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<p class="MsoNormal">Hi Tim,<o:p></o:p></p>
<p class="MsoNormal"><o:p> </o:p></p>
<p class="MsoNormal">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.<o:p></o:p></p>
<p class="MsoNormal"><o:p> </o:p></p>
<p class="MsoNormal">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.<o:p></o:p></p>
<p class="MsoNormal"><o:p> </o:p></p>
<p class="MsoNormal">Best,<o:p></o:p></p>
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<p class="MsoNormal">- Dennis<o:p></o:p></p>
<p class="MsoNormal">---------------------------------<o:p></o:p></p>
<p class="MsoNormal">Dennis C. Winkler, PhD<o:p></o:p></p>
<p class="MsoNormal">National Institutes of Health<o:p></o:p></p>
<p class="MsoNormal">NIDCD<o:p></o:p></p>
<p class="MsoNormal">35A Convent Drive<o:p></o:p></p>
<p class="MsoNormal">Bldg. 35A, Room 1F-127, MSC-3745<o:p></o:p></p>
<p class="MsoNormal">Bethesda, MD 20892-3745, USA<o:p></o:p></p>
<p class="MsoNormal">Phone: (301) 451-7220<o:p></o:p></p>
<p class="MsoNormal">Email: Dennis.Winkler@nih.gov<o:p></o:p></p>
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<p class="MsoNormal"><o:p> </o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt"><b><span style="font-size:12.0pt;color:black">From:
</span></b><span style="font-size:12.0pt;color:black">3dem <3dem-bounces@ncmir.ucsd.edu> on behalf of Tim Gruene <tim.gruene@univie.ac.at><br>
<b>Organization: </b>University of Vienna<br>
<b>Date: </b>Tuesday, August 30, 2022 at 5:34 AM<br>
<b>To: </b>Andrei Moiseenko <postmoiseenko@gmail.com><br>
<b>Cc: </b>"3dem@ncmir.ucsd.edu" <3dem@ncmir.ucsd.edu><br>
<b>Subject: </b>[EXTERNAL] Re: [3dem] Elsa 698 : best-practice bake-out procedure<o:p></o:p></span></p>
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<p class="MsoNormal" style="margin-left:36.0pt">Hi Andrei,<o:p></o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt"><o:p> </o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt">thanks a lot for sharing these details!<o:p></o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt"><o:p> </o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt">I was mostly curious about frequencies of the various steps (just<o:p></o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt">pumping / pumping and baking), and the temperature. My former PhD<o:p></o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt">student, Julian Wennmacher, would bake out zeolites at much higher<o:p></o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt">temperatures, and I would have guessed for 150C. So it is good to know<o:p></o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt">100C is recommended.<o:p></o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt"><o:p> </o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt">Best,<o:p></o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt">Tim<o:p></o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt"><o:p> </o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt">On Mon, 29 Aug 2022 22:48:21 +0300 Andrei Moiseenko<o:p></o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt"><<a href="mailto:postmoiseenko@gmail.com">postmoiseenko@gmail.com</a>> wrote:<o:p></o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt">Hi Tim, we use Elsa 698 with the Gatan 1905 controller and 655 pumping<o:p></o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt">station. The bakeout temperature is kept at 100C, never exceeding it<o:p></o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt">for more than a few degrees. We usually perform overnight bakeout<o:p></o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt">once a week, but we pump out the holder dewar after each cryo-day. I<o:p></o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt">think that it is ok for the holder to perform bakeout more often in<o:p></o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt">case of extensive sample exchange. You definitely need to do the<o:p></o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt">holder bakeout if: 1) The holder fails to reach the -170 C<o:p></o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt">temperature within reasonable time. In our case ~45-50 min inside the<o:p></o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt">pumping station, but may be different for your holder.<o:p></o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt">2) The holder cannot keep the cold temperature during operation<o:p></o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt">3) The frost or condensate forms on the holder dewar<o:p></o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt">4) The holder was not used for a couple of weeks.<o:p></o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt">In case the holder was not used for a longer time or in case the<o:p></o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt">overnight bakeout does not solve the temperature problem, the longer<o:p></o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt">bakeout times should be used, like 48h or 72h.<o:p></o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt"><o:p> </o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt">пн, 29 авг. 2022 г. в 15:52, Tim Gruene <<a href="mailto:tim.gruene@univie.ac.at">tim.gruene@univie.ac.at</a>>:<o:p></o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt"><o:p> </o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt">> Dear all,<o:p></o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt">><o:p> </o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt">> we recently received our Gatan Elsa 698 holder. I would like to<o:p></o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt">> gather some recommendations for daily use and bake-out procedure.