Jhana
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Storing Diethyl Ether, some questions
I realize this has been discussed a fair bit all over the web. I've spent quite a bit of time searching and studying this before posting but still
have some specific details I would appreciate resolved by a knowledgeable party.
I have 4 glass vials of anhydrous Diethyl Ether, 99.9%.
3 are 30ml Kimax test tubes, 1 is 10ml generic flat bottom glass storage vial.
Each sealed with a cap of some form of very hard dense plastic that screws on.
Electrical tape is wrapped to enhance the cap seal.
The vials are wrapped with solid white label stock to prevent any light from entering.
1. First question regards the escaping ether vapors. Despite the containers being well sealed it is clear by the smell that vapor is escaping. If the
vials are placed in a small closed container/box for even a short time, when the container is opened the smell is very strong.
How much actual material is escaping? Is it a sufficient amount to be able to accumulate to an explosive volume? Or is this amount small enough that
it will disperse sufficiently over time? Is this simply aromatic or is it enough vapor that requires special storage / ventilation?
To keep the vials safe from damage/breakage I am inclined to store them in a small clam shell sunglasses type enclosure that is lined with soft
padding. Is this safe? Is the build up of vapors in that small enclosure dangerous? Is it essential to keep the vials fully exposed to moving
ventilated air so absolutely no vapors build up anywhere?
2. Is it safe to keep the ether in the vials with the screw on caps sealed tight or is there danger from pressure build up? The vials are filled to
the top with very little air space. I would expect more danger from pressure with larger containers, I'm wondering if since these are relatively small
containers with little air space is pressure build up something I should worry about?
3. Is it safe to leave the electrical tape wrapped around the cap/vial? Logically the vapor must be escaping through the seal where the cap presses
against the top edge of the vial, then the threads of the cap, and then through the electrical tape. How much will the vapors degrade the electrical
tape? If the electrical tape is reducing the amount of vapor that escapes I would prefer to keep it on, but is there any danger on this?
I want to store them in as protected environment as possible, but also allow as much ventilation as possible.
My concern is if vapor is leaking even very slowly will it build up in an enclosed space over a long period such as several weeks?
Any advice for my specific situation is appreciated.
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woelen
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I would buy a 100 ml bottle with a good screw cap, which preferrably has an aluminium-coated liner inside the cap. At least you should put all the
ether in one vial. Now you have 4 points of vapor loss, putting it in a singe bottle reduced this to one point of vapor loss. if you cannot find a
bottle with aluminium-coated liner in the cap, then you can cut a nice circle of aluminium foil, which just covers the opening of the bottle and the
glass rim. Then put this on the opening and then put on the screw cap. This thin liner has no influence on the mechanical connection between the cap
and the glass, but it largely prevents loss of ether-vapor. Ether does not react with aluminium and it does not pass through it. Many plastics do not
perfectly block ether, the chemical can be absorbed a little by the plastic and through this mechanism some vapor may be released as well.
Ether is a nasty on storage. Even with very good bottles you still can smell the vapors. Fortunately, the vapors are virtually non-toxic and our nose
is very sensitive to these vapors, so even very low concentrations can be smelled. But in the long run (over weeks or months) there indeed can be
buildup of vapor concentrations such that explosion is possible when these vapors are ignited.
I would put the single 100 ml bottle in a garage or other fairly large room, which is opened frequently, but where you do not spend your whole day. In
a large room which is opened frequently you do not have to worry about vapor buildup as long as the bottle remains closed.
[Edited on 23-8-12 by woelen]
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Jhana
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Thank you.
So the vapor loss shouldn't be too much of concern for the next 24-48 hours? I may be being overly cautious, but want to be sure.
What about tightly wrapping the vials in aluminum foil until ideal conditions can be arranged, any unusual dangers with that?
I wrapped the tops tightly in aluminum foil, when I sniff at the cap now the scent seems to be significantly reduced. My only thought is the potential
for the foil attracting a static discharge.
I should note this is HPLC grade, I am pretty sure it is inhibitor free.
Quote: Originally posted by woelen  | I would buy a 100 ml bottle with a good screw cap, which preferrably has an aluminium-coated liner inside the cap. At least you should put all the
ether in one vial. Now you have 4 points of vapor loss, putting it in a singe bottle reduced this to one point of vapor loss. if you cannot find a
bottle with aluminium-coated liner in the cap, then you can cut a nice circle of aluminium foil, which just covers the opening of the bottle and the
glass rim. Then put this on the opening and then put on the screw cap. This thin liner has no influence on the mechanical connection between the cap
and the glass, but it largely prevents loss of ether-vapor. Ether does not react with aluminium and it does not pass through it. Many plastics do not
perfectly block ether, the chemical can be absorbed a little by the plastic and through this mechanism some vapor may be released as well.
Ether is a nasty on storage. Even with very good bottles you still can smell the vapors. Fortunately, the vapors are virtually non-toxic and our nose
is very sensitive to these vapors, so even very low concentrations can be smelled. But in the long run (over weeks or months) there indeed can be
buildup of vapor concentrations such that explosion is possible when these vapors are ignited.
