View Full Version : separating hydrophilic essence oil
ristortion
2008-11-04, 23:31
nothing.
stateofhack
2008-11-05, 00:22
when freezing does not work, what are some ways to separate the oils from the condensate proceeding a steam distillation? (i am looking for various options here)
they considered distilling off the water, but were concerned that there would be some azeotropic association?
come to think of it should it even be mixing with the water like that? the liquid is very cloudy white and a few droplets are seen in the bottom of the funnel. i'm thinking his method of steaming is shit?
I do get what you wanna do, but not what your rambling on about :(
Care to make yourself more clear? What essential oil are we talking about here?
(if sassfrass oil, then you can freeze out the safrole!)
ristortion
2008-11-05, 00:33
nevermind.
FullMetalJacket
2008-11-05, 03:06
You've got an emulsion, by the sound of it. Either that or you haven't pulled much oil, jsut a bunch of shit which is now suspended in your water.
Try breaking the emulsion with brine.
ristortion
2008-11-05, 06:05
thanks guys
put water in flask with bark heat till boiling extract oil with a np distill off np then vac distill oil
Sweet. While I love my peers, I was getting kinda sick of LT being a mix of people who know everything, and people who not only know nothing but have no interest in learning.
Someone with pretty good knowledge is, like, a godsend. Congratulations, noob, you are breathing life into this forum. 'n since the regulars who were hanging on and dying of boredom really do know everything, your questions will be easy to solve, lol...
So... where are we...
hydrophilic... oil
Is an oxymoron. 'n
liquid is very cloudy
Is a suspension. Always. So...
they considered distilling off the water, but were concerned that there would be some azeotropic association?
...while this is impossible, you will be at risk to get a surface layer of oils on the steam droplets - essentially re-steam-distilling if you do so.
Ergo, I can think of a few solutions... pun intended on one of 'em.
1. Centrifuging the crap out of a suspension will force it to settle. At this point, a sep funnel will fix at least a large part of your problem, though you may have to kick a shard of epsom salt around the oil to get rid of the last water droplet.
2. Butane pull + sep funnel ftmfw. Serious defatting.
...or...
3. Tie a sock filled with salt to the lid, and let it sit for a few months. When you have dessicated all of the water from the jar, only oil will be left... and if nothing evaporates, but just absorbs into the salt, you'll keep your oil and lose water.
...there's also some neat tricks involving adding iso/'tone/ethanol/et al and cooking it off. Tends to take water with it. 1-3 should help you.
swim added salt and the oil layer grew by a couple mL's and became more defined, but the yields arent nearly what they should be. swim made work on 1 kilo of bark and now has apprx. 10 mL combined w/ nearly a liter of this cloudy aqueous layer.
I would reckon the easiest option would be to just sling in a reasonable (maybe 500ml) of an appropriate non-polar solvent (maybe diethyl ether, DCM or something) and just do a straightforward phase extraction. Sounds like you've just got a litre of shitty emulsion that needs separating...
ristortion
2008-11-05, 14:20
awsome
TheWhiteMan000
2008-11-12, 04:57
put it in a jar with 200-300 ml of chloroform, shake and let stand until the water is clear
incorporated
2008-11-12, 12:16
2. Butane pull + sep funnel ftmfw. Serious defatting.
How do you recommend keeping the pressure high/the temperature low enough to thoroughly mix the butane with the sol'n? If this is some serious defatting, and it sounds like it is, I would love to test it's efficiency on another application (involving cactus :) ).
More info, plz.
How do you recommend keeping the pressure high/the temperature low enough to thoroughly mix the butane with the sol'n? If this is some serious defatting, and it sounds like it is, I would love to test it's efficiency on another application (involving cactus :) ).
More info, plz.
I'm not convinced that butane would be the best/easiest solvent to use, as it would presumably evaporate in a matter of seconds. I'd imagine that something less volatile (ether, hexane, DCM, chloroform etc.) would be more manageable...
incorporated
2008-11-12, 12:49
I'm not convinced that butane would be the best/easiest solvent to use, as it would presumably evaporate in a matter of seconds. I'd imagine that something less volatile (ether, hexane, DCM, chloroform etc.) would be more manageable...
In the past, xylene was reported for the procedure to which I was referring. But if JP has some crazy idea on how to make butane viable, I'd like to hear it. It would have to work for ~1L of sol'n, in my case.
Also, I've constructed a working "honey-bee extractor" but don't think the same idea would work for liquid.
stupid noob
2008-11-12, 18:17
You would be surprised just how long it takes butane to evaporate.
You would be surprised just how long it takes butane to evaporate.
really?
I filled up a blowtorch recently and it took a couple of seconds for the leaked butane to fully evaporate...
stupid noob
2008-11-12, 23:12
I've done BTHO extractions before into dishes with edges, and it took over a full minute.
With a damn good ice bath, like ether and dry ice it could be made workable.
But if JP has some crazy idea on how to make butane viable, I'd like to hear it.
Well, there's two ways to implement phase control - temperature and pressure.
As SN noted, temperature's pretty easy - with a condensation point of -5c, a little table salt over common ice will suffice to give it all the properties of warm mineral spirits...
More interesting to me, because I'm stark raving insane, is pressure. 'n if one happens to have one's ghetto sep funnel with a valve on the inlet, a valve on the outlet, and a nice cozy hole above the inlet valve to trigger a butane canister, it just so happens that, much like inside the canister, a lighter, or anything else, it will not boil until pressure allows it to do so.
This is funny fucking shit, because when you release the outlet valve, gently-boiling butane will rocket-propel the expulsion from the sep funnel, even with a closed inlet. With sufficient butane, this will leave one with a concentrated goodies-laden (or in your case, trash-laden, unless you're a/bing for the cacti freebase in a glass dick) butane under butane atmosphere. All very self-regulating.
Of course, combinations can be chosen. If it rocket-propels the aqueous layer forth at too great a rate, one can chill it to just above the boiling point, instead of "majorly above boiling" (though it tends to cool itself with evaporation quite well, it'll at least slow it down a tad)... or, one could get lazy and actually drop the whole thing in an icebath 'till it's at about -10c, and just run it like a straight liquid, rather than a supercritical butane extraction in a pressurized sep funnel... or, lots of other things...
...but the boiling point of -5c is high enough that you could actually distill the solvent in a standard salted icebath without having to reach for the calcium chloride, the dry ice, or too much else in the way of special measures. Main problem there is that your aqueous layer freezes at 0c - unless you cut it with traces of ethanol, which presents its own issues in both defatting and subfreezing ethanol extraction into the np.
...but butane is really freakin' easy to get to be a supercritical solvent, to the point at which that is how it's usually encountered. 'n since it's not exactly super-flash-boiling above its bp - you won't get explosive decompression until you add either a spark or some measure of containment and containment failure - it can actually be worked with as a liquid at temperatures above its boiling point, if one is working fast enough.
...but mostly? Pressurized sep funnel at the temperature of your choice. Butane reflux between 5c and -10c from the boiling flask to the condenser would also work.
There's lots of options. Sky's the limit.
stupid noob
2008-11-14, 09:41
*waits for regulation of butane*
*waits for regulation of butane*
now that would be fun, I can just imagine the wave of zippo clones rushing to market whem bic's are banned.
And then some one in the position "learns" that zippo/ronson fuel can be used for ewul extractions and the fun bigins again.
While the rest of the world laugh their asses off.