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Hawkguy
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Got the setup ready to go, everything prepared. If you don't hear from me, it's because I'm being hunted down by Mr.Clean, his Lysol henchmen, and
their Febreeze goons.
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Hawkguy
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Okay so I put 5ml Sulfuric Acid in a 25ml Erlenmeyer flask, stoppered, with a bent glass pipet protruding from the stopper( I just heated it to bend
it, nothing funky) the pipet went into a scintillation vial with 10ml acetone and 5ml hydrochloric acid. The scintillation vial was in an ice bath. I
added 0.8g of FeS to the Sulfuric Acid, and heated until it started bubbling. It turned cloudy (the flask was cloudy, the vial stayed clear), and
bubbled for 5m. I took the vial and added it to 20ml ice water. Put that in the freezer. My lab smells shitty, and although this wouldn't have made
Thioacetone monomer, it still smells like a weird butyl pyrolysis product or something. It smells like the black polymer gunk from an iodoacetone
preparation awhile ago, but I think theres just a side reaction and no smelly thiones have been formed yet.
[Edited on 23-1-2016 by Hawkguy]
[Edited on 23-1-2016 by Hawkguy]
[Edited on 23-1-2016 by Hawkguy]
[Edited on 23-1-2016 by Hawkguy]
In the photo, everything had finished and I took a bad photo of the vial and flask
[Edited on 23-1-2016 by Hawkguy]
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Hawkguy
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Okay so its been a few minutes and it really shouldn't smell bad but the garage smells aweful. I think its because suckback during the bubbling heated
tiny amounts of TA trimer and cracked it. Like it doesn't small bad in the conventional sense, it smells bad in a stranger way. It makes you want to
throw up. The smell also goes away after about 2min which is strange too.
It makes you feel pretty sick I'm lying down right now.
I know I sound like a fear mongerer, but it is honestly dreadful.
[Edited on 23-1-2016 by Hawkguy]
[Edited on 23-1-2016 by Hawkguy]
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Hawkguy
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Hmm its gone away, but no precipitate has formed. I'll cool it down more and do a larger scale tomorrow
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careysub
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You are aware that one of the notable characteristics of thioacetone is that it can be smelled only in extremely low concentrations are you
not? It rapidly shuts down the ability to smell it, so that you cannot tell if you gassing the entire neighborhood.
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Hawkguy
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Quote: Originally posted by careysub  |
You are aware that one of the notable characteristics of thioacetone is that it can be smelled only in extremely low concentrations are you
not? It rapidly shuts down the ability to smell it, so that you cannot tell if you gassing the entire neighborhood. |
Im pretty sure only tiny amounts of the monomer were actually produced. I went out for a few hours and when I came back I couldn't smell it much at
all. Although a few other people remarked on the smell, it definitely didnt gas anyone. I also feel like it might not be completely stable in air,
because of how it faded somewhat fast over what must have been a few hours.
Another note; even when I couldn't smell it, like half an hour after making it, I really felt like throwing up. Its kinda involuntary, a weird
property for a smell IMO, as I usually have a strong stomach and can ignore bad odors.
Final note; I'm pointlessly trying to defend myself, and even though I might officially be an asshole neighbor now, at least one SM member did it and
can tell other people not to do the same.
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Tsjerk
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Is there anything know about toxicity of this compound? And about smell/toxicity/volatility of the trimer?
Maybe you didn't make any monomer and was what you smelled the trimer. It could be that the guys describing the trimer didn't mention this smell
because if you work under a hood, the smell is not that bad (compared to other sulfur organics). OR you just made some random other acetone/sulfur
compound, which I could perfectly imaging to be smelly/toxic.
Feeling like have to trow up sounds like something toxic to me.
One more thing: Did you ever smell H2S? As a comparison? What you did sounds like a nice way to produce H2S.
[Edited on 24-1-2016 by Tsjerk]
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Hawkguy
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| Quote: Originally posted by Tsjerk | Is there anything know about toxicity of this compound? And about smell/toxicity/volatility of the trimer?
Maybe you didn't make any monomer and was what you smelled the trimer. It could be that the guys describing the trimer didn't mention this smell
because if you work under a hood, the smell is not that bad (compared to other sulfur organics). OR you just made some random other acetone/sulfur
compound, which I could perfectly imaging to be smelly/toxic.
Feeling like have to trow up sounds like something toxic to me.
One more thing: Did you ever smell H2S? As a comparison? What you did sounds like a nice way to produce H2S.
[Edited on 24-1-2016 by Tsjerk] |
I smelled the FAINTEST traces of H2S while doing the reactions, but I'm pretty sure most dissolved, so it was really a minor thing. The bad smell
wasn't anything like H2S, it was wierder, like a sulfurousy rubbery plastiky smell.
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Tsjerk
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Ok, I'm really interested in reports about real monomeric thioacetone. But do you have a place to experiment with better equipment in a way more
desolated place? Then I would like you to encourage you in keeping your experiments going.
But until then, especially if people in your surroundings already noticed/mentioned the smell, please consider the possibility you didn't make
anything but carbon-sulfur crap or that you only got to the trimer state.
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careysub
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Experiments with this stuff should ideally be done in an "air-sensitive" compound set-up. But then there is the problem with eventual decontamination
of the set-up.
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Praxichys
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@Hawkguy - It's not very stinky because your experiment is only halfway there.
Bubbling H2S into acetone gives the trimer, trithioacetone. You need to isolate that (presumably via distillation) and heat it to thermally crack it
to the linear polymeric state. This is what the researchers were doing when they contaminated a city - they were trying to isolate the monomer. Trithioacetone itself is moderately stinky but easily available commercially and is used as a food and fragrance additive to enhance earthy notes.
You will have to fractionally distill the trithioacetone from your mixture, or perhaps try a water extraction to get rid of the acetone. You will then
need to pass trithioacetone over a hot wire or something similar to depolymerize it. Maybe try heating a nail red-hot and touching a drop of
trithioacetone with it.
EDIT: If I could read, I would realize that you already know this. Whoops.
[Edited on 25-1-2016 by Praxichys]
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Neuro-
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I was having horrible ideas of making that. Since acetone is readily available all you would need to do is convert that oxygen into a sulfur. I found
this little piece under thioketones on wikipedia to be quite useful "Thiones are usually prepared from ketones using reagents that exchange S and O
atoms. A common reagent is phosphorus pentasulfide[2] and the related reagent Lawesson's reagent. Other methods uses a mixture of hydrogen chloride
combined with hydrogen sulfide. Bis(trimethylsilyl)sulfide has also been employed." Best of luck, RIP to your nose
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Blunotte
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Excuse me, but at this point it would also work if I put a small piece of Na2S in a solution of acetone and hydrochloric acid, it's right? 
I could make the experiment using small amounts in a open country, far away from the houses, these days
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