<o:p></o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt">> - what temperature do you use for bake-out?<o:p></o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt">> - how long do you bake-out for?<o:p></o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt">> - are there special maintenance procedures?<o:p></o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt">> - what would be signs of deterioriation, abd after what period would<o:p></o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt">> they occur?<o:p></o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt">><o:p> </o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt">> We use the holder both for room-temperature and for<o:p></o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt">> cryo-measurements.<o:p></o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt">><o:p> </o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt">> The manual refers to the Gatan pumping station, but ours was<o:p></o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt">> delivered with a Pfeiffer pumping station ;-)<o:p></o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt">><o:p> </o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt">> Thanks a lot for your time!<o:p></o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt">><o:p> </o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt">> Best,<o:p></o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt">> Tim<o:p></o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt">><o:p> </o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt">> --<o:p></o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt">> --<o:p></o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt">> Tim Gruene<o:p></o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt">> Head of the Centre for X-ray Structure Analysis<o:p></o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt">> Faculty of Chemistry<o:p></o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt">> University of Vienna<o:p></o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt">><o:p> </o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt">> Phone: +43-1-4277-70202<o:p></o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt">><o:p> </o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt">> GPG Key ID = A46BEE1A<o:p></o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt">> _______________________________________________<o:p></o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt">> 3dem mailing list<o:p></o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt">> <a href="mailto:3dem@ncmir.ucsd.edu">
3dem@ncmir.ucsd.edu</a><o:p></o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt">> <a href="https://urldefense.com/v3/__https://gcc02.safelinks.protection.outlook.com/?url=https*3A*2F*2Fmail.ncmir.ucsd.edu*2Fmailman*2Flistinfo*2F3dem&data=05*7C01*7Cdennis.winkler*40nih.gov*7Ca83f6bf7b6d94d3a577f08da8a6ad49f*7C14b77578977342d58507251ca2dc2b06*7C0*7C0*7C637974488707634941*7CUnknown*7CTWFpbGZsb3d8eyJWIjoiMC4wLjAwMDAiLCJQIjoiV2luMzIiLCJBTiI6Ik1haWwiLCJXVCI6Mn0*3D*7C3000*7C*7C*7C&sdata=yxPalkI9oIousKw*2Bw*2F6qoZv8Tyuf4GrlSqQKQ8VXHAU*3D&reserved=0__;JSUlJSUlJSUlJSUlJSUlJSUlJSUlJSUl!!Mih3wA!EN1pefz6bZeDZNRbYkGoqUCJ8mA697VPx9sZ2N04agOhq18CkFbBx6ySKdb2OPVo46C7S3rZVTSO0YfBFsdijyxWWNjo$">
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<p class="MsoNormal" style="margin-left:36.0pt">--<o:p></o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt"><o:p> </o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt">Best regards,<o:p></o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt">Andrey Moiseenko<o:p></o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt">Electron Microscopy Lab @ Biology Department<o:p></o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt">Moscow State University<o:p></o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt"><a href="mailto:postmoiseenko@gmail.com">postmoiseenko@gmail.com</a><o:p></o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt">--<o:p></o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt">--<o:p></o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt">Tim Gruene<o:p></o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt">Head of the Centre for X-ray Structure Analysis<o:p></o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt">Faculty of Chemistry<o:p></o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt">University of Vienna<o:p></o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt"><o:p> </o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt">Phone: +43-1-4277-70202<o:p></o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt"><o:p> </o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt">GPG Key ID = A46BEE1A<o:p></o:p></p>
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<p class="MsoNormal" style="margin-left:36.0pt">CAUTION: This email originated from outside of the organization. Do not click links or open attachments unless you recognize the sender and are confident the content is safe.<o:p></o:p></p>
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