Tincturing Violet Flowers?

Discussion in 'The Natural Perfumer's Palette' started by Woodland Note, Mar 25, 2019.

  1. Woodland Note

    Woodland Note Oud Fan Staff Member

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    Dear fellow ouddicts, the violet blooming season has begun here and soon the fields will turn purplish from fragrant viola flowers. I would like to make a tincture (I know enfleurage is the better way, but repeated tincturing might be much easier for me, and I don’t care about pigmentation much).

    What bothers me is not knowing which part of the flower is fragrant. They are too little to tell for sure using my nose. I tried dissecting their parts and smelling, but all the parts seem fragrant...

    I wish I knew for sure, is it whole flower? Petals? Stigma? The whole core? I have tried to find the answer on the web, but I failed. Some sources like fragrantica suggest it’s petals... Nonetheless it’s not very clear and convincing. Knowing which part to use would make the process more efficient. Less testing/trials. Better concentration of the molecules, and less water of plant origin in the ethanol tincture. I would be grateful for any suggestions.
     
  2. Mr.P

    Mr.P Oud Fan

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    I made a hexane extract of violet flowers. Just tossed the whole flower in. It made a strange smelling grease once the hexane evaporated (just a thin layer on the bottom of the dish which smelled amazingly fresh and lifelike when diluted way down.

    Violet is funny - the closer you try to smell it, the less you can detect the scent. If you think you failed, go away for a few hours and try again. Maybe apply this to your flower dissection, as you won’t be able to tell what smells like what for a while after getting your nose in it.

    https://io9.gizmodo.com/how-violets-steal-your-sense-of-smell-5913813
     
  3. F4R1d0uX

    F4R1d0uX Resident Artisan

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    Hi @Woodland Note !

    The only thing I know about violet is that its leaves are used to produce essential oil and absolute.

    If you use the leaves as tincture, you'd rather have a green leafy smell with maybe violet nuances.

    I never experienced violet tincture by myself.

    If I were you, I'd tincture both petals and leaves as experiment.

    Another one only with leaves and another only with flowers.

    To be honest, I'm not sure of the result you'd get. I bet it would be extremely mild scent (even weak).

    Violet blossom is being tinctured for medecine purpose, not for perfumery.

    It's kinda frustrating because it maybe my favourite floral lol.
     
  4. Woodland Note

    Woodland Note Oud Fan Staff Member

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    Thank you @Mr.P and @F4R1d0uX Those are certainly very helpful and valuable information.
    I might try solvent extraction with hexane as well, as it happens I know it’s sold in a hardware store near by. The only thing I’m worried about is petroleum-like smell... if it will all go away once evaporated or not if I use solvent from local hardware store, that might not be high purity. But it’s probably worth giving a try. @Mr.P what techniques did you use for evaporation of hexane solvent in order to separate it from the fragrant oil/concrete?
     
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  5. Feder Unix

    Feder Unix Whats this Oud About?

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    Hexane should not be used unless you know what you are doing and how to handle it, hexane is not a toy, however if you are determined on using hexane to extract a concrete from violet, you need to use some precautions. Hexane is very toxic for human and the environment [1], it's also highly flammable. You should distill the solvent out [2] after the extraction has completed, instead of just evaporating it, to avoid to release the solvent in the environment, also to get a proper extraction you should use a Soxhlet extractor [3]. If you will distill the solvent, please DO NOT USE AN OPEN FLAME, use a heating mantle or a water/oil bath and never use a flame or spark source nearby your hexane distillation/extraction equipment.

    Also after the hexane extraction you will be left with a concrete, which contains non alcohol soluble waxes, to remove the waxes, you need to wash out the hexane with alcohol 96%, you need to use a separatory funnel [4] to do that, after washing the hexane with the alcohol, and evaporation/distillation of the alcohol, you will get an absolute.

    BTW at your small scale is not economically feasible to make an absolute, it will be more cheap to purchase an absolute from a reputable supplier than making your own.

    On the other hand, making a tincture is more simple, it doesn't require any complicated and expensive equipment, nor handling dangerous chemicals and it will give you a decent result. You might only need a tincture press [5] to extract all the juice from the violets. You can make your own press or eventually use a potato masher and filter paper as a replacement.

    Good luck with your project and let us know the results.

