[3dem] Elsa 698 : best-practice bake-out procedure

[Tim Gruene]

Hi Andrei,

thanks a lot for sharing these details!

I was mostly curious about frequencies of the various steps (just
pumping / pumping and baking), and the temperature. My former PhD
student, Julian Wennmacher, would bake out zeolites at much higher
temperatures, and I would have guessed for 150C. So it is good to know
100C is recommended.

Best,
Tim

On Mon, 29 Aug 2022 22:48:21 +0300 Andrei Moiseenko
<postmoiseenko at gmail.com> wrote:

> Hi Tim, we use Elsa 698 with the Gatan 1905 controller and 655 pumping
> station. The bakeout temperature is kept at 100C, never exceeding it
> for more than a few degrees. We usually perform overnight bakeout
> once a week, but we pump out the holder dewar after each cryo-day. I
> think that it is ok for the holder to perform bakeout more often in
> case of extensive sample exchange. You definitely need to do the
> holder bakeout if: 1) The holder fails to reach the -170 C
> temperature within reasonable time. In our case ~45-50 min inside the
> pumping station, but may be different for your holder.
> 2) The holder cannot keep the cold temperature during operation
> 3) The frost or condensate forms on the holder dewar
> 4) The holder was not used for a couple of weeks.
> In case the holder was not used for a longer time or in case the
> overnight bakeout does not solve the temperature problem, the longer
> bakeout times should be used, like 48h or 72h.
> 
> пн, 29 авг. 2022 г. в 15:52, Tim Gruene <tim.gruene at univie.ac.at>:
> 
> > Dear all,
> >
> > we recently received our Gatan Elsa 698 holder. I would like to
> > gather some recommendations for daily use and bake-out procedure.
> > - what temperature do you use for bake-out?
> > - how long do you bake-out for?
> > - are there special maintenance procedures?
> > - what would be signs of deterioriation, abd after what period would
> >   they occur?
> >
> > We use the holder both for room-temperature and for
> > cryo-measurements.
> >
> > The manual refers to the Gatan pumping station, but ours was
> > delivered with a Pfeiffer pumping station ;-)
> >
> > Thanks a lot for your time!
> >
> > Best,
> > Tim
> >
> > --
> > --
> > Tim Gruene
> > Head of the Centre for X-ray Structure Analysis
> > Faculty of Chemistry
> > University of Vienna
> >
> > Phone: +43-1-4277-70202
> >
> > GPG Key ID = A46BEE1A
> > _______________________________________________
> > 3dem mailing list
> > 3dem at ncmir.ucsd.edu
> > https://mail.ncmir.ucsd.edu/mailman/listinfo/3dem
> >  
> 
> --
> 
> Best regards,
> Andrey Moiseenko
> Electron Microscopy Lab @ Biology Department
> Moscow State University
> postmoiseenko at gmail.com



-- 
--
Tim Gruene
Head of the Centre for X-ray Structure Analysis
Faculty of Chemistry
University of Vienna

Phone: +43-1-4277-70202

GPG Key ID = A46BEE1A
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