Re: AMMRL: Co59 NMR

From: Craig Grimmer <craig.grimmer_at_gmail.com>
Date: Fri, 12 Dec 2014 07:32:34 +0200

Hello Sheng

I suspect there's something wrong with the experiment setup, if your
hardware is appropriate and working correctly.

Start with whatever experimental setup you use for 13C (with decoupler off)
because that will give you a reasonable starting point for
pw90/tpwr/p1/pl1, change the observe frequency, tune, match, etc, then
increase the sweep with to something wide (~2000 ppm). For the
hexacyanocobaltate in H2O/D2O, you should see a sharp singlet with a single
pulse. The recycle time can be short (~500 ms) so you can adjust d1, aq,
np/td.

"I even got no signal from the standard..."; "even" implies that you've
tried something other than the standard. You must get the parameters
correct with the hexacyanocobaltate before looking for signals from
anything else. 59Co linewidths can be very large, 1000's Hz, because of
the quad moment, and difficult to find. Also, only Co3+ is suitable for
NMR, contamination with Co2+ will prevent observation.

Craig.


On 11 December 2014 at 00:06, Cai, Sheng <sheng.cai_at_marquette.edu> wrote:
>
> Hi,
>
>
>
> Did anybody run 59Co NMR before? I tried everything and it didn't work. I
> even got no signal from the standard K3Co(CN)6, which should give a sharp
> peak. My tuning is good and I am sure my probe is OK. Any trick I might be
> missing? Thanks.
>
>
>
> Sheng Cai
>
> Marquette University
>
> Milwaukee, WI 53233
>
Received on Thu Dec 11 2014 - 19:32:37 MST

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