    [1] https://en.wikipedia.org/wiki/Hexane#Safety
    [2] https://en.wikipedia.org/wiki/Distillation
    [3] https://en.wikipedia.org/wiki/Soxhlet_extractor
    [4] https://en.wikipedia.org/wiki/Separatory_funnel
    [5] https://www.permacrafters.com/how-to-make-an-herb-press/
     
  6. F4R1d0uX

    F4R1d0uX Resident Artisan

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    True @Feder Unix you need to have a low pressure distillation set up to make an abs with a heating mantle better than gas flame :Thumbsup:
     
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  7. Feder Unix

    Feder Unix Whats this Oud About?

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    Better safe than sorry

    [​IMG]
     
    Last edited: Mar 26, 2019
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  8. Mr.P

    Mr.P Oud Fan

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    Yes use caution with the hexane of course as you would with any flammable volatile substance. I suppose that is worth mentioning.... Don’t sniff the fumes, smoke cigars, or gargle with the hexane! It is basically a more volatile fraction of petroleum than gasoline so watch out for fumes, sparks, etc..

    I did my extraction outdoors, and used a warm water bath (again, outdoors) to evaporate hexane. Had a jar with the flowers and hexane. When I felt enough time had passed, I boiled water in my kitchen and decanted the hexane into a new jar, then set the jar in a bowl. Poured in enough hot water to not quite float the jar. The hexane boils off rapidly, giving the occasional swirl really helps move it along. I repeated until all the liquid was gone, then left the little residue on the bottom open to the air for a while.

    If you want to make it complicated and expensive you can buy vacuum pumps, rotovac, soxhlet. But the beauty of this is you don’t need any of that, regardless of what is usually done for the sake of efficiency, economy, etc..

    Super simple, no need to set up a lab and complicate things.


    Soak, evaporate, enjoy.

    Do not use alcohol! That’s a bad idea with fresh violet I promise - the tinctures of fresh flowers I have experienced are mediocre at best. Hexane is very selective for non-polar substances and thus does not extract all the polar garbage that alcohol extracts. With alcohol extracts there is this “vegetable” note that really detracts from the scent and the alcohol takes up the water from the flowers so the alcohol becomes more dilute with each change of flowers. I can’t recommend tincturing of anything but dried material.
     
  9. Mr.P

    Mr.P Oud Fan

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    You could try making a butane violet oil. Again, a dangerous activity if basic precautions are not taken, but might work really well.
     
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  10. Feder Unix

    Feder Unix Whats this Oud About?

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    I don't agree on evaporating the hexane, but if it's done on a small scale that is not going to harm too much the environment.

    Noted, that is a good info to know, thanks @Mr.P
     
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  11. Mr.P

    Mr.P Oud Fan

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    My batches were tiny experiments... maybe only 200 ml hexane. Good point about solvent recovery - it would be better not to release it.
     
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  12. Woodland Note

    Woodland Note Oud Fan Staff Member

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    Thank you guys for the precious input/suggestions. :Thumbsup:

    Yes, it will be a small scale operation, mainly for the sake of learning, not big expectations about the yield etc. :)
    I’ve been to hardware store yesterday, sadly I did not find pure hexane after all, but light compound solvent mixes, the most appropriate seems a one with boiling point below 80°C with 20% of hexane. There is pure toluene and xylene, but their boiling points are higher than 100°C so perhaps evaporation process would be more difficult.

    I consider trying butane extraction too. This way possibly could be much better, I’m guessing, easier to recapture the solvent with spartan ways, without any special lab equipment..


    Also thank you @Feder Unix for all the safety precautions warnings. :Thumbsup:

    @Mr.P Thank you once again! The “vegetable” note is what I’m actually struggling with in fresh sweet grass tincture. Tincturing sweet grass works well, but there are 2 problems. The smaller one is green strong pigmentation the bigger one is somewhat a bitter green/vegetable note. That is not how sweet grass violate compounds smell when I sniff a living plant. There is something extra in it, especially when it's fresh. So I might try sweet grass extraction with non-polar solvent sometime in future too.
     
    Last edited: Mar 27, 2019
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  13. Mr.P

    Mr.P Oud Fan

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    Glad to help. I love hearing about experiments like this. Extraction of oils really is best handled by labs or industrial facilities or whatever, of course, but it is always exciting to hear people giving it a go and extracting something special or of personal significance. I wish there were some easy simple compact solvent system to make this more streamlined. Someone here was posting about an automated ethanol extractor but I guess they never actually did the extraction as they never posted back about their results.
     
