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Author: Subject: How long can I store ethyl bromide in a mason jar at room temperature?
Cou
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[*] posted on 2-6-2020 at 15:03
How long can I store ethyl bromide in a mason jar at room temperature?


Don't have a lab freezer. Will there be a significant loss from evaporation in just one or two days? if necessary I will plan my labs so i use bromoethane in the same day it's made, but kind of a pain.

I am considering some kind of option like a dry ice styrofoam box.



[Edited on 2-6-2020 by Cou]




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morganbw
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[*] posted on 2-6-2020 at 15:15


Not sure but did you look at the characteristics of this particular compound?
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karlosĀ³
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[*] posted on 2-6-2020 at 15:16


Turn it into the ethyl iodide with the Finkelstein.
And throw that mason jar away and get a proper container.
I have around almost 90ml of ethyl iodide and I store that for like 4-5 years without an issue.
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Cou
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[*] posted on 2-6-2020 at 15:21


I know it's carcinogenic, which concerns me, as someone who hopes to see year 2100. And alkyl halides are useful in organic synthesis so i would get a long-term exposure over my hobby.
the best PPE I can get is doing this outdoors, respirator, gloves, and a big fan. Unless my research professor at UTD would let me do it in their fume hood.
It's the first step of multistep synthesis of pentan-3-yl acetate, hoping to make a youtube video about it.

[Edited on 2-6-2020 by Cou]




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Ubya
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[*] posted on 2-6-2020 at 16:37



Quote:

the best PPE I can get is doing this outdoors, respirator, gloves, and a big fan


but you are not storing it outside, you really shouldn't use mason jars to store volatile carcinogenic compounds, get an empty bottle from your university, a good one.





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Cou
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[*] posted on 2-6-2020 at 16:51


based on what has been said here, i'm just gonna use the bromoethane on the same day i make it.



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mackolol
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[*] posted on 3-6-2020 at 03:37


Buy yourself lab bottle with blue cap. These are great for low boiling point - very volatile liquid storing. You will be able to store such compunds for year without significant loss and it is not expensive. I have DCM as well as alkyl halides in mine and it doesn't leak.
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[*] posted on 3-6-2020 at 04:36


Place PE membrane between cap and glass rim. You can also use al foil on top of PE to reduce permeation. For some stuff a PTFE film works.

[Edited on 3-6-2020 by Refinery]
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Cou
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[*] posted on 3-6-2020 at 20:13


Quote: Originally posted by mackolol  
Buy yourself lab bottle with blue cap. These are great for low boiling point - very volatile liquid storing. You will be able to store such compunds for year without significant loss and it is not expensive. I have DCM as well as alkyl halides in mine and it doesn't leak.


Do you store the carcinogenic alkyl halides indoors in those bottles?

I will not be storing for a long time. Maybe a few days max.

Here in Texas a typical daytime temperature is 33 C, and the boiling point of bromoethane is 38 C. On some summer days it might even reach 38 C. So I will have to store them indoors if I do this. Otherwise I have to plan for making bromoethane the same day as the reaction that uses it, which will be a pain b/c i have to dry solvents and make an ether still and everything.

i am considering these:

https://www.amazon.com/Corning-PYREX-1395-100-Storage-Bottle...


[Edited on 4-6-2020 by Cou]




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mackolol
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[*] posted on 4-6-2020 at 01:44


Quote: Originally posted by Cou  

Do you store the carcinogenic alkyl halides indoors in those bottles?

I will not be storing for a long time. Maybe a few days max.

Here in Texas a typical daytime temperature is 33 C, and the boiling point of bromoethane is 38 C. On some summer days it might even reach 38 C. So I will have to store them indoors if I do this. Otherwise I have to plan for making bromoethane the same day as the reaction that uses it, which will be a pain b/c i have to dry solvents and make an ether still and everything.
[Edited on 4-6-2020 by Cou]

Yes, I store them indoors, why not? , the bottles are perfectly tight and blue caps are made for volatile liquids storage. I don't notice any leaks, however I can't predict how would they behave in 38C...

