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How to make vanilla absolute?

post #1 of 37
3/28/10 at 9:30am
Thread Starter 
Hi there,

I've read that it's the most difficult absolute to make. I want to give it a try and am really looking for the recipe and if you have some tips...

Thank you very much.
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post #2 of 37
3/29/10 at 2:57am
I would really like to know this too. I have some vanilla essence for cooking from Morocco. It says Vanilla extract in water, alcohol and corn syrup.
Can one doctor cooking vanilla in some way to make an absolute?
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post #3 of 37
3/29/10 at 5:09pm
Thread Starter 
Apparently, no one knows how to make vanilla absolute...

Actually, Vanilla extract is not at all vanilla absolute.

Vanilla extract is only for cooking purpose. You can make homemade extract with vodka. Here are few links to make your own extract:

http://www.instructables.com/id/DIY-Vanilla-Extraction/
http://bethanyactually.com/make-your...nilla-extract/
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post #4 of 37
3/29/10 at 8:34pm
I think you would need a LOT of vanilla pods to make an absolute, and you would need a method for doing solvent or CO2 extraction. Vanilla extract is a low concentration of vanilla aroma substances in alcohol, actually an infusion if you soak the beans in the alcohol. There's no reason why you couldn't use a home-made vanilla infusion as a base for perfumery or for cooking.
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post #5 of 37
3/30/10 at 1:52am
A big thank you for those links. Never mind the perfume aspect, I know what I'm making everyone for Christmas now. Fab.
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post #6 of 37
3/31/10 at 3:37pm
Thread Starter 
Thanks for your reply, Doc Elly.

For the amount of vanilla, it's not a probleme, I have a HUGE "réserve" of an excellent of fresh Bourbon vanilla from Madagascar. That's why I am looking for a method to preserve the quality of it and make my own absolute at a cheapest cost.

For the solvent or CO2 extraction, yes, definitely, I will need the method, but apparently, no one knows how to make it... I'll have to do a serious investigation on the net, and it might be tricky as it will request chemical knowledge , proprer supplies (but these solvents might be not sold to the general public) and of course, proper material.

I have a very good vanilla extract which I made from my beans (good luck, Mumsy!). I tried to make a scent with extract, not good at all... Maybe the vodka?... I really want to experiment vanilla absolute.
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post #7 of 37
3/31/10 at 4:41pm
argane, what was the matter with it, could you describe its faults?

i am planning to make a tincture with 95% ethanol for perfumery purpose. i've read that the yield is supposedly higher with 47% alcohol, something i find rather strange. however, i don't need something that's 50% water in my blends.

i would like to hear a bit more from perfumery people's experience.

btw. i was thinking along the lines of, mm.. i can use this extract to enhance my ethyl vanillin, to make it more complex and natural..
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post #8 of 37
4/1/10 at 4:35am
Maybe the enfleurage would work with vanilla too. I don't see why not. It's smelly enough and scents sugar strongly. I reckon it may work quite fast if there is enough oil in the pods.
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post #9 of 37
4/1/10 at 4:51am
i still hope the original question gets an answer. we have enough knowledgeable people here, but some of them i haven't seen around for a while.
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post #10 of 37
4/1/10 at 3:47pm
Thread Starter 
"what was the matter with it, could you describe its faults?", I don't get your question, gido...

I've never made a tincture with vanilla, it might be a thing to try. I don't have ethanol yet, I'll try to find out where to get in Toronto as I think, it's a hazardous material that cannot come from far, I am not sure if we can find it here....

Enfleurage might be another interesting experience. I've never heard about vanilla enfleurage though... Isn't that only for flowers?

For vanilla absolute, I've read on the net that it's made with hexane solvent, but it's a very dangerous material to manipulate, only in a good ventilated place (hard to do so when you live in an apartment and during winter time!!) and may cause lots of side effects. The list is very impressive indeed!! Not surprised about the high cost of absolutes!! :-)

Hope one of our expert Basnoters will be around this post one day and give us an accessible method for amateurs like us...
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post #11 of 37
4/1/10 at 11:00pm
Here's a site with some basic information about the process used to make absolutes. http://www.naturalingredient.org/Articles/cech2.html
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post #12 of 37
4/2/10 at 2:07am
Quote:
Originally Posted by Argane View Post

"what was the matter with it, could you describe its faults?", I don't get your question, gido... I've never made a tincture with vanilla, it might be a thing to try.

i meant the extract you made. if the alcohol percentage is 40% (or higher) then that is a tincture.
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post #13 of 37
4/2/10 at 7:32am
Thread Starter 
Thanks for the link, Doc Elly!

Hey, Gido, I used a 40 % vodka, so it was a tincture?? OMG!!!
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post #14 of 37
4/2/10 at 9:55am
argane, you still haven't answered my original question, 'what was the matter with it, could you describe its faults?' if you don't mind.

i just have purchased a couple of vanilla pods, going to make a tincture. and if it does not smell right, i still can still use it for cooking (after i add a little water).
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post #15 of 37
4/7/10 at 11:03pm
Vanilla absolute is made by solvent extraction. What you need is a lot of cured vanilla pods, cut them in pieces and soak them in a suitable solvent. Most common are pentane and hexane. Of course these solvents have to be free from any odor. After some time you remove the vanilla pods and replace them by others. After repeating this process several times you evaporate the solvent by vacuum distillation. The sticky residue is vanilla concrete. This you solve in alcohol. After some time you filter. The liquid contains the absolute that is obtained by evaporating the alcohol.

