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Little_Ghost_again
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ONLY on here could I crack a joke and get more information on Pet. Ether than I could ever read!! Just so we are clear and I look less retarded, I did
know what was meant and the PET crack was just a joke  .
Never thought about the thermostat in a fridge sparking, easy to solve with something like a DS18s20 temp sensor and a few bits. No idea how you would
seal a fridge enough to make the rest of it safe. Bit harsh on Aga seeing as clearly no one where you worked thought of it or you would still have a
fridge with a door on! Not starting but just saying it was a bit harsh on him.
Dont ask me, I only know enough to be dangerous
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Amos
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The formation of peroxides can be avoided by storing your ether over prills of sodium hydroxide, which in my experience is very convenient as they
tend to stick to the bottom surface and sequester any water as well.
As for ferrous sulfate, it can easily be prepared quickly and in large amounts by a single replacement reaction between copper(II) sulfate(root killer
in many places) and an excess of steel wool. Filter the solution, boil it down in a long-necked container to keep air out, and crystallize. Done.
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Little_Ghost_again
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Quote: Originally posted by Amos  | The formation of peroxides can be avoided by storing your ether over prills of sodium hydroxide, which in my experience is very convenient as they
tend to stick to the bottom surface and sequester any water as well.
As for ferrous sulfate, it can easily be prepared quickly and in large amounts by a single replacement reaction between copper(II) sulfate(root killer
in many places) and an excess of steel wool. Filter the solution, boil it down in a long-necked container to keep air out, and crystallize. Done.
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Just to clarify and sorry for the question.............. You mean putting the prills into the ether solution?
or did you mean in the container where the ether is being stored?
Sound great either way and tip noted
Dont ask me, I only know enough to be dangerous
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gdflp
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| Quote: Originally posted by Little_Ghost_again |
Just to clarify and sorry for the question.............. You mean putting the prills into the ether solution?
or did you mean in the container where the ether is being stored?
Sound great either way and tip noted |
Yes, directly in contact with the ether. The peroxides are not volatile so the hydroxide would have no effect on them if not in direct contact.
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Droso
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I'm less worried now about pressure built up in the bottle since temps, have been mild these days. I also have an old water cooler that I can use to
submerge the bottle in chilled water during hot days.
The peroxide formation is what worries me the most at the moment. I got a response from the manufacturer via email and they said their ether is always
stabilized with BHT, but I just don't seem to trust them. Would it be wise to add a few mg of BHT to my ether just to be safe?
| Quote: Originally posted by Amos | The formation of peroxides can be avoided by storing your ether over prills of sodium hydroxide, which in my experience is very convenient as they
tend to stick to the bottom surface and sequester any water as well.
As for ferrous sulfate, it can easily be prepared quickly and in large amounts by a single replacement reaction between copper(II) sulfate(root killer
in many places) and an excess of steel wool. Filter the solution, boil it down in a long-necked container to keep air out, and crystallize. Done.
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Yes, I have been reading about sodium hydroxide in ether to stop peroxides, but will it work permanently?
That seems like a good way to make ferrous sulfate, but how would I avoid the contamination by small quantities of ferric sulfate during the reaction?
No contact with atmospheric oxygen seems impossible. Would that make the ferrous sulfate useless to neutralize ether peroxide?
If there is really no way to stop the formation of explosive peroxide in the long run even if the ether is stabilized or by adding sodium hydroxide
then most likely i'll get rid off, because right now it feels like I have a time bomb waiting to explode.
[Edited on 20-8-2015 by Droso]
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gdflp
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There isn't any real downside except for a slightly larger BHT contamination in your final product if you perform any extractions. This isn't a big
deal and is definitely worth it if you want peace of mind.
| Quote: Originally posted by Droso | That seems like a good way to make ferrous sulfate, but how would I avoid the contamination by small quantities of ferric sulfate during the reaction?
No contact with atmospheric oxygen seems impossible. Would that make the ferrous sulfate useless to neutralize ether peroxide?
