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Topic: NMR Chloroform  (Read 4448 times)

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Offline Messi

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NMR Chloroform
« on: October 22, 2012, 02:11:55 PM »
Hey guys,

How long can I leave my sample in chloroform before I put it in the NMR machine? Is it OK if I leave my sample in there for 2-3 hours then take the NMR of it?

How about 2-3 days?

Thanks!

Offline discodermolide

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Re: NMR Chloroform
« Reply #1 on: October 22, 2012, 02:14:46 PM »
Chloroform has a tendency to decompose to produce HCl and even phosgene. That's why the bottle has silver wool in it to help prevent this.
So 2-3 hours is OK but 2-3 days probably not. You can check this by NMR of course.
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Offline Babcock_Hall

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Re: NMR Chloroform
« Reply #2 on: October 22, 2012, 02:54:50 PM »
Some compounds degrade on their own; others react with some NMR solvents.  I have synthesized one that seemed to react with DMSO, but I did not fully characterize the process.

Offline OC pro

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Re: NMR Chloroform
« Reply #3 on: October 22, 2012, 03:59:12 PM »
For most of the compounds they are ok even for several weeks in the NMR tube. When I did PhD we had to wait sometimes for more than a week to get a 1H and 13C spec. I never saw any degradation in CDCl3. And I worked with highly sensitive pyrrole compounds.

Offline Messi

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Re: NMR Chloroform
« Reply #4 on: October 22, 2012, 05:09:45 PM »
Thanks guys. Good stuff! I'll def keep that in mind!

Regarding a C13 NMR, what's a good standard amount of time to leave my sample in the NMR machine for?

Offline OC pro

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Re: NMR Chloroform
« Reply #5 on: October 22, 2012, 05:13:44 PM »
Depends on the machine and of course sample amount. I you have enough material and use 50mg+ for 13C then ~100 scans should be ok. But for normal 10-20mg samples I would do at least make 1024 scans (~2h) for 13C and DEPT. So ~4h altogether.

Offline Messi

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Re: NMR Chloroform
« Reply #6 on: October 22, 2012, 09:44:53 PM »
Boy oh boy is your guys' help invaluable! You guys are simply awesome!

Thanks OC Pro! :)

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