Just as with making essential oils it is a process that had developement, it was not invented in one day. When you want to learn it you better learn it from someone with experience, otherwise you have to do a lot of experiments before you even will obtain a reasonable product.
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post #16 of 37
4/9/10 at 10:38pm
Thread Starter 
Actually, gido, I replied to you by saying that I did'nt get your question about the "faults"of vanilla extract... There is nothing wrong with my vanilla extract, except that it's just an homemade extract or tincture, if you prefer, in a 40 % vodka, it's not strong enough to make a perfume and has nothing to compare with vanilla absolute. I just made it for fun and for cooking. I am only interested in vanilla absolute.

Hey, janmeut, thanks a lot for your advices. Waow, it's very complicated (I didn't know that vanilla beans have to be removed and replaced by fresh ones, I thought it's all melted in the solvent as vanilla absolute is dark and thick). You're right, it's a long process that has to be supervised by a specialist and I guess pentane and hexane are not easy to find although I've read somewhere that it's not very expensive... But with the number of different absolutes increasing more and more (we can find absolutes of everything nowadays : beeswax absolute, fir needle absolute and I don't know what...), there are still some possibilities...
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post #17 of 37
4/10/10 at 11:36pm
i was very surprised about the notes on vanilla absolute at tgsc, 'The highest concentration of vanilla aroma is found in the Vanilla Absolute. Vanilla Absolute is very dark black brown and solid. It is less rich in odor than the direct alcohol extraction products, and the perfumery effect is not proportional to its concentration over the vanilla tinctures.'

i have also found this recipe for the tincture, "vanilla tincture is the most commonly used perfume and flavour vanilla and up as 125g vanilla fruit pods too 1000g 95% ethanol and is therefore akin to an absolute, but then diluted 1:10 in ethanol" (Arctander, 1960)
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post #18 of 37
4/11/10 at 7:24pm
Thread Starter 
Quote:
Originally Posted by gido View Post

i was very surprised about the notes on vanilla absolute at tgsc, 'The highest concentration of vanilla aroma is found in the Vanilla Absolute. Vanilla Absolute is very dark black brown and solid. It is less rich in odor than the direct alcohol extraction products, and the perfumery effect is not proportional to its concentration over the vanilla tinctures.'

i have also found this recipe for the tincture, "vanilla tincture is the most commonly used perfume and flavour vanilla and up as 125g vanilla fruit pods too 1000g 95% ethanol and is therefore akin to an absolute, but then diluted 1:10 in ethanol" (Arctander, 1960)

Very interesting, but hmmm, tgsc seems contradictory to me: 'The highest concentration of vanilla aroma is found in the Vanilla Absolute. [...] It is less rich in odor than the direct alcohol extraction products, and the perfumery effect is not proportional to its concentration over the vanilla tinctures".... I have a serious doubt that vanilla absolute is less "rich in order" than alcohol extracts...
Immediately after reading your post, I've compared my tincture with Vanilla planifolia 10 fold EO to see ( I don't have vanilla absolute, that why I want to make my own...). Verdict: the EO (vanilla from India and 10 fold is usually less stonger than the 20 fold) is much stonger than the tincture made with the highest grade of Madagascar vanilla (maybe it's a question of proportion? My tincture contains around 25 vanilla pods (100g) for one bottle of 750 ml vodka though...). It would be interesting to make a tincture with your formula and see, but, I don't have ethanol yet.
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post #19 of 37
4/12/10 at 3:15am
no, you're wrong, concentrated means something different than rich. thus it is not contradictory to say the absolute is 10x stronger than the tincture, but the tincture is richer in odor.
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post #20 of 37
4/14/10 at 6:43pm
Thread Starter 
All right, got it, gido! Thanks for the precision. I want to make my absolute though... but not easy to find pentane and hexane. I've tried the Perfumer Apprentice and the goodscentscompany, nothing! I guess it's not accessible and might be solded only in large quantity and for industrial purpose only...
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post #21 of 37
4/18/11 at 8:20am
First off let me say that this is for the brave. NEED A PYREX BOWL
1.Can of pure butane-2.pvc pipe 7-8 inches long x 1.5 inches-3.Two caps that fit snug-4.In one cap (top) drill a hole that will allow the tip of the butane can to fit perfectly (test on wood).The other cap (bottom) should have a pepper shaker look (4 or 5 holes)-5.Fit a coffee filter into the bottom cap and secure to the pipe-6.Cut up your beans to small pieces and dry (1-2 oz dry weight per can of butane-20 beans or so)-7.Stuff your bean pieces in the pipe and close off with top cap-8.Go outside.Nowhere near people or anything that could create a spark and you want a breeze-9.Position pipe over the bowl and empty butane into pipe.When the drips are a couple seconds apart give a tap on the top to release what is left.Allow the solution to boil off 20 min or so OUTSIDE.You will be left with vanilla concrete-10.Add 90-100% rubbing alcohol to dissolve the concrete(not sure of amount)-11.Put into dark glass vials DONT CAP and store in a dark ventilated area for 2-4 weeks to allow the alcohol to evaporate.
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post #22 of 37
4/18/11 at 1:34pm
Apart from the danger, I would not use butane. It stinks. You will end up with vaguely vanilla-scented lighter fluid.
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post #23 of 37
4/18/11 at 3:37pm
Hexane also has a strong odor. As far as I know the odor will dissipate as the butane boils off. This has not been tested for this application, but the process has been used since the 60's to make honey oil.
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post #24 of 37
4/19/11 at 6:34am
Oh noes! wooznib is back and roaring! check this bad boy out. I think this is the perfect size for the at home perfume creator. My tax return is buying one of these as soon as it arrives. the key to butane extraction is that the odorants are filtered out of the butane you buy. I have successfully extracted essential oils in the method that nakedsweet mentioned. This extractor seems the most cost effective way to make your own absolutes and oils. There are quite a few videos on youtube showing how to use this device. Thoughts?
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post #25 of 37
4/19/11 at 7:13am
Dam, that thing is awesome. With the price of some absolutes it seems like a good avenue to pursue. Being able to use steel and not plastic would ensure a high quality product with no chance of chemical leech from the pvc. And SAFER as well.
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post #26 of 37
4/19/11 at 12:20pm
Quote:
Originally Posted by gwperfuma View Post

