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  1. #1

    Default "Washing" oils with ethanol

    All the chemists out there, please lend a hand. I have obtained a most exquisite smelling Poplar oil from Saltspring Island here in British Columbia. It was made by harvesting the spring buds of populus balsamerifera and somehow getting their essence into apricot kernel oil. I don't think any distillation took place. I now have the idea of using a separatory funnel to "wash" the oil with 95% ethanol to see if I can get the essence out of the oil and into alcohol so that it's easier to work with in perfume formulations. Any advice would be appreciated. I do have a degree in organic chemistry and worked as a chemist for a few years way back in the 70s, but it was so long ago I cannot remember everything. For instance, is there something I can put into the mix that will sort of "chase" the various terpenes and things out of the oil and into the alcohol? Also, what would you recommend for proportions? I know that it's best to do a series of washes, but how much oil and how much alcohol (relatively speaking) would you use for each wash? I only have about 25ml of this poplar oil, so everything will be done on a very small scale.

  2. #2
    gecko214's Avatar
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    Default Re: "Washing" oils with ethanol

    I am sorry no one answered yet. I think it is an interesting question, but, as you suggest, on best answered by a chemist or someone with experience. Forgive me if I am stating the obvious, but from the reading I have done, it sounds like what you are proposing is basically the same as the last stage of enfleurage or maceration, washing the pomade or oil in alcohol. How exactly this is done best is still not completely clear to me and probably something of a(n old) trade secret. My guess is if you just take 50% ethanol and 50% of your oil, put it in a bottle, shake regularly, you will get the desired result. BUT, with 25 mls of a macerated oil you end product is likely to be minute... just a guess as again others are probably more qualified.

  3. #3

    Default Re: "Washing" oils with ethanol

    I had great success washing the essence of Poplar Bud from the carrier oil. I obtained a 60ml seperatory funnel from a chemistry lab and put about 5ml of oil in. Then about 10ml of 95% ethanol. Shook for a while, then seperated. Then washed the oil again with another 5ml of ethanol. I combined both ethanol fractions then filtered into a dropping bottle. Result: I now have an amazing tincture of Poplar Bud EO. Really nice.

  4. #4

    Default Re: "Washing" oils with ethanol

    As a fellow resident of Cascadia (what we USAians call the "Pacific Northwest"), I must say that sounds exquisite. I can't wait to hear what you decide to make out of it.

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    gecko214's Avatar
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    Default Re: "Washing" oils with ethanol

    Good to know Bshell, sounds very nice. And it gives me courage to try my own enfleurage/maceration, as the "washing" part was always what I was afraid of.

  6. #6

    Default Re: "Washing" oils with ethanol

    Just make sure you have a proper separatory funnel to do the job and know the technique. You shake, then open the valve with the contents in the bulb part of the sep funnel. You have to do this because gas is created by the shaking and you have to release the pressure. A separatory funnel looks like this: http://www.chem.ucla.edu/~bacher/Gen...Sepfunnel.html

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    gecko214's Avatar
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    Default Re: "Washing" oils with ethanol

    Thanks I do have a sep funnel. Would it not be okay to do the shaking in a separate container and then transfer to the sep funnel for the final operation (separation?)

  8. #8

    Default Re: "Washing" oils with ethanol

    I guess you could, but why? I worked in an organic chem lab for several years and I never saw this done. Washing *in* the funnel was always the way. Also, be sure to do at least two washes. You'd be amazed how much more comes out in the second wash. This all has to do with things like partitioning and equilibrium. You can look all this up in organic chem books.

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    gecko214's Avatar
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    Default Re: "Washing" oils with ethanol

    Good to know thanks. Why? My thinking was because I may have say 2 liters of oil/alcohol mixture but I only have a 500 ml sep funnel, so once shaken in a larger container would pour and separate in stages in the funnel.

  10. #10

    Default Re: "Washing" oils with ethanol

    What length of time did you 'wash' for? I have some lovely Thai smellies, Frangipani, lotus, rose, sandal, jasmine, lavender and a musk, each in a Thai version of olive oil. Doesn't the oil dissolve in the alcohol? Not that I mind getting some glassware, but can I do this at home without the separator equipment?

  11. #11

    Default Re: "Washing" oils with ethanol

    Ethanol is a polar solvent, like water. Oil is non-polar. By polar, I mean it has a positive + end and a negative - (minus) end. Oil is non-polar. This is why water and oil don't mix. To be perfectly correct, they mix, but only a little bit. Most of the oil stays in the oil, and most of the alcohol (or water) stays on the water side. So anything in the oil that is soluble in alcohol will cross over into the alcohol when you shake the oil and alcohol together. The first time maybe 60 or 70% will come over. Then if you wash again with fresh alcohol, you will get another percentage. You'll never get it all. Your oil will still smell, but lo and behold, a LOT of the fragrant elements will now also be in the alcohol. Of course any that are simply not soluble in ethanol will stay over in the oil fraction. I find alcohol easier to work with when making perfumes. So it's great to have all one's smells in alcohol and not in oil.

    You could probably do it at home without a separatory funnel but it won't be as efficient. When you shake your alcohol and oil together, use small amounts of alcohol, so that the end result won't be too dilute. When you do the shaking, after half a second, you have to release pressure, by maybe unscrewing the jam jar lid, or whatever it is you are shaking it in. I shook mine for a few minutes. Maybe 3 or 4 minutes. After you shake it a second time, release pressure. After those two, you can probably shake and shake and shake and there won't be a pressure problem. Now comes the separation part. First you let the mixture sit for a while, maybe ten or 20 minutes so that both fractions separate into layers. The beauty of a sep funnel is that it is tapered in a cone shape at one end. That's good, because when you drain off one layer, from the bottom, the region between the two layers is kind of amplified so you can really see where the separation between the two is. I guess if you can find something around the house that has this conical shape then you will be ok. Otherwise, you won't be able to separate the two layers as perfectly, or as efficiently as with a real separatory funnel.

    By the way, this is why shampoo bottle instructions say to "rinse and repeat". You are basically washing your hair twice to get the oils out. The second time a greater fraction of oil comes out. You can wash oils with a sep funnel three times to get out even more, but each time you are using more ethanol and getting less and less out of the oil, so it could be diluting things too much and you reach a point of diminishing returns.

  12. #12

    Default Re: "Washing" oils with ethanol

    How am I ever going to get any work done? I just want to play. I have ordered some filter papers and pipettes too. Not the separation funnel.... yet. Maybe washing up will have a new fascination knowing that I need to do it twice to be truly efficient!!!!

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