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Monoamine
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Update
For the sake of safety I feel I have to give a quick update on later developments.
So, as I said, I put the empty battery shells under mineral oil so the lithium wouldn't react. I then tightly sealed the beaker with aluminum foil,
which was probably my first mistake.
The next day when I went to where I stored it the air REEKED of HCl which was so acrid I couldn't even take the beaker outside without eye and lung
protection. When I checked on it a few hours later the foil that had covered the beaker was completely gone. Guess I got lucky that the hydrogen gas
this must have generated was all outdoors... The battery shells themselves were also super corroded...
On the one hand this is clearly a lesson to be more careful next time, but on the plus side it also means that there was obviously still a pretty
large amount of SOCl2 left in the batteries, so if you make sure to drain them completely you should be able to get a much better yield
than me.
There was a question about cost. I don't remember exactly, but I think it was around 20sh a pop, which means I can't do this very often, but on the
other hand, since Alibaba has them for around 4$ (and less for bulk orders), it will have to come from there in the future.
Also, an acid resistant metal saw would come in handy to be able to open them completely, but I don't know if there even is such think, haha.
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Monoamine
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Quote: Originally posted by teodor  | "Also, as for safety equipment, as long as you're working in a well ventilated space and use plenty of gloves and ideally some kind of gas mask, you
should be fine. I actually just rinsed the glassware in the sink and the resulting fumes were no problem."
You are not quite right, Monoamine, repeating again that the danger is associated with SOCl2 decomposition products, those HCl and SO2 fumes. The
toxicity is connected with SOCl2 itself.
1. It is very volatile. Vapour pressure is 1/2 of acetone. There is not enough water vapour in the air to neutralise it.
2. The fumes are denser than air. Ventilation which can work well with most of other compound (let say, NO2, HCl or SO2) doesn't work well.
3. Usual gas mask with protection from "acid fumes" doesn't protect at the same level.
4. I red studies of SOBr2 toxic action but I think for SOCl2 it should be similar. When somebody breath its fumes he gets SOBr2 dissolved in fat.
So, I am glad you managed the process but I think you don't properly marked the dangers, making accents on decomposition products HCl and SO2. SOCl2
is much more toxic than any of them.
Also I can see you were working in a professional fume hood with baffles. Baffles are effective against dense fumes SOCl2. But I believe this element
could be absent in many DIY fume hoods.
[Edited on 9-8-2021 by teodor] |
TBH, I'm not sure how well this fume hood protects against acidic fumes, since it's ductless and uses filters. I think the ones in this one are more
designed for hydrocarbons (but maybe filters designed to handle acids exist??) I'm also kind of tempted to try to build a DIY vent to minimize the
risk of anything toxic floating around indoors. Project for a rainy day...
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karlos³
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If its something corroding, that gives off HCl fumes or so, I put a layer of plastic foil in between, and then Al foil over this, to avoid direct
exposure and it turn, Al crumbles falling into whatever is in the beaker.
Works fine.
| Quote: | | There was a question about cost. I don't remember exactly, but I think it was around 20sh a pop, which means I can't do this very often, but on the
other hand, since Alibaba has them for around 4$ (and less for bulk orders), it will have to come from there in the future. |
You mean "a pop", like in, per battery opened?
So it was over 120$ just for the batteries? 
Wow.
Quite the expense for only 30ml of SOCl2!
I think I paid 18€ for 100ml or so ten years ago.
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teodor
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| Quote: Originally posted by Monoamine |
TBH, I'm not sure how well this fume hood protects against acidic fumes, since it's ductless and uses filters. I think the ones in this one are more
designed for hydrocarbons (but maybe filters designed to handle acids exist??) I'm also kind of tempted to try to build a DIY vent to minimize the
risk of anything toxic floating around indoors. Project for a rainy day... |
I didn't know that ductless fume hood are effective for this case but if you haven't troubles (like burning throat or hoarse voice after the
experiment) your protection was probably OK.
Also probably you can modify any ductless fume hood and add an air exhaust line.
What I can confirm is that the exhaust line which collects the air only from a top of a hood is not enough to work with this compound, you have to
draw air from the bottom, so if you plan to do work with SOCl2 design your hood draw line the same way as it is in your ductless hood.
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Monoamine
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| Quote: Originally posted by karlos³ | If its something corroding, that gives off HCl fumes or so, I put a layer of plastic foil in between, and then Al foil over this, to avoid direct
exposure and it turn, Al crumbles falling into whatever is in the beaker.
Works fine.
| Quote: | | There was a question about cost. I don't remember exactly, but I think it was around 20sh a pop, which means I can't do this very often, but on the
other hand, since Alibaba has them for around 4$ (and less for bulk orders), it will have to come from there in the future. |
You mean "a pop", like in, per battery opened?
So it was over 120$ just for the batteries?
Wow.
Quite the expense for only 30ml of SOCl2!
I think I paid 18€ for 100ml or so ten years ago. |
Yea definitely an experiment I won't be able to repeat at that cost. If I do it again I'll definitely order from Alibaba. Still not as good as
store-bought, but sadly I haven't found one that sells it to private individuals...
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