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Author: Subject: what do you use to store iodine/bromine
wxyz
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[*] posted on 6-2-2011 at 10:29
what do you use to store iodine/bromine


I once had bottle of 25g iodine from some chemical manufacturer. After about 10 or 15 years the iodine totally destroyed the cap (it was plastic, maybe bakelite). Since then I have tried storing the iodine in various jars, test tubes with rubber stoppers, or finally glass bottle with ground glass stopper, possibly enclosed in multiple ziplock bags. It has either destroyed the cap or leaked out of all of the above. Now I have it in a glass bottle with a ground glass stopper AND vacuum grease on the stopper AND I store it in the mini fridge in my "lab". The vacuum grease has turned brown but at least I don't smell iodine around the jar anymore. So that is a somewhat happy solution.

I am planning on making some bromine soon and I imagine I will have the same problems storing it long term as well.

Does anybody have suggestions for long term storage of these halogens?
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[*] posted on 6-2-2011 at 10:34


Bromine is awful. I have a tiny amount, which I keep in a test tube with a ground glass stopper wrapped with teflon tape. I've then got that inside a closed plastic fizzy drinks bottle which is inside my fume cupboard (the fan itself is only on when I'm in the lab, but it means that the gases can vent to the air outside).

I also got noticeable amounts of rust on all the metal things in the area (bad, because the lab is in a garage which also houses my lathe and woodturning tools), so I spent some time removing all the rust with steel wool and spraying everything with WD40.
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[*] posted on 6-2-2011 at 10:41


I store my ~25 ml of bromine in one of these, the one on the left with a red cap. The red caps are far more durable than the standard blue ones, which are made of PP. The red ones are melamine with a ETFE pouring ring and PTFE liner IIRC.

It still smells, though. Storing the bottle in a tightly closed plastic box filled with sodium thiosulfate might solve that problem as well as make storage more secure. Alternatively, you could store it in a refrigerator or fridge, but only if you have one dedicated to lab use.

[Edited on 6-2-2011 by Lambda-Eyde]
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[*] posted on 6-2-2011 at 11:05


Thanks for the pointer to the bottles. And I like that tightly closed box with sodium thiosulfate idea. Think I will give that a try.

Actually,.... this reminds that I have vacuum desiccator that I can't use for vacuum work anymore because of some chipping on the glass. I could but the Br and the I in there over the NaS203.
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[*] posted on 6-2-2011 at 11:20


Iodine has always been a pain in the ass to me and I would assume Bromine to be just as bad. With the iodine I find storing it underwater to help alot so that the cap does not corrode.




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[*] posted on 6-2-2011 at 11:32


I store Iodine in a amber glass jar with a plastic/teflon lined cap. The inside of the cap is purple now but I've never had a leak. I would imagine ground glass would work very well as well though.

Bromine is crazy. I am able to store it, but after much trial and error. I keep mine in a glass ampule like this <a href="http://www.sks-science.com/images/176772LRG.jpg" target="tab">these</a>. Just pour it in and melt the top closed with a torch, and break at the score line when you need to open it. Ive also heard of it being safely stored under a layer of conc. sulfuric acid in a jar (to keep it from fuming I guess as well as dehydrate it if theres any water in it).




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[*] posted on 6-2-2011 at 11:45


Quote: Originally posted by hkparker  
I store Iodine in a amber glass jar with a plastic/teflon lined cap. The inside of the cap is purple now but I've never had a leak. I would imagine ground glass would work very well as well though.



I thought the ground glass would be the final solution too, but at least with ground glass I had, which admittedly was not top quality, it managed to leak out. I think with higher quality ground glass (better tolerances ground finer) it would leak out much less. But like I said, adding vacuum grease does stop it cold.
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[*] posted on 6-2-2011 at 12:07


I have seen commercial bromine sold in the container Lambda-Eyde referenced. The bromine was stored in a cabinet on its own, and the area around it was not noticeably corroded. I think this would be the best way to go.

[Edited on 2-6-2011 by smuv]
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[*] posted on 6-2-2011 at 17:05


I've had no problem with Iodine using teflon lined silicone septa on vials. It's also pretty easy to seal into ampoules--but do it outside, as any iodine stuck in the neck will vaporize when you take a torch to it.

I don't yet have any bromine, but I would store it in multiple small ampoules, to break open as needed. Just make sure they're borosilicate.
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[*] posted on 6-2-2011 at 20:10


I have stored iodine in standard glass medicine bottles and plastic containers without any problems.

Smells yummy!



This is a strip of lithium, which should be stored under inert gas or oil. But I figured I'd just stick it in the bottle as I'm not particularly bothered about having a shiny single gram quantity of lithium. The metal is still active, but is now crispier than a crisp due to it reacting with the oxygen left in the bottle - the thread is taped shut.


