Essential Oils Distillation

Making Mint and later Rose Essential Oil, classes coming soon!

@Kriskat30

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I’d be happy to take a class like that. Would that in turn work for scenting soap and candles? Cheers!

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yes! That is the idea!

It is difficult to get good hot throw with essential oil scented candles. If someone knows how to do it and wants to teach a class I would sign up…I haven’t figured this out on my own candles yet.

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Really cool! This will be a hit. Wonderful demo of distillation. Thanks.

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Did this class ever take place? I was looking into oil extraction. Rather than post a new thread, I’m adding to this one.

I’m specifically looking at tea (camelia sinensis) and coffee oil extraction, more or as much for a sort of quantitative analysis than for consumption but the consumption or use of the oils would be good as well.

Looking at the apparatus, is that typical for oil extraction? Looks like a reflux condenser then a distillation step. Are these done at once? Separately? Under reduced pressure?

YES, these classes happened. This is steam extraction; typical for many essential oils. We can do vacuum distillation now but so far have only done ambient pressure. Our setup is a bit more streamlined now. We now also have a soxhlet extractor, which might be better for tea, especially if you used a solvent other than water. Do you really mean to extract OILS from tea? As opposed to water-soluble components? because that is what the separatory funnel is for, to separate oils from water-solubles.

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True, many of the important and beneficial components of c. sinensis tea are water soluble but there are some tea compounds that prefer the lipid partition.

So, on that apparatus, do you reflux first for a while and then shut that down and proceed with distillation?

NO, the steam is condensed continuously and the oil just floats on top. No
real refluxing.
We have a pressure bypass funnel now that goes directly over the boiling
liquid, so we can re-extract the water portion without taking the apparatus
apart (just open stopcock); that allows us to boil for the hours that steam
extraction requires without starting with a huge water volume. We also have
a soxhlet now, which will automatically re-distill the solvent continuously
via a siphon action without you having to be there to turn the stopcock.
Check attachment (hope animation works)

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Thanks, Gonzalo! That is a cool concept.

I found a nice description from the NurdRage channel. He has some great stuff. The video also describes a cheaper alternative to the Soxhlet, assuming you have the pressure equalized sep funnel.

YES, we have ordered a pressure equalized funnel, should arrive in a couple
days (was ordered dec 3 but took a slow boat from china) it looks like the
best way to do our steam distill and makes a much simpler and sturdier
setup than the one in the picture you sent.

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Gonzalo,

Assuming equal cost and efforts to set up, how would you compare a Soxhlet extraction config with the pressure compensated separatory funnel as noted in the video? I think the NurdRage guy says the sep funnel tech is a bit less efficient.

I looked at Soxhlet sets on Amazon. They price seems about comparable to the pressure compensated funnel and in fact, the Soxhlet might be a bit cheaper from what I see. Another factor in the decision might be as to other uses for the glassware. That is, the Soxhlet seems very specific to one task. The sep funnel might be useful elsewhere. And the Soxhlet looks like it could be tough to clean.

Either way, what an ingenious technique! - Soxhlet reflux and extraction with automatic siphon return of solvent.

They are really quite different things, cost is not the difference. Using a
equalized funnel still requires you to manually turn the cock and return
the water to the boiling flask, it can NOT be left unattended or it will
dry out. The soxhlet keeps the boiling flask full automatically for days,
there is no stopcock. Also, you use the sep funnel when you have clear
separation and can easily return just the aqueous part at the bottom.
Soxhlet will work even if you only have cloudy solution with no separation,
and even when the desired oil is DENSER than water. Oddly, Soxhlet is
favored when your desired material boils much hotter than solvent, like
cinnemaldehyde (BP 248C). Finally, Soxhlet is usally used with volatile
organic solvents, not water; the cycles take too long with water. You get a
much more concentrated extract, and complete extraction of the solid
material; after many repeat cycles nothing is left in the solid. I
recommend getting a fritted glass thimble instead of those teabaggy paper
thimbles. People complain about keeping glass clean and unclogged compared
to disposable but it is really not a big deal. Some folks also just plug
the bottom hole with glass wool and stuff their solid on top, that is
enough to keep it from dribbling down into the boil flask.

Hi, I should have watched the video before answering, I mistook it for
another video. I see he did cover the various appraoches to thimbles, so my
remarks on that topic were superfluous. I personally would not trust the
drip method to go unattended; if you did not match the rates of
condensation and drip perfectly cold be disaster, besides it is not
actually cheaper than a real soxhlet. Soxhlet extractors are quite cheap on
ebay, you can get a 500 ml for $25 including shipping, and a 125 ml for
about $17,

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Thanks, your experience with this is impressive and important. I agree about using glass and just keeping things clean. Unattended (or minimally attended) use with the Soxhlet is a huge plus not to mention the other advantages you cite.

Sad to say our pressure equalized sep funnel finally arrived from china, and it was shattered into four pieces. I sent a picture back to the seller, he has promised to do something (either refund or replace), but in meantime we are still without it.

Please explain what you mean by “good hot throw” I am not familiar with this term. I think for candles cinnemaldehyde extraction from cinnamon sticks would give the best results in terms of getting sufficient material with sufficient strength for reasonable materials cost, and “oily” enough to blend well with wax, but must confess no personal experience with candles.

By the way, many compounds that are the key aroma in essential oils are scandalously expensive (sold by ounce) if bought from perfumers, but cheap (sold by gallon) when bought as a chemical. It is more fun to make them yourself of course, anyone who makes their own candles would enjoy making their own scents. They are probably marketable as well, just put the scents into beautiful little bottles.

Oh, no! Sorry about that. Maybe put in an order for a Soxhlet from Amazon in the mean time.

Oh the soxhlet was ordered weeks ago, that came in OK, Kobin has it I assume he has taken it to the space. All distillation apparatus is in the long drawer marked “distillation”. Stir bars are hidden because they have unfortunate tendency to walk away or fall down sink, recommend you have your own and keep in personal bin, they are tiny and easily lost.

Also incense, food flavorings (though personally I’d go with ethanol or aqueous extraction methods depending on the base organic), organic pesticides, and in some cases medicinal precursors (ie low grade pain reliever from oil of wintergreen aka salicylic acid).