Zoen melting at low temperatures

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oiggab_odracir
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Zoen melting at low temperatures

Post by oiggab_odracir » 11 Nov 2015, 13:03

Dear Fellows:

I need to grow some organic single crystals (suitable for a structural determination) al about -35ºC, below a glassy phase. I had thought of something like zone melting under a N2 flow, probably in a Lindeman tube.
Does anybody know of some (home made) suitable setup, from where to take some illuminating ideas?

Thanks in advance.
Ricardo

nils
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Joined: 20 Aug 2010, 09:30
Location: Zürich

Re: Zoen melting at low temperatures

Post by nils » 11 Nov 2015, 15:24

I've seen somebody here do it using a flame-sealed capillary, a glass pipette, some tubing and argon (at RT). For cooling the cryostream of the diffractometer was used. For monitoring he used diffraction, but you could also see the crystallization with the microscope camera. IIRC he taped the "nozzle" to a lab jack to repeatedly move it up and down. It took a while to figure out the temperature and Ar flow, but after that he could crystallize similar substances repeatedly. But be warned that the crystals might still be pooh pooh :-)

nils
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Re: Zoen melting at low temperatures

Post by nils » 11 Nov 2015, 15:25

Oh how I hate this profanity filter.

oiggab_odracir
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Joined: 13 Jul 2011, 18:56
Location: Buenos Aires

Re: Zoen melting at low temperatures

Post by oiggab_odracir » 11 Nov 2015, 16:24

Thanks, Nils, for your message...
By the way, I guess you did not mean "pooh pooh" after all?

nils
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Posts: 119
Joined: 20 Aug 2010, 09:30
Location: Zürich

Re: Zoen melting at low temperatures

Post by nils » 12 Nov 2015, 07:37

Well the meaning is still covered, only I don't really write like a three-year old :D

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