This is an example of where things start getting difficult. It's a supplier bottle of anhydrous AlCl3. Without opening it, I could already see it was rotting it's own label. Moisture was getting around the seal, coming into contact with the AlCl3 and this was then releasing hydrogen chloride gas. Gradually. If it's anhydrous, tape it. Better yet, reform in situ just prior to use, as it's very unlikely it'll still be in the state it was bottled under. Even Sigma's Sure Seal septums leak and solvents bottled in them will be redistilled for critical work.


The above bottle would have benefited from a wrap with this, yet I suppose they look down on such solutions, whilst their bottles leak. In the example above, it is particularly bad as the contents decompose on contact with water, and contaminate the supposedly dry lewis acid with bronsted lowry acid, which will then catalyse the lewis acid into doing things it wouldn't normally.


[Edited on 7-2-2011 by peach]




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[*] posted on 6-2-2011 at 20:58


Mmm beautiful iodine :cool:

I keep my home made sample of iodine in a test tube with a standard plastic cap (PE or PP). I glued a penny to the top followed by metal duct tape. The plastic threads haven't been discolored at all after a few years. Of course the top of the cap is black.

I stopped my sodium from bubbling by covering the entire cap with metal duct tape followed by wrapping the outside. Sneak past that, bloody water! Has anyone else used this tape? Never had much luck with teflon tape on the threads.




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[*] posted on 6-2-2011 at 21:05


You need to put a good few wraps on. It's designed for sealing close fitting parallel pipe threads, whereas the bottles have much coarser and lower tolerance threads.

{edit}Oh, the Iodine is in a bottle marked 5, which would be Polypropylene. It's brown because the plastic is amber tainted.

[Edited on 7-2-2011 by peach]




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[*] posted on 6-2-2011 at 21:13


I've never had luck wrapping pipes either. It always leaks! I used the thicker gas line tape as per your recommendation in another thread on the pipes and it was fine.



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[*] posted on 6-2-2011 at 22:41


@Peach: AlCl3 and many others such chems do have an expiry date and this is for an obvious reason. Ethyl ether for instance is meant to be used whithin 6 months from manufacturing date otherwise it'll peroxidize. They don't take any risk when it comes to selling stuff. Shortening a validity date for a certain chem by half could mean doubling the sales. I guess the modern chemists lost his skill when it comes to purifying organic solvents, redistiling them and such. There are many old books describing these methods in detail.

For the underground chemist an old half oxidized sodium bottle, or some wet, acid RP in a rusty can are simply treasures.

I read in shock on one of my PE Merk bottles with 30% H2O2 that "after 5 years from manufacturing date the bottle may become brittle". Been 15 years now and it's still fine.

All the chemical bottles are made to hold for a certain time, then they "expire" and should be recycled. Ecologicaly. And for a glass bottle it all begins and ends with the cap. The better the cap is, the longer the warranty. As a matter of fact most of our chems are "expired" and "given away". Some were tossed away waiting to be scavenged by us. Ebay is just such a place. Just think about it where you got "yor chemz" from and how. They should have been properly disposed of long ago.

The absolute best solution is vialing. Some chems simply cannot be stored otherwise (think Cs).

As about iodine storing besides vialing, the best bet is PTFE lined cap with amber bottle. Bromine is far worse, as it's way more volatile and more corrosive.

[Edited on 7-2-2011 by a_bab]
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[*] posted on 7-2-2011 at 00:20


I realise a number of chemicals are contaminated or ruined overtime, those that are particularly sensitive to the atmosphere or reactive with regards to the container.

Using AlCl3 as an example, since most people here don't have a Sigma account and so can't get the Sure Seals, and don't have the gas handling equipment and cannula to carry out an anhydrous transfer, it may be better for such things to either be dried or generated IN the flask it's about to be used in - so it can be used without ever having to open said flask to the atmosphere. Even if you have Sure Seal bottles, they leak - Sigma actually have a page on the site about the leakage rate.

Lifespan depends entirely on what is in it and what you want from it. As you've point out, your container is over 15 years old and fine. There are a number of less reactive things that are going to keep indefinitely in terms of at home use, even when stored in fairly basic conditions. I'm thinking of the kinds of things you'd find in a GCSE or A-level chemistry lab, where there is no specialised handling equipment or critical purity involved.

I can see the use of PTFE liners, but I don't see why iodine is so needing of one. If you've got them, use them. If not, I don't think you need to buy a pack just for iodine. Sulphuric is more of a storage problem.

Iodine can be sublimated and sulphuric can be redistilled without too much trouble at home. Again, pretty much no one here has the ability to work under truly anhydrous conditions, so trying to store anhydrous solvents is something of a waste of time.