Quote: Originally posted by Cou  
i am considering these:

https://www.amazon.com/Corning-PYREX-1395-100-Storage-Bottle...
[Edited on 4-6-2020 by Cou]


Yeah, these are the ones that I'm talking about, but in Poland they have "blue" caps which means, what I have said above, red ones are coated with PTFE, but I think that in this case, the colour doesn't matter and it should be fine.

[Edited on 4-6-2020 by mackolol]
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[*] posted on 4-6-2020 at 01:56


Indoors is not a problem, because it's climate controlled with HVAC to always be around 23 C.



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[*] posted on 14-7-2020 at 10:11


You could always make a "earth cellar".
If you dig a deep hole somewhere that are always in the shade, like almost a meter deep and have a styrofoam lid it will be cool even in summer as the soil is a good insulator and a bit down in the soil the temps are cooler.
When i was younger we dug a hole about 80cm deep, this was in spring when it was cold and we put an iceblock down the hole and put a styrofoam lid with some stones on to keep it in place.
At the end of the summer i looked in the hole and there was still some ice left.
So soil have very good isolating properties, thats why some people dig out earth cellars.
Of cause it will vary in how cold it will be inside depending on your climate but its always a good bit cooler than ordinary outside temps.
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[*] posted on 15-7-2020 at 12:18


Quote: Originally posted by mackolol  

Quote: Originally posted by Cou  
i am considering these:

https://www.amazon.com/Corning-PYREX-1395-100-Storage-Bottle...
[Edited on 4-6-2020 by Cou]


Yeah, these are the ones that I'm talking about, but in Poland they have "blue" caps which means, what I have said above, red ones are coated with PTFE, but I think that in this case, the colour doesn't matter and it should be fine.

[Edited on 4-6-2020 by mackolol]

I just want to add that alkyl halides should be stored in brown glass bottles or darkness, as light induces decomposition and will turn your ethyl iodide purple over time. If you want to keep it fresh for a long time it's also smart to add some copper or silver metal to the bottle.
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[*] posted on 20-7-2020 at 18:09


Almost 40 mL of crude bromoethane stored in a 100 mL GL45 bottle. 40% yield, Made it sloppily from sodium bromide, ethanol, and sulfuric acid (next time i should cool the NaBr/EtOH/H2O mixture in a cold dry ice/alcohol bath before adding H2SO4, it seems that adding H2SO4 overheats the mixture and boils off some product)

It makes a very good seal. Should be safe to store indoors for short periods of time. tomorrow i'm going to dry it for grignard reactions. Bromoethane has a strong ethereal smell at low concentrations, but I can't smell anything escaping from the cap. I have no choice but to store it inside the house b/c Texas temperatures get hot enough to boil it.

20200720_210641.jpg - 46kB

[Edited on 7-21-2020 by Cou]

[Edited on 7-21-2020 by Cou]




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[*] posted on 20-7-2020 at 18:48


Hi Cou, I enjoy reading your input.

Re: summer temperatures and volatiles, if you have no practical means of cool storage, then have you considered an "earth locker"?

https://www.builditsolar.com/Projects/Cooling/EarthTemperatu...

Of course, you would need to make considerations for water/rain, but a suitably sealed secondary containment in a ~3ft hole in a shaded spot, would keep temperatures down below ~20C.
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[*] posted on 20-7-2020 at 19:08


Not worth it for short-term storage. I'm going to use all the bromoethane in a few days for a grignard reactoin.



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[*] posted on 11-9-2020 at 06:34


My only problem with undergound storage was having to break sheet of rock. The safety benefit of being able to vent outdoors in case of leaks is too good to pass up. My storage tote is currently flush with the ground and covered with a piece of plywood so I can walk on it. I keep flat rocks and some dirt to sloppily cover it up. I checked it after a couple strong rains and was surprised to find it totally dry inside. If you only need to store one bottle, you could put a short piece of pipe underground with a pvc cap on it. Pvc is cheap.
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