except
> that one should probably be very careful of the CPD pulses because of
> the wide dispersion of F19 signal and avoid probe heating. Probably
> experts should be consulted anyway.
>
> Hsin
>
> --
>
> Hsin Wang, Ph.D.
>
> Center for Discovery and Innovation, Room 01304
>
> The City College of New York
>
> 85 St. Nicholas Terrace
>
> New York, NY 10031
>
> Phone: 212-650-5831
>
> Email: hwang1_at_ccny.cuny.edu
>
> *From:* Hsin Wang
> *Sent:* Monday, April 24, 2017 4:45 PM
> *To:* 'ammrl_at_ammrl.org' <ammrl_at_ammrl.org>
> *Subject:* H2-decoupled H1-spectrum on Avance III HD
>
> I would like to know how to set up H2-decoupled H1 experiment on a
> 2-channel Avance III HD spectrometer with a BBFO probe.
>
> I would also like to do X-decoupled H1-experiments on the same
> spectrometer.
>
> Perhaps these are fairly simple experiments. But I am not familiar.
> Any pointer (rpar, etc) would be greatly appreciated.
>
> Hsin
>
> --
>
> Hsin Wang, Ph.D.
>
> Center for Discovery and Innovation, Room 01304
>
> The City College of New York
>
> 85 St. Nicholas Terrace
>
> New York, NY 10031
>
> Phone: 212-650-5831
>
> Email: hwang1_at_ccny.cuny.edu <mailto:hwang1_at_ccny.cuny.edu>
>
--
~~~~~~~~~~~~~~~~~~~~~~~
Charles G. Fry, Ph.D. Tel: (608)262-3182
Director, MR Facility Fax: (608)262-0381
Chem. Dept., 1101 University Ave, Univ. Wisconsin-Madison
Madison, WI 53706 USA email: fry_at_chem.wisc.edu
Received on Thu Apr 27 2017 - 12:21:33 MST