Sciencemadness Discussion Board - ether recycling and storage

ether recycling and storage

AdamAlden - 26-3-2025 at 20:06

just wondering if anyone has a good process for recycling and storing / purifying this solvent without it blowing up. after reading a lot about it i decided i cannot work with it till i fully understand it. to understand it i need someone to tell me what to do to purify it and what not. cause i read it degrades into explosive compounds over time how could i neutralize these compounds and then distill it before use (after drying)

im honestly not trolling im actually afraid of ether i made it a few times with i swear i think its sodium nitrate and sulfuric acid but the yeild is pretty small but to be honest if its purest quality is from a proce oh wait thats nitric acid i did that too i need pure ethanol and some other shit to make ether i forget though. i followed a video on nurdrages youtube channel back in the day to make the ether. it was funny i think they are my cousins or some shit but they were only little i was in the garage making ether and they came in i immediately told them to get out they asked what are you doing i said... im making a bomb lolololol they ran off

teodor - 27-3-2025 at 03:25

I'm not an expert here, but what I basically do:

1. Test for peroxides with sodium ferrothiocyanate reagent. I did some posts about it here: https://www.sciencemadness.org/talk/viewthread.php?tid=15793...

2. Remove peroxides if present with ferrous sulfate. Vogel has a procedure.

3. Distill if necessary. Use only a long spiral condenser (Graham) and cold ethanl (let say, -20C). There is still no guarantee there is no lost on this stage. Be careful, can catch fire. (The autoignition temperature is just 160C)

4. Dry over CaCl2.

5. If you need super dry put a sodium wire. I modified a tobacco press bought on amazon for the purpose of making it. Also was following Vogel.

Update: as a field of experiments, if you have very dirty ether, you can try
making and breaking various etherates. But practically, if you can manage distillation without considerable loss making of you own ether could be more economical.

[Edited on 27-3-2025 by teodor]

[Edited on 27-3-2025 by teodor]

MrDoctor - 27-3-2025 at 03:36

so, with radical scavengers such as BHT, or perhaps hydroquinone? you can pretty much keep the ether peroxide at bay. what is tricky is storing it, but there are some tricks i have found.

On aliexpress there are these things called "leak proof essential oil bottles", its an aluminum cannister with a very firm push-insert plug of sorts, followed by a PP screw cap, its the same bottle youll find high-end or just especially noxious epoxy/fiberglass resins come in. this combination provides a pressure-tight seal preventing ether from escaping.
if you buy 10 at a time or more they can get rather cheap, i think i paid no more than $3 or 4ea for the 250ml ones.

Otherwise, a close second is cheap "fuel bottles" which i dont really understand, their application is camping, and they connect to gas stoves, but, they are meant to contain gasoline? certainly not butane/LPG, i dont know. but they have a screw cap with a rudimentary gasket and while they leak enough vapor to smell, they barely lose a gram of mass per month if you use teflon tape to improve the seal. ether and DCM however soften the cap so you want to be rather conservative with how often you use it. i dont use them anymore except for long term storage of my DCM.

Ether is very difficult to keep contained, and if even a trace is escaping you pretty much cannot refrigerate it at all then, through various mechanisms, it causes refrigerators to blow up.

what i have heard is the ether condenses on icy coils, where it oxidizes and can form ether peroxide, eventually resulting in combustion, though its the fumes that fill the fridge that actually do the damage, the ether peroxide on the dry evaporator coil ice just potentially provides some form of ignition eventually, assuming this fridge doesnt have the thermostat inside the cooling compartment. especially small bar fridges, will have the thermostat inside, resulting in there being a periodic arc as the contacts connect.
My workaround has been to simply keep my bottles which barely leak as it is, inside a 12v peltier cooler with no fans or anything, the lid is super leaky and moisture is constantly flushing any residues out as it dissolves into condensation, which can drain away. its inefficient but i dont lose any tangible amount of ether even during 40C days, and i can keep it outside of the house too. though the place i keep it could be defined as a barn i suppose, or car shed, which is why the sweet-water that dribbles on the ground doesnt make a smell. indoors in an enclosed space it could be a problem. During winter the fridge doesnt need to run at all so i leave it open and off, but spring and summer, i think my bottles would explode. without cooling i had the issue of ether just freely boiling if i opened the bottle.

Note: ether diffuses rapidly through teflon and silicone, the more of either you use, like, the thicker it is, the worse diffusive leakeage becomes.

Osmiridium - 27-3-2025 at 08:32

First of all you really tried to produce ether from NITRATE, sulfuric acid and ethanol? I hope you didn't distill that shit off the mixture?

What you will produce is not diethyl ether but ethyl nitrate and that is unstable and explosive as hell. This would be a really stupid idea.

