thors.lab
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EtOEt leaking out of reagent bottle?
Hi,
I made some EtOEt a while back (about a year or so?) for an upcoming video, but then had to move back to uni and was unable to complete the video.
Placed the ether in a reagent bottle — the type with the big ass cap and polymer coating to prevent cracks — and wrapped the threads in teflon,
tightened it as hard as I could, and wrapped the whole thing in aluminum foil to prevent light. I put that in my garage.
Now it's summer, and I was moving things out of my garage to place in the attic. I came across the ether and decided to move it, but I didn't know
just where yet so I put it in my house for a couple days until I had organized a place to put it in a shed outside. (dumb I know, but it was only
temporary)
I noticed a smell of ether after a couple days, checked the ether and sure enough it was coming from there. The bottle cap felt loose.
Is it possible that with the summer being hot, enough pressure was able to build to literally loosen the cap? I'm now worried about autoignition —
especially because I wasn't able to fill the bottle fully (only about half way) so it had contact with oxygen and may have formed peroxides.
What should I do here? Just tighten the cap and but it away back outside? Or should I just dispose of it? Is there anything I can do to store it more
safely?
Thanks,
Thor
[Edited on 7-5-2020 by thors.lab]
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mackolol
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If you made it a year ago it probably has enough peroxides to not be useful.
And after all its boiling point is 34,6C, so it's super hard to store it, it's not recommended to store it for long time at all. And if you have to
it's good to put it in the freezer.
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B(a)P
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It is impossible to contain in any sort of a reagent bottle. Best to make it as required. If you wanted to store it you would be looking for storage
vessel suitable for a gas in an inert atmosphere.
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thors.lab
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Quote: Originally posted by mackolol  | If you made it a year ago it probably has enough peroxides to not be useful.
And after all its boiling point is 34,6C, so it's super hard to store it, it's not recommended to store it for long time at all. And if you have to
it's good to put it in the freezer. |
| Quote: Originally posted by B(a)P | | It is impossible to contain in any sort of a reagent bottle. Best to make it as required. If you wanted to store it you would be looking for storage
vessel suitable for a gas in an inert atmosphere. |
This is what I thought. Alright, disposal it is then — any tips on that? It's only like 250mL, should I just evaporate it outside? I don't want to
take any risks distilling with those peroxides in there so using it would be useless anyway. Unfortunately I don't have any KI right now and I want to
deal with this sooner rather than later.
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Herr Haber
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| Quote: Originally posted by mackolol | If you made it a year ago it probably has enough peroxides to not be useful.
And after all its boiling point is 34,6C, so it's super hard to store it, it's not recommended to store it for long time at all. And if you have to
it's good to put it in the freezer. |
Hard to store ?
When in a container pressure develops and the boiling point changes...
I've had 200ml in the bottom drawer of the fridge that has not changed for years. Sure, I'll test for peroxydes when I need it but besides that it's
ok.
DCM has a similar BP and is a pain to store too.
Not sure what happened to yours Thor butI wonder if the teflon didnt do more harm than good.
The spirit of adventure was upon me. Having nitric acid and copper, I had only to learn what the words 'act upon' meant. - Ira Remsen
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B(a)P
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From the sound of the description it was not in the fridge, which would obviously make a big difference.
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monolithic
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You can buy peroxide test strips on Amazon if you're concerned about peroxides, or you could could do a qualitative test with KI. Do some research but
if there's not a "lot" of peroxides in there, you can neutralize what little peroxides may be present by washing with ferrous sulfate or sodium
bisulfite or metabisulfite. You might find this paper useful. http://www.sciencemadness.org/talk/files.php?pid=153704&... And of course if there's a "lot" of peroxides in there, it's safest to dispose of
it.
In the future you could buy some BHT to inhibit peroxide formation. A lifetime supply is like $20 on Amazon since you only need a very small amount.
This is how it's stored commercially, with a tiny amount of BHT.
[Edited on 5-7-2020 by monolithic]
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thors.lab
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| Quote: Originally posted by B(a)P | | From the sound of the description it was not in the fridge, which would obviously make a big difference. |
I don't really want to put chemicals in my food fridge & I don't have a chemical minifridge. I would get one but I don't have much space to work
with, unfortunately. It would be nice to have a good place to store my stuff :/
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thors.lab
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| Quote: Originally posted by monolithic | You can buy peroxide test strips on Amazon if you're concerned about peroxides, or you could could do a qualitative test with KI. Do some research but
if there's not a "lot" of peroxides in there, you can neutralize what little peroxides may be present by washing with ferrous sulfate or sodium
bisulfite or metabisulfite. You might find this paper useful. http://www.sciencemadness.org/talk/files.php?pid=153704&... And of course if there's a "lot" of peroxides in there, it's safest to dispose of
it.
In the future you could buy some BHT to inhibit peroxide formation. A lifetime supply is like $20 on Amazon since you only need a very small amount.
This is how it's stored commercially, with a tiny amount of BHT.
[Edited on 5-7-2020 by monolithic] |
Thanks! I will be buying those preemptively before making ether next time. I've already evapped off the possibly dangerous stuff that's giving me a
hard time with storage.
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morganbw
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I think that there might be a slight Irish perversion of the sorts of just drinking it. Maybe no reason to waste.
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draculic acid69
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This is what I thought. Alright, disposal it is then — any tips on that? It's only like 250mL, should I just evaporate it outside? I don't want to
take any risks distilling with those peroxides in there so using it would be useless anyway. Unfortunately I don't have any KI right now and I want to
deal with this sooner rather than later.[/rquote]
Letting possibly peroxide tainted ether evaporate in or on anything sounds like a bad idea.better to destroy the peroxides first with some iron
sulfate.
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