Susceptibility Plugs with Methanol
Michael.Bernstein@astrazeneca.com
Thu, 9 Aug 2001 18:07:27 +0200
Dear All,
We have just taken delivery of a 3 mm probe, and want to extend our
low-concentration work from LC-NMR to this configuration. We've always done
well by 5 mm Shigemi tubes, and were keen to try the equivalent for 3 mm
tubes: Wilmad/Doty Susceptibility Plugs. We have used the plugs made from
G-10 (Wilmad PN SP-PR-G-3 and Doty 99851).
We use LC-NMR grade methanol, which we find to be very clean,
chemically. We "conditioned" the G-10 plugs & positioning rod with soaks
and washes in ethanol and methanol.
The problem is that we see a LOT of chemical interference leeching
from the plugs/positioning rod. On a ca. 5 ug solute sample, the
contaminating peaks would be _much_ more intense than the solute. And
there's a wide range of crap coming off the plugs: we see the biggest peaks
at 1.3 and 4.6 ppm, but less intense contamination giving rise to peaks at
0.9, 1.6, ca. 2, ca. 3, ca. 7, and 8 ppm
Has anyone out there had similar experience? Have you found good
cleaning conditions? Any experience would be appreciated.
Thanks a lot,
Mike
PS I am not aware of anyone making Shigemi-type tubes (all glass
construction) at 3 mm. M.