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

Tue Aug 30 13:00:11 PDT 2022

Hi Tim,

I agree 100% with Dennis.

Basically, baking any Gatan cryo holder, e.g., 626, 636, Elsa 698 above 100°C, i.e., 150°C, could mean expensive repairs for the holder. There are components soldered to the internal thermal conductor that are likely to be damaged if the holder is baked at elevated temperatures(above 100°C). 

I would stick with the 100°C bake out temperature, unless of course the Elsa’s user’s manual specifies otherwise.

I hope this helps.

Best,

Tom

Tom Schmelzer

TGS Technologies LLC

USA

724-453-3865

email: tom at tgstechnologies.net

From: 3dem-bounces <3dem-bounces at ncmir.ucsd.edu> on behalf of "dennis.winkler at nih.gov" <dennis.winkler at nih.gov>
Date: Tuesday, August 30, 2022 at 11:35 AM
To: Tim Gruene <tim.gruene at univie.ac.at>
Cc: "3dem at ncmir.ucsd.edu" <3dem at ncmir.ucsd.edu>
Subject: Re: [3dem] [EXTERNAL] Re: Elsa 698 : best-practice bake-out procedure

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> 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

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--

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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