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fractional vacuum distillation of camphor essential oil Options
 
Mindlusion
#1 Posted : 3/29/2017 7:09:51 PM

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my favorite new smell is this yellow/brown camphor, I can't go a day without sticking my face to the bottle and inhaling (like you might do with a bag of freshly roasted beans). A sharp and fresh camphor which melds into sweet sassafrassy cologne... (inhales deeply)

So I distill it's components. Sadly its a bit like cutting open the goose in search of the golden egg. The essence can never be recreated...


--

so we set up an apparatus with a short-path w/ vigreux column, a 3-way adapter, thermometer, and three round bottom flasks. joints are greased with high-vac greased and joints clipped. In the distillation flask is placed 100mL of yellow/brown camphor oil with a teflon stirbar. The flask placed in a heating mantle connected to a variac regulator and this is placed on top of a magnetic stir plate.

[photo]


The condenser hoses attached and vacuum hose leading to vacuum trap and the pump. Vacuum trap is cooled to about -35C using a mixture of saturated CaCl2 and some snow from outside.

[photo]


The pump is turned on and a vacuum of approximately 1mmHg is reached. The absolute vacuum of this pump can reach 0.08mmHg but the gauge isn't that sensitive so for sake we say its ~1mmHg

[photo]
First fraction to come over was at 50-60C @ ~1mmHg (~60mLs)

This smelled strongly of eucalyptus. The drip rate was very fast, and this was the largest fraction in the oil

Second fraction came over at 80-90C @ ~1mmHg (~15mL)

this fraction smelled strongly of camphor, and had a tendency of crystallizing inside the condenser column.

The third fraction came over at 95-110C @ ~1mmHg (~15mL) and smelled candy sweet, strongly of safrole, but with a hint of something else, almost like Buckleys cough syrup.

The reminding red tar in the flask (~10mL) continued to distill over at +140C, but started to smoke. at this point the distillation was stopped. The residue that distilled over smelled slightly sweet but burnt.

[photo]

[photo]

Expect nothing, Receive everything.
"Experiment and extrapolation is the only means the organic chemists (humans) currrently have - in contrast to "God" (and possibly R. B. Woodward). "
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downwardsfromzero
#2 Posted : 3/29/2017 7:45:55 PM

Boundary condition

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There are so many different grades of camphor oil. Which one did you use? The one known as Ho wood always smells wonderful to me.




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Mindlusion
#3 Posted : 3/29/2017 8:08:53 PM

Chairman of the Celestial Divison

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downwardsfromzero wrote:
There are so many different grades of camphor oil. Which one did you use? The one known as Ho wood always smells wonderful to me.


Indeed, this is Ho wood Smile

the medium yellow/brown fraction
Expect nothing, Receive everything.
"Experiment and extrapolation is the only means the organic chemists (humans) currrently have - in contrast to "God" (and possibly R. B. Woodward). "
He alone sees truly who sees the Absolute the same in every creature...seeing the same Absolute everywhere, he does not harm himself or others. - The Bhagavad Gita
"The most beautiful thing we can experience, is the mysterious. The source of all true art and science."
 
 
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