A few other remarks:

It's never good to be afraid of things in chemistry. This can lead to accidents too. But of course it's crucial to inform yourself about any dangers and properties of the substances you intend to work with. What you apparently did not. If you are afraid and don't know what you are doing, leave it alone.
And I would really never make jokes about making a bomb. You know, people talk. You can have the best intentions and do nothing wrong, still in our paranoid society if the wrong people hear something you can get in serious trouble. Then it's no joke anymore.

MrDoctor - 27-3-2025 at 18:07

Quote: Originally posted by Osmiridium

First of all you really tried to produce ether from NITRATE, sulfuric acid and ethanol? I hope you didn't distill that shit off the mixture?

What you will produce is not diethyl ether but ethyl nitrate and that is unstable and explosive as hell. This would be a really stupid idea.

From the looks of it they used speech to text and forgot to cut the nitrate part out. Nurdrage afaik never made ethyl nitrate, but has done ether.

Also, just mentioning this but if you have access to iodine tincture, the fact you have a strong purple solution (as iodine not povidone iodine) means you have enough iodine for a colormetric test for peroxides. off hand i forget what the test was i think starch and iodine? or perhaps it was a weak acid and iodide salt, since the peroxide would oxidize the colorless iodide/hydroiodic acid into dark iodine again. in any case the iodine is the only one tricky to get for some in this very easy and versatile set of colormetric tests, but all this requires is a visual color change which even milligrams in tincture gets you easily, and afaik tincture is available almost universally.

Osmiridium - 28-3-2025 at 04:17

Quote: Originally posted by MrDoctor

Quote: Originally posted by Osmiridium

You would use iodide and starch. Iodide is oxidized to iodine and that forms a deep blue complex with starch and indicates presence of an oxidizing agent. This test is so sensitive that it can be used to quantitatively determine oxidizer concentrations through titration.

Ether purfication

eyeemplus - 29-3-2025 at 02:19

See the attached graphic

Screenshot 2025-03-27 at 16.21.22.png - 699kB

MrDoctor - 29-3-2025 at 03:14

oh i need to try that, my ether contains something, and if aldehydes for example dont just distill out normally, or wash out with water, i would assume that means they are quite difficult to remove by any means of seperation.
How reliable would permanganate be for this? like to totally eliminate, if that fails ill try that copper-zinc stuff. Some of my ether comes through the reactor with this strong odor attached that no amount of distillation can cure, nor soaking with acid, base, charcoal or just water. i thought it was some polymer of some kind which is why it could have virtually identical physical properties, based on something i read somewhere

Mateo_swe - 1-4-2025 at 04:17

You can get proxide test strips from stores that sell pool supplys or internet.
Never tried these but it sounds like a good way to check your diethyl ether for peroxides.
I think if you want to have diethyl ether a good idea is to make sure you have good ventilation or even better store it outside.

I have thought about installing a small explosion proof fan (look for engine room fans) with a vent pipe down to the floor in the lab or where you store your ether.
Then program the fan to start once a day or so for a while and lead the exaust outside.
Then even if your ether bottle would leak a little you vent the fumes out before it can build up to explosive levels.
Ether fumes are heavier than air so you need to suck the air out from the floor level.
If a bottle of ether leaks fumes and are left alone they will pool at the lowest point and i think they will build up the concentration over time, not good.

I have a large glass bottle of diethyl ether but i havent opened it yet, in original bottle.
It´s one of those glass storage bottles with a red colored plastic screw cap.
Last time i checked it, nothing seem to have escaped.
Isn´t the chemical storage glass bottles with red crew caps made for things like ether and dcm?

Osmiridium - 2-4-2025 at 04:38

If ether is stored and handled correctly there is not much danger. If you notice any loss of ether from your bottle during storage you clearly don't have a proper bottle. Without ventilation vapours can of course accumulate in potentially dangerous concentrations. It must be a tight sealing bottle meant for chemicals storage and there should not be any noticeable ether escape (please don't use pickle jars or plastic bottles and the like). Also don't store it in a normal household fridge. Besides of being absolutely not necessary, this can be dangerous.

Regarding handling, same security measures apply as with gasoline, propane, acetylene or any highly volatile flammable compund. Ether has a distinct smell and the explosive concentrations are far beyond the smelling threshold.

Furthermore it should be clear that the amounts of ether make a big difference. If you store for example 50 ml in a normal room, even with some leakage, it's unlikely to ever achieve dangerous concentrations. Whole another story is if you work with 10l or whatever.

Regarding peroxides: They are only formed slowly with oxygen and sunlight present (generally, shorter wavelength light). Thus storing it in tight sealing brown glass or metal bottles in a dark cool place mitigates risk. Fully filled bottles are good practice. Clearly there's no point in storing 50ml in a 1l bottle. If in doubt after longer storage, make a peroxide test.

[Edited on 2-4-2025 by Osmiridium]