You will end up with vaguely vanilla-scented lighter fluid.

You're incorrect. n-Butane will completely boil off and no odor will be left behind.

edit: wooznib, thanks for that link!

Which size are you considering? 2 oz. or 8 oz.? The 8 oz size is nearly 4 times the price, which I think is an unfortunate mistake. If I bought one, I'd buy the smaller table top unit, even though I'd want the larger size. Having to spend over $4,000 for the 8 oz unit is enough motivation to get off my butt and make it myself if I need one that big.
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post #27 of 37
4/19/11 at 6:59pm
SF, do you know what the bp of butane is?
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post #28 of 37
4/20/11 at 8:55am
I am buying the 800 dollars unit with recovery tank. I can't wait to try this thing out. My mother gave me a 50 pound bag of home grown organic lavender.
I can only imagine vanilla would work extremely well in this unit.
Sent from my T-Mobile myTouch 3G using Tapatalk
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post #29 of 37
4/20/11 at 8:29pm
Wooznib, I am having a hard time finding the price for the smaller unit on the website (sorry so clueless...). Is the $800 for the 2 oz model?
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post #30 of 37
4/20/11 at 9:15pm
Quote:
Originally Posted by gwperfuma View Post

SF, do you know what the bp of butane is?

I didn't know off the top of my head, so I looked it up. I did know that n-butane boils at room temp., however. It turns out that butane's boiling point is -0.5 *C which is about 31*F.

@gecko. Here's a link to a different site run by the same guy, which seems to be more complete: http://www.tamisiumextractors.com/

@wooznib. 50 pounds? That's freakin crazy man! Lucky man, congrats! Your mom must have a big back yard. If she needs to get rid of any more I'd be happy to buy some...
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post #31 of 37
4/24/11 at 4:40pm
Supercritical CO2 would probably be the best for getting the vanillin and higher homologues. Nothing that some swagelock stainless steel and a quick browse through McMaster Carr couldn't fix!

For the amateur though: invest in a soxhlet apparatus and then carefully distill off the excess alcohol. A soxhlet has a porous paper cup or ceramic cup that the material to be extracted sits in, while a boiling flask is connected underneath. The boiling solvent evaporates travels into the condenser where it condenses and runs though the extraction cup. The solvent keeps boiling and keeps extracting, making it highly efficient.
http://en.wikipedia.org/wiki/Soxhlet_extractor
You can use different solvents (or make an azeotrope) to modulate the polarity. Vanillin is a phenol and an aldehyde (think aromatic alcohol, polar due to inductive effects), so it is water and alcohol soluble. This means that butane, heptane, pentane, hexane, and other aliphatic solvents won't work AT ALL.

I can make a tutorial if people would like...
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post #32 of 37
4/24/11 at 7:38pm
i haven't properly read this thread (very little time) but this is interesting stuff. chemistwithanose, a tutorial would be lovely.
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post #33 of 37
4/24/11 at 8:42pm
Chemist, thanks as usual for your insight. I a have a small Soxhlet that I have used successfully to extract various things into ethanol (e.g. tea, ambrette seed) . Your comment: "carefully distill off the excess alcohol" has always been my problem. I can find nowhere (on the internet...) that discusses other than in the vaguest terms, how to do that (same with tinctures). My assumption is one would want to evaporate the alcohol under a vacuum to keep the temperature low? Or is there an easier way (for hobby/tabletop)?

PS I bought a 48 watt 2 liter ultrasound machine over the weekend and I have been playing with it. I put a vanilla pod, cut finely, in 30 mls of ethanol, then sonicated it for an hour. Seems to work well, although I don't have an