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  14. Woodland Note

    Woodland Note Oud Fan Staff Member

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    Violet experiments are progressing with quite satisfactory results! In 4 small jars, 1 x tincture and 3 x petroleum ether.
    2 days ago I evaporated 20ml test sample of the petroleum ether extract, and it showed up just like Mr.P said. :Thumbsup: It smells very beautiful once dissolved back again in ethanol.

    I will update soon with more info and pics.


    On a side note, it seems like there are many types or perhaps subspecies of wild violets here.
    Of different sizes and colors, from pale white to deep dark violet, pinkish, purple, blue, various tint of violet color.
    And they seem to smell differently. I like the most scent of the small deep dark violet color ones, it’s strong and as I've always thought about violets, most familiar to me. But there are violets with a lighter shade of violet color, almost pink, that seem to have more creamy light scent. Some don’t seem to have much scent at all. (might be the anosmia thing too, I’m not entirely sure) And there are the larger ones, more violet-blue like color with thicker petals which seem to smell hmm a bit in a way of ammonia/urine does... I know what you might think... that someone/something peed on them. Well, maybe, but unlikely. I got it only from the particular size/color ones that I picked in a few different parts of area, I cared to pick them in non-easily accessible places, unlikely visited by anyone. I don’t imagine human or dog climbing there to pee on it, maybe cat, but yeah, I’m convinced it’s just the type of the particular violet scent. Hmm... or maybe it’s because of the saturation of some scent compound in these larger thicker violet petals? Or maybe something in the soil absorbed by the plant? Either way I’ve decided to not use them, to be sure. I used all other violets, though sometimes they look similar.


    For the tincture I used only small classic violets I found among conifer trees here on the yard.
    For the ether extract mix of different ones gathered in area, but trying to avoid the ammonia-like smelling ones.
     
    Last edited: Apr 8, 2019
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  15. Mr.P

    Mr.P Oud Fan

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    Violet is so strange. I can tell if just one or two flowers are open when I’m cleaning my roof, from a large distance, but can’t smell a thing when I stick my nose right in the flower half the time.

    I also smell the urine / animal note. I think this is just part of the allure of violet. It has two sides...
     
  16. Woodland Note

    Woodland Note Oud Fan Staff Member

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    Petroleum Ether Extraction

    1st Stage: Gathering Flowers

    Can you spot the violet flowers? This 1-2 hectare field by the river was full of them, almost every square meter had some and I’m quite convinced I did not harm more than 1% of the flowers there. (The violets there were not having as strong scent as the ones growing on my yard and in other areas though. I’m not sure if it’s about the soil, flower variety, sunlight exposure, or some other factors.)

    violets-river-side-p1.jpg

    violets-river-side-p2.jpg

    At home:
    violets-from-the-riverside.png

    I left them in this glass container for around 30 minutes, occasionally shaking it, in order to make bugs come out, there were not many, but there were some.

    2nd Stage: Maceration
    violets-in-ether.png

    Filling the jar...

    mixed-v-in-ether-20hours.png
    After some time in the ether bright bubble like formations could be observed in the flowers, including petals.. Water? Air? I would be guessing water.
    Speaking of water, I was thinking it will come out and form separate layer on the bottom... but I couldn’t notice any such separation.
    By the way, the white flower that can be seen in the jar is just the white variety. :)

    pe-extract-p2.png

    The extraction liquid turned slightly hmm... it got slightly golden tint to it after 2 days.

    (I did 2-3 cycles of more or less 48-72h maceration in same liquid with new batches of flowers, before the evaporation.)

    3rd Stage: The Evaporation
    pe-extract-p3.jpg

    pe-extract-p4.jpg

    When the solvent almost evaporated and the color got denser, more saturated... golden, tad greenish maybe... it looks fluorescent, and it is indeed in uv light.

    pe-extract-p5.jpg

    The Final Product:
    pe-extract-p6.jpg

    Kind of waxy thing, with an intense violet/floral odour. I left it as it is for 30 more minutes in a room temperature to make sure all the solvent is evaporated.
    pe-extract-p6b.png

    And once re-dissolved back in 95% ethanol:

    pe-extract-final.jpg


    pe-extract-final2.jpg
    (3ml glass vials) From the left: 1 the evaporation test sample (mentioned in the post above), 2 the rest of the first jar, 3 from the second jar, 4 the washing of the leftovers from the second jar.

    pe-extract-final3.jpg

    For the second jar I used a different petroleum ether, sold as a carbrake cleaner spray. The result was quite similar. I have not noticed significant differences.

