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

Tue Aug 30 08:35:28 PDT 2022

Hi Tim,

For what it is worth, I seem to recall being told many years ago that over time the construction of cryoholders changed (perhaps the type of neck epoxy used?) and the recommended bake temperature changed with it.

Of course there are always the “more is better” folks, but I think it best to stick to the temperature recommendation and we use 100C.

Best,
- Dennis
---------------------------------
Dennis C. Winkler, PhD
National Institutes of Health
NIDCD
35A Convent Drive
Bldg. 35A, Room 1F-127, MSC-3745
Bethesda, MD  20892-3745, USA
Phone: (301) 451-7220
Email: Dennis.Winkler at nih.gov

From: 3dem <3dem-bounces at ncmir.ucsd.edu> on behalf of Tim Gruene <tim.gruene at univie.ac.at>
Organization: University of Vienna
Date: Tuesday, August 30, 2022 at 5:34 AM
To: Andrei Moiseenko <postmoiseenko at gmail.com>
Cc: "3dem at ncmir.ucsd.edu" <3dem at ncmir.ucsd.edu>
Subject: [EXTERNAL] Re: [3dem] Elsa 698 : best-practice bake-out procedure

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<mailto: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<mailto: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
>
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--

Best regards,
Andrey Moiseenko
Electron Microscopy Lab @ Biology Department
Moscow State University
postmoiseenko at gmail.com<mailto: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

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