To carry on from Michael, you could also see if a less power-demanding
decoupling pulse sequence is sufficient, e.g Waltz will do 12 kHz which
equates to 200 ppm for 15N at 600 MHz which is more than likely adequate
to cover proton bearing nitrogens.
Regards,
K. Klika
________________________________________
> From: clarkson.michael via groups.io
> Sent: 04 November 2024 19:21:23
> To: main_at_ammrl.groups.io
> Subject: Re: [AMMRL] Pulse width variability
Adding my voice to the sample-heating hypothesis. Salt will increase the
susceptibility to this problem, particularly in a 5 mm tube. Given that you
are running a "fast" HSQC the balance between aq and d1 is something to
consider. If you have an NMR thermometer system you could test this directly;
alternately you could try cutting back 15N decoupling power (the default is
often higher than necessary), decreasing aq, increasing d1, or transferring
the sample to a 3 mm tube (shigemi or otherwise). Any of these should
attenuate or alleviate the problem.
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Received on Mon Nov 04 2024 - 09:31:30 MST