    One tip though, for those who would like to try it. Test petroleum ether first. In the hardware shop near by there were 3 different brands. In a sneaky way I opened bottles in a shop to sniff which one gives least smell. I picked one. But at home when I did some trial with a paper tissue, after the evaporation it showed up that chemical/naphta scent was left on the tissue for long hours. So I got another brand, that once evaporated was leaving no scent instantly. The car brake cleaner had almost no scent, and was not leaving any behind as well.



    I'll post some more pics and stuff later.
     
    Last edited: Apr 12, 2019
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  17. Mr.P

    Mr.P Oud Fan

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    Beautiful post. I have found the variety of violet seems to matter in terms of odor intensity. I have encountered a number of varieties of wild and cultivated violet and only one has a really strong scent - a large-leaved, very dark purple variety. I’ve noticed that some pansies have a very strong violet aroma as well.
     
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  18. Woodland Note

    Woodland Note Oud Fan Staff Member

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    Thank you! And yes, indeed, that’s my observations as well.
    I’ve been thinking about pansies, since they are violets too, but somehow I haven’t tried to sniff them for a very long time...
     
  19. Woodland Note

    Woodland Note Oud Fan Staff Member

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    Tincture (95% ethanol)

    Violets from the yard, with an intense pleasant powdery odour:
    first-violets-from-the-yard.png

    And a few minutes after first submerge in ethanol:
    tincture-just-sumbmerged.jpg

    I observed some groovy color changes. First minutes with fresh ethanol the color was turning to violet, then pinkish and to light green at the end. When I was tincturing another batches of flowers in the same liquid it was at first turning to kind of how would you expect, somewhat pink/purple and then back to green again.

    tincture-2.jpg

    I was tincturing each batch of flowers for a few hours, followed with a bit of washing with clean ethanol to gather more stuff.
    After many batches, the liquid color got darker, more saturated green, kind of like dark virgin olive oil.

    Interestingly if some of this liquid is evaporated it leaves violet color pigment residue when it’s fresh, but after some days passed it leaves vivid turquoise-green color residue.

    tincture.jpg

    I was tincturing flowers only for a few hours because I just thought to myself that flower scent compounds/oils might come out faster, and water slower, so I decided to do it each time only for a few hours. There is no factual logic to it.

    As for the ethanol/water ratio, I was thinking to myself about using alcohol content meter, one that people use to check on their high percentage brewery. But I did not do it after all, cause I kind of can tell with my eye by judging liquid flammability if it’s (more or less) 40%, 50%, 60% or more, and as long as it’s 60%+ then I think it’s fine, it should not spoil.

    How does it smell? Well, not really like a violet flower, but surprisingly not that bad either. Somewhat green/floral, bittersweet. There is violet flower note somewhere in this scent, though it might be not obvious.



    To sum it all up, I’m much more happy with the ether extract. (Thanks to @Mr.P encouragement :Thumbsup:. Otherwise I would probably not dare to try it withouth proper lab equipment.)

    So, how does petroleum ether extract smell like? Floral, hmm, much more like flowers I guess, but very very intense, and much much sweeter. It’s strange scent when it’s in such concentrated form, but once diluted... MMMMMMMMMM... delightful! :):Thumbsup:

    This might become a serial thing for me. :) Next I plan to do ether extraction of white lilacs, which will blossom here in around 3-5 weeks from now. (The purple ones have also a beautiful scent, but a bit different, and I prefer white ones.)
    And then common clover flowers. I’ve tried tincturing some clover flowers (not every clover flower seem fragrant) around 2 years ago, but the result was terrible. I guess most flowers are not suitable for tincturing indeed.
    But this non-polar solvent extraction is very promising so far . In future I may try to acquire some a proper lab glassware for a more efficient extraction and solvent recovery (so that I do not pollute the environment and my lungs).

    violets-by-the-river.png

    v-lighter-creamy-variety.png
     
    Last edited: Apr 12, 2019
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  20. Sproaty

    Sproaty Sproudy Staff Member

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    very informative post, Mr. Note :)
     
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