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Ferrous sulfate is actually quite resistant to atmospheric oxidation if kept in a slightly acidic solution, e.g. add a few ml of sulfuric acid. The
reaction of ferrous sulfate to destroy peroxides is as follows, ROOR' + 2H<sup>+</sup> + 2Fe<sup>2+</sup> --> ROR' +
H2O + 2Fe<sup>3+</sup>. Thus, a small amount of ferric ion contamination in your ferrous sulfate has no impact as long as
enough ferrous ions are still present to be oxidized. To be sure all peroxides have been removed if you suspect that your ferrous sulfate has been
oxidized to ferric sulfate, test the ether afterwards for peroxides with acidified iodide. If still present, repeat as necessary.
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Amateurpharmacologist
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My exciting discovery, to myself, of + pressure and seperation.
Hey guys so this is something I just recently posted on reddit but, I would like to share it here because I think this a better environment to share
things I've learned. So the following will be my copy-and pasted post.--- This is something I have just discovered, to myself. Whilst isolating,
through fractional distillation, diethyl ether from starter fluid containing both light and heavy napthenic lubricants, I was able to visually
separate the un-wanted lubricants from the aq. solution left in the reaction vessel by putting the heptane and lubricants under pressure. They first
looked a cloud white distillate which now rests at the bottom. I find that really quite interesting. I will soon put my fresh anhydrous diethyl ether
under the same vacuum and pressure experiments. The complete list of ingregients in this start fluid can were: heptane, ether, CO2, and light
napthenic lubricant 64742-53-6, heavy napthenic lubricant 64742-52-5. I believe the precipitate is indeed the lubricant(s) because of the smell and
high boiling point. awesome.
Thanks for reading and any input, advice, criticism, or similar experiences would be read joyfully.
-AmateurPharmacologist
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Dan Vizine
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I've never seen ether stored in a sealed glass container. I'm surprised that anyone would do that. This invites peroxide formation. That's why all
chemical houses that sell ether (that I've ever seen in the US) use metal cans exclusively, either tin-coated steel with soldered seams or extruded
and spun aluminum. The closures are really nothing special, mainly plastic with aluminum faced liners and they contain the vapor pretty well. You
could be sitting 2 feet from 10 gallons of J.T. Baker ether in gallon cans and not even smell it.
Metal cans cost more to make than glass bottles, and the fact that all manufacturers of ether use metal should tell you something. Why actively court
disaster? There's plenty waiting in hiding.
[Edited on 23-9-2015 by Dan Vizine]
"All Your Children Are Poor Unfortunate Victims of Lies You Believe, a Plague Upon Your Ignorance that Keeps the Youth from the Truth They
Deserve"...F. Zappa
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aga
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Low probability of that.
Sometimes i post when sober.
Having the full range of human experience is also of some value, although not necessarily savoury or acceptable.
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zed
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Hot-Air gun, to heat highly volatile flammables? Fuck no.
Explosion proof items only.
When working with Ether, I used to sometimes use hotplates on waterbaths. Those hot plates were connected to long extension cords, that were plugged
in, in a distant part of the house. The controls were preset, then to turn the hot plate on or off, I'd walk to that remote switch or plugin to
activate. Likewise, if you have a light switch in the room, it must either be of an explosion-proof type, or you must tape it over to prevent
accidental use. Lightbulbs should be the heavy duty plastic coated type, that do not fail catastrophically.
Good ventilation is helpful. Provided that any fans used, are explosion proof!
Ideally, use of a fume hood(explosion proof), or working in a open/outside area, is desirable.
No pilot lights. No spark sources. Etc., etc.
Me and the boys down at the general store, used to figure that any accident involving unplanned combustion of Ether, Gasoline type hydrocarbons, or
Natural Gas..... would probably result in death. Or worse, becoming a crispy critter.