Solvent stills are still very much in use. In fact, things have moved on to solvent purifications systems using alumina. Even today, people will buy dry solvents and then redistill them as they need them, realising it will have picked up moisture. They opt for the predried things to ease the redistillation or drying.

You're correct that ampoules are the only true way to ensure something remains as bottled. I'm probably one of the few people here that sits around with his beer watching videos of students in Russia pulling them by hand. But if the thing in them is in anyway sensitive to the atmosphere, you need some decent gear to get the material out and into the experiment without it being contaminated as soon as the ampoule is opened.

The solvent still room at Cambridge University, showing that stills are not only in use, but now have their own room - the photo is from Dan's blog, Curly Arrow
<img src="http://photos1.blogger.com/x/blogger2/4300/535534669109052/1600/433308/for%20dan%20-%2007.jpg" width="800" />

A sodium free solvent purification system dries and deoxygenates solvents on demand under an inert blanket, each tap is for a different solvent


<!-- bfesser_edit_tag -->[<a href="u2u.php?action=send&username=bfesser">bfesser</a>: reduced image size]

[Edited on 21.2.14 by bfesser]




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[*] posted on 7-2-2011 at 06:58


For iodine and bromine, would a glass bottle with a teflon lined cap be better if it was sealed with a few layers of wax?

I've noticed that some hygroscopic chems often have a wax seal over the bottle cap. Would parrafin be good to prevent the iodine and bromine from leaking out? Or will it eat through the wax too?

The idea of empty ampules for bromine is probably the best bet to keep it from leaking. But since iodine is less aggressive, I was thinking of using a wax seal to keep it in a bottle.

Robert


[Edited on 7-2-2011 by Arthur Dent]




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[*] posted on 7-2-2011 at 07:34


You're not going to have problems with iodine if the cap liner makes a half decent seal or you tape the threads.

Putting wax on it, I suspect you're more likely to end up with problems due to bits of wax ending up in the iodine as you seal and open the bottles.




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[*] posted on 7-2-2011 at 09:46


Quote: Originally posted by peach  
I'm probably one of the few people here that sits around with his beer watching videos of students in Russia pulling them by hand.


Glad I'm not the only one...
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[*] posted on 10-2-2011 at 14:40


store it like i do, at minus 80C, the bromine crystals tend to be quite sedate, i have almost a full 1L bottle stored this way that previously required a new teflon insert and cap every other week at RT. For some reason the world is flush with cheap ultra-lows atm, you just need to have your feelers out. Try simply cold calling pathology labs, they routinely replace perfectly fine working ones because of protocol.
once you're used to the having one around they can tend to drive your interest into the cryo-zone though and contrary to popular myth they don't suck much power really.




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[*] posted on 10-2-2011 at 20:54


I keep my iodine in a FEP bottle at -20C and it has done absolutely nothing of interest over years. No leaking, no secondary bottle needed, nothing.



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[*] posted on 24-2-2011 at 15:13


My iodine is stored slightly moist in a regular plastic container. The plastic is fine, but stained intense purple.
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[*] posted on 24-4-2011 at 15:44
Storing 100g of iodine crystals at room temp?


Hi guys, i have a nice element collection going, but the 100g of Iodine i put in a screw top jam jar last year has pretty much eroded the metal top and is slowly escaping into the surrounding element "cubicles" (i have removed the others for now). I'm about to buy another 100g (i live in the UK, perfectly legal) and was wondering if you guys had a link to a glass jar i could buy to safely keep it as contained as I can be. It has to be room temp ideally as i have em on display.

Maybe a sealed ampoule would be a better idea? I'm toying with buying some long borosilicate tubes and attempting to make my own. Is that a viable solution? Will the Iodine survive while im heating the top end of the tube to soften and seal it? Is there any chance of the ampoule shattering if the pressure inside gets too high from sublimated iodine?

I did a search btw, but the links to jars on the article i found in this forum are dead.

Thanks for reading
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[*] posted on 24-4-2011 at 16:25


Please use the forum search engine before asking. Here's a thread on this question:
https://www.sciencemadness.org/whisper/viewthread.php?tid=15...

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[*] posted on 24-4-2011 at 16:34


Quote: Originally posted by bob800  
Please use the forum search engine before asking. Here's a thread on this question:
https://www.sciencemadness.org/whisper/viewthread.php?tid=15...



Just so you know, i DID do a search, but didnt come across that post. But thanks for the link

I would still like any advice on the ampoule question if anyone has any.
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[*] posted on 24-4-2011 at 16:41


Quote: Originally posted by thethule  

I would still like any advice on the ampoule question if anyone has any.

I don't know if this answers your question, but here's another thread on ampoule sealing:

https://www.sciencemadness.org/whisper/viewthread.php?tid=25...
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