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Author: Subject: Separating a mixture containing solvents and a dissolved solid that sublimes
GhostAliensFromMars
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[*] posted on 28-4-2025 at 23:01
Separating a mixture containing solvents and a dissolved solid that sublimes


Hi all

I have a small question regarding separation. If one had a mixture of different liquids containing a dissolved solid that sublimes when heated, could distillation be used? I'm not sure if the solid would deposit inside the condenser and contaminate the different fractions. Has anyone attempted anything similar to this?
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imidazole
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[*] posted on 29-4-2025 at 04:56


This sounds like a job for a cold finger, or some other form of trap for the solid, what exactly are you trying to do?

If you don't care about the solid, maybe a cotton block before your condenser would be enough to trap it, depending on what it is and how much.
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bnull
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[*] posted on 29-4-2025 at 11:51


What is in the mixture? There are physical processes and chemical processes that can be applied but, if we have no idea of the composition, albeit approximate, we can't do better than a guessing game. Unfortunately, there is no one-size-fits-all process.



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GhostAliensFromMars
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[*] posted on 29-4-2025 at 22:38


Its made up of about 50% camphor dissolved in around 20%eugenol and 20% cineole. According to the MSDS the extra 10% is "non volatile terpinoids" The goal is to remove the camphor to be left with eugenol and cineole. The terpinoids I do not care for
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[*] posted on 29-4-2025 at 22:56


Eugenol can be removed with liquid-liquid extraction with sodium hydroxide.

You might have better luck separating the camphor and cineole using column chromatography.




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GhostAliensFromMars
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[*] posted on 30-4-2025 at 01:42


Hmm, thx for the ideas. Perhaps il just first stir the mixture with no heat and apply a vacuum to sublime out the camphor, filter and fractionally distill the camphor free oil.
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chempyre235
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[*] posted on 30-4-2025 at 08:01


Quote:

Eucalyptol [cineole] forms crystalline adducts with hydrohalic acids, o-cresol, resorcinol, and phosphoric acid. Formation of these adducts is useful for purification.

https://en.wikipedia.org/wiki/Eucalyptol
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JackleApp
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[*] posted on 30-4-2025 at 17:19


Quote: Originally posted by GhostAliensFromMars  
Hmm, thx for the ideas. Perhaps il just first stir the mixture with no heat and apply a vacuum to sublime out the camphor, filter and fractionally distill the camphor free oil.


check what the BP or vapor pressure does at different reduced pressures. there are some things which cannot be seperated at atm but under even just half vacuum go from 2-3C difference to 20C
a similar principle also exists for reduced pressure steam distillation but all i know is it exists, ive never bothered to try understanding it because water at least prevents any sort of fractionation, it pulls everything with poor selectivity. steam distillation with alcohols or other solvents yields different results. Might be worth looking into.

Another thing to try is, adding a solvent that dissolves one component radically more than the rest, may cause these substances to be less intimately co-dissolved, allowing them to freeze precipitate out, maybe not at around zero as they would when pure, but -20, perhaps. if you remove enough you get a sacrificial fraction worth discarding sometimes.
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