[Edited on 23-9-2015 by zed]
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byko3y
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What reaction happens between diethyl ether peroxide and stabilizers? One thing I know for sure - iron or copper salt produce hydroxyl radicals
leading to acetaldehyde production, while acetaldehyde is an OXIDATION CATALYST, thus when you've mixed the diethyl ether and ferrous or copper salt,
you need to distill it, otherwise your ether will slowly be converted into acetaldehyde.
But I have no idea what happens with NaOH or some other stabilizer.
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karlos³
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Put some copper wire in it. Prevents peroxide formation even more... and don´t be so scared of Et2O, its not that dangerous, purchased one not the
least bit!
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clearly_not_atara
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Unfortunately, on the Internet, the only way to determine if someone's advice is valid is to wait a few years and see if they disappear all of a
sudden.
Can dioxane or dioxolane be used for Grignards? They have much higher flash points... easier to store for those without proper chemical refrigerators.
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byko3y
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Dioxane can't be used for grignard, because it forms a strong adduct or some other kind of shit with grignard.
Dioxolane can't solvate the grignard complex.
Something like dibutyl diglycol could be used. It can be made by reacting bromobutane with diglycol and alkali. It seems to be less toxic than glymes (dimethyl
ethers), but I think they might be less effective than THF or diethyl ether. EP0632043B1
As you can see, grignard reagent preparation requires heating, but the positive side is that you can actually perform some grignard coupling, that
requires strong heating, without changing the solvent, because glymes boil reeeealy high.
[Edited on 26-9-2015 by byko3y]
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Justin Blaise
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When you add dioxane to solutions of MeMgBr or EtMgBr, you precipitate MgBr2 and form the dialkyl magnesium compounds. These are very pyrophoric as a
recent experiment has taught me.
[Edited on 26-9-2015 by Justin Blaise]
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xfusion44
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@op
I stored it in amber bottle, with a piece of electrical tape (it would be better to use PTFE tape) and I had no problems with it, even in summer time
(temperature in room didn't get over 30°C). The pressure does build up, but it's far too low to cause bottle to explode, so don't worry. Unless
you'll leave it closed outside on sun or you live in the desert, there's no problem.
Please don't throw away your ether, that would be such a loss. It's very hard to get ether in my country, unless you distill it from starter fluid.
Once I ordered it on ebay (200ml for about 25eur with shipping - may look very expensive for you, but that's all I could get) and now the mentioned
offer on ebay is gone... I'd be very happy to have 1000ml of ether if I'd be you 
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Amos
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| Quote: | | Diethyl ether is so precious, so I use it for huffing only. |
u wot m8?
[Edited on 10-1-2015 by Amos]
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byko3y
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xfusion44, simple distillation device, sulfuric acid and ethanol are sufficient to make you own diethyl ether. That's how chemists in the old times
used to obtain it, while chloroform was much more costly to prepare.
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aga
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| Quote: Originally posted by byko3y | | xfusion44, simple distillation device, sulfuric acid and ethanol are sufficient to make you own diethyl ether. That's how chemists in the old times
used to obtain it, while chloroform was much more costly to prepare. |
Please explain/provide a reference for that.
So much better if people can follow up on these things.
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Detonationology
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I think this is what byko is talking about.
Preparation of Diethyl Ether
“There are no differences but differences of degree between different degrees of difference and no difference.” ― William James
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aga
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Excellent Detonationology.
Thanks.
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xfusion44
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| Quote: Originally posted by byko3y | | xfusion44, simple distillation device, sulfuric acid and ethanol are sufficient to make you own diethyl ether. That's how chemists in the old times
used to obtain it, while chloroform was much more costly to prepare. |
Yeah, I wanted to make it that way, but I'm still missing one of reagents... Sulfuric acid. Unfortunately there isn't any H2SO4 in drain cleaning
products in our country. The only way I could get it is probably lead acid battery electrolyte...
Thanks anyway 
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byko3y
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85-90% H2SO4 is enough to make ether.
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