I would put the single 100 ml bottle in a garage or other fairly large room, which is opened frequently, but where you do not spend your whole day. In
a large room which is opened frequently you do not have to worry about vapor buildup as long as the bottle remains closed.
[Edited on 23-8-12 by woelen] |
[Edited on 23-8-2012 by Jhana]
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woelen
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Try to arrange a good bottle for the ether in the next one or two days. In the meantime you can wrap the vials in aluminium foil, assuring that they
are completely enclosed in foil. Keep the vials upright, so that no liquid gets in contact with the caps of the vials. I this way you can store them
safely for a few days, but I would not keep them in that way for weeks.
If the foil is tightly wrapped and the vials are stored in a normal room, not in an enclosing container, then there is no need to worry about vapor
buildup. If the smell is uncomfortable to you, just store the vials in another room where you do not stay a large part of the day. There is no need to
worry about a static discharge igniting the vapors.
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Pyro
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empty medicine bottles can be used if you can't find any proper ones.
just wash and dry them out well before use
all above information is intellectual property of Pyro.  |
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ScienceHideout
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Dude- I have 100 mL of ether- I am not at all worried about the vapor... If you store it all together in a proper bottle with a phenolic cap you
wouldn't have any probs.
I would be mainly concerned that peroxides might form. I keep all my ether over KOH... it prevents peroxides.
hey, if you are reading this, I can't U2U, but you are always welcome to send me an email!
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Jhana
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Thanks for all the advice.
They appear to have come with a phenolic cap.
Will aim for a 100ml amber bottle and line the cap with aluminum.
But why not use a completely aluminum cap then?
Is there a preferred procedure for mixing the KoH and ether?
[Edited on 23-8-2012 by Jhana]
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Pyro
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just throw in some dry KOH.
nope, plastic seals better than all Al. Al just doesn't react to ether as plastic might get attacked by the ether
all above information is intellectual property of Pyro. |
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woelen
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A cap, completely made of aluminium would never exactly match the glass thread and there would always be an air-gap between the glass and the
aluminium cap. For this reason, I also mentioned that when you cut a circle of aluminium foil you should make it large enough to cover the opening of
the bottle and the rim, but it should not cover the thread of the bottle. The bottle of ether I have has a cap with an aluminium liner and this keeps
the ether in quite well. Over several years of storage I did not have noticeable loss of ether.
Diethyl ether can form peroxides, but the risk of that is not that high as some people suggest. In the Netherlands ether is an OTC chemical, used for
degreasing purposes and especially the last years it has become more popular, because of the 'green' nature of this chemical. It is virtually
non-toxic and it is non-corrosive and replaces chemicals like trichloroethylene, ligroin and all kinds of aromatics. In all those households without
knowledge of chemistry never one case of peroxide explosion occurred. If such a thing only happens once, then diethyl ether will disappear from the
shelves at once!
As far as I know the diisopropyl ether is much more prone to peroxide formation and that ether is more dangerous on storage.
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Jhana
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Great, thank you everyone for your time and effort. I have a much better understanding now.
Two final points and I should be set.
On the KOH, I assume it has absolutely no reactivity with the Ether? Any phenomena at all to know about over time?
Is it safe to understand that the KOH will remain at the bottom of the container and any Ether drawn off the top will be unaffected by the KOH?
(Will be using USP grade KOH, not the best but will do.)
I'm familiar with Borosilicate but am also seeing 'soda-lime glass', is there a type of glass that is known to be the most ideal for Ether?
Does Ether penetrate the glass at all, even a little?
If so is there a type of glass Ether will not penetrate?
Thanks again, I've read so many MSDS's and data sheets, but didn't come across the points asked about here, maybe I missed them.
Perhaps to make this thread more valuable to someone else looking for info on Diethyl Ether here's the collection of excellent data sheets I poured
through.
Standard Operating Procedure for work with Diethyl Ether Duke.edu
Read online Google Docs
http://tinyurl.com/ethersop
Direct .DOC download
http://www.safety.duke.edu/OHS/Documents/SOP/SOP%20Diethyl%2...
http://www.ed.ac.uk/schools-departments/health-safety/guidan...
http://www.sciencelab.com/msds.php?msdsId=9927164
Another forum discussion with some good coverage on the Ether subject
http://www.chemicalforums.com/index.php?topic=55583.0
http://anesthesiageneral.com/ether/
http://www.osha.gov/SLTC/healthguidelines/ethylether/recogni...
http://www.chemicalbook.com/ChemicalProductProperty_EN_CB685...
