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International Hazard
Posts: 1939
Registered: 23-11-2008
Member Is Offline
Mood: Manic Expressive
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Well I told you I would figure something out to distill this stuff and indeed I did. I was kind of surprised by what resulted. There are at lest three
fractions with distinct BPs. One was the initial BP I already mentioned, there was a 72 degree C fraction that came over as a milky oil that showed
the flammability traits I was seeing, there was a second fraction that was also flammable but this could just be due to carryover from the first
fraction which boiled at 97 degree C and what remains in the test tube right now boils at 120 degrees Celsius. What is striking me as odd is the smell
of mainly the first fraction. It smelled exactly like DMSO. The last fraction smelled similar but more like acetic acid and the DMSO smell is more
then likely just due to the crude distillation attempt and small scale causing carryover of the various fractions.
What the hell could be the DMSO smelling stuff. I honestly feel somehow the Dichloromethane underwent some sort of minor chemical reaction yielding
these contaminates. I do not know what the hell they are so I am a bit leary about reporting anymore smells and what not about them.
I highly doubt its acetic anhydride in any amount so quite honestly im more then likely just going to toss the stuff before it becomes a nuisance. I
already feel like its decreasing my yields so Im not at all happy that its there because I have to not only clean it from my GAA but It more then
likely also decreases the solubility of my AcOH in the DCM making it an even greater pain in my ass.
I must not allow curiosity to side track me this time even though I do want to know what the hell this smelly contaminate is.
Knowledge is useless to useless people...
"I see a lot of patterns in our behavior as a nation that parallel a lot of other historical processes. The fall of Rome, the fall of Germany — the
fall of the ruling country, the people who think they can do whatever they want without anybody else's consent. I've seen this story
before."~Maynard James Keenan
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Neil
National Hazard
Posts: 556
Registered: 19-3-2008
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Pictures? While I have no insight into what is going on, I am finding your ordeal intensely interesting.
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International Hazard
Posts: 1939
Registered: 23-11-2008
Member Is Offline
Mood: Manic Expressive
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I was going to take pictures but theres nothing really interesting about it, just some vials of clear liquids(the first fraction was mlilky but you
get the point). The other pictures I already uploaded show the material I am distilling. The brown stuff being caught in the jar in the third picture
is the stuff I'm now distilling. I always assumed it was trace DCM or wet Acetic acid so I would toss it back in for the next pull not realizing it
was something else all together.
I find it interesting as well but I also don't really see any ideas as to what it may be and as such I could find myself wasting alot of time trying
to figure out what it is. I have seen it in the past as well so its not something unusual to this run. When all is said and done I suppose I could
combine all the gunk and see about identification. If I can gather more material I could perform better test in an effort to identify it.
Knowledge is useless to useless people...
"I see a lot of patterns in our behavior as a nation that parallel a lot of other historical processes. The fall of Rome, the fall of Germany — the
fall of the ruling country, the people who think they can do whatever they want without anybody else's consent. I've seen this story
before."~Maynard James Keenan
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Athiril
Harmless
Posts: 24
Registered: 8-5-2011
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With simple distillation to get to higher percentages, you could just use ethyl acetate to lower the water boiling point drastically, then just drive
that off, then use a small amount of drying agent.
In any case, with the copper sulphate drying, how are you going to filter that? Shouldn't dissolve a fair bit of the paper filter into cellulose
acetate?
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Sedit
International Hazard
Posts: 1939
Registered: 23-11-2008
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Mood: Manic Expressive
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Use fritted glass. I find it to filter better anyway since it does not seem to stick to polar solvents like paper does. I normally just stuff fiber
glass into the stem of funnels anymore as i like the way it filters over paper.
Knowledge is useless to useless people...
"I see a lot of patterns in our behavior as a nation that parallel a lot of other historical processes. The fall of Rome, the fall of Germany — the
fall of the ruling country, the people who think they can do whatever they want without anybody else's consent. I've seen this story
before."~Maynard James Keenan
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Fantasma4500
International Hazard
Posts: 1681
Registered: 12-12-2012
Location: Dysrope (aka europe)
Member Is Offline
Mood: dangerously practical
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okay- old thread
but a returning issue
i see DCM mentioned here, thats rather difficult to get to in europe nowadays
so i came across a study mentioning using other solvents
i went ahead and tried it with my hexane-heptane gasoline fraction. it was difficult getting data on density since acetic acid is quite damn similar
i used 32%
unfortunately it gave me basically nothing, i shaked it quite vigorously and used seperatory funnel, then i distilled off the solvent- in this picture
it does describe quite low concentrations, i didnt bother with higher boiling fractions since theyre just an pain in the ass- however if they can
extract it, acetic acid would distill off first? must have extremely low solubility if this didnt work
https://gyazo.com/66e97a7b79f832855b17a733a859988e
i guess the only feasible method is to use H2SO4 to dry out high concentration acetic acid- or conc H2SO4 (or NaHSO4 with sodium acetate, silly me)
if HAc is used from start, the H2SO4 is merely gonna hold the water and it should be doable to evaporate out the water and a bit of SO3 +70% inside of
a flask, with a hose attachment leading into a bucket of CaCO3 rocks or similarily a funnel-gas trap to prevent suckback
i used 150mL of organic solvent for about .. 87mL of 32% HAc, only minor hint of HAc in the solvent, so little bubbles forming with Na2CO3 that im not
even sure that they did form from a chemical reaction.
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