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paw_20
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Ethers (not epoxides though) are inert to the vast majority of reagents, including bases, which is one reason diethyl ether is a good solvent. Strong
acids cleave, and that's about it. I imagine USP grade KOH would be fine. Although I would add some molecular sieves or other drying agent as well, to
keep the ether anhydrous
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Magic Muzzlet
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If you store your Et2O over KOH a flocculent precipitate forms and you must distill the material before use. This has happened to me with homemade
ether, commercial stabilized with BHT, and also with the commercial anhydrous material after distillation so I think it always occurs with KOH. Sieves
or Na are better to keep in the bottom of the bottle.
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Mailinmypocket
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Manufacturer bottles not adequate?
I just bought a bottle of diethyl ether last week, from a reputable chemical supplier. When I picked it up I could smell ether on the outside of the
box! When I opened it up it was very well packaged in a glass reagent bottle with a black phenolic cap, inside a heavy duty plastic bag. The supplier
also wrapped the cap in parafilm, yet still, the smell is very noticeable around the cap and somewhat noticeable in the room where it is stored.
I opened the bottle to check the seal and it is in good condition with a silvery plastic liner. I'm not so much concerned with explosive vapor buildup
as I am with losing the ether slowly through the cap, and the somewhat annoying ever present smell. Storing it outside is not an option, and in a
fridge is a big no-no. Does anyone/has anyone ever had this problem and found a way to stop the damned bottle from making their lab have the slight
smell of an Exxon station? :S
I wrapped the cap in Teflon tape very tightly and it still smells, maybe now a layer of tight black electrical tape on top of that?
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woelen
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As I wrote before in this thread, aluminium foil does the trick. Line the cap with clean aluminium foil in such a way that the rim of the bottle is
covered, but not the thread. I'm quite sure that this reduces the smell of ether vapor considerably.
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Mailinmypocket
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| Quote: Originally posted by woelen | | As I wrote before in this thread, aluminium foil does the trick. Line the cap with clean aluminium foil in such a way that the rim of the bottle is
covered, but not the thread. I'm quite sure that this reduces the smell of ether vapor considerably. |
Sorry- I somehow missed where you said that, my apologies as I went back and read that. I will give it a try then. I find it curious that a well known
company like Fluka would not think to do this beforehand. Their warehouse must reek or the stuff.
Thank you!
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Endimion17
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I remember when my college bought ether, I think it was made by Fluka, and it came in aluminium bottles with plastic aluminium caps with aluminium
tops on the inside.
As long as you don't open your bottles frequently, and keep your ether in tightly closed bottles of appropriate size, the buildup of peroxides is
minimal.
All this peroxide scare is because of college laboratories keeping 200 ml of ether in 1-2 litre bottles and then using it for extractions and
distillations. Of course that's dangerous.
However if there's a small amount of air above a considerable amount of ether (900 ml ether, 1L bottle; 75ml ether, 100 ml bottle) and the cap fits
tightly so that the vapors hardly ever get out, the danger is extremely reduced.
Ether is not a boogeyman, people.
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mr.crow
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Try wrapping the plastic cap with metal tape (the one you are actually supposed to use on ducts) then wrapping the outside of the cap to the bottle
with the tape. Metal seal! The glue may get dissolved eventually
Double, double toil and trouble; Fire burn, and caldron bubble
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Mailinmypocket
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Problem solved thanks to aluminum foil I simply screwed on the cap with a piece
of foil a bit too large, removed the "cast" of the bottle mouth, cut it to size and voila! Metal cap insert! Then wrapped in Teflon and then
electrical tape, only a very very slight smell can be detected on the outside which is fine. Thanks Woelen!
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DraconicAcid
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And if the cap gets stuck, never, EVER try using a heat gun to loosen it.
One of my coworkers was thrown out of a lab for attempting this stunt.
Please remember: "Filtrate" is not a verb.
Write up your lab reports the way your instructor wants them, not the way your ex-instructor wants them.
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Mailinmypocket
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| Quote: Originally posted by DraconicAcid | And if the cap gets stuck, never, EVER try using a heat gun to loosen it.
One of my coworkers was thrown out of a lab for attempting this stunt. |
Oh, was this because he finished huffing on the other bottles and needed to wet his rag with a new bottle?  what a stupid thing to do!
Back when I was in school we had a teacher who had once used permanent marker on a whiteboard by accident and used ether to wipe it away. Burners were
in use at a moderate distance but for christs sakes, didnt he ever hear of ethanol!!? It could have been a disaster. I mean... Pouring it onto brown
paper towel, walking across the lab to the whiteboard and cleaning it.
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DraconicAcid
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| Quote: Originally posted by Mailinmypocket |
Oh, was this because he finished huffing on the other bottles and needed to wet his rag with a new bottle? what a stupid thing to do!
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No- this was a grad student of the "demented genius" type. He was a brilliant chemist, as long as you didn't actually see him working in the lab....
Please remember: "Filtrate" is not a verb.
Write up your lab reports the way your instructor wants them, not the way your ex-instructor wants them.
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GammaFunction
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Qorpak bottles with the Teflon cap lining (the blue-green ones) seem to be good, and they're not expensive. Don't think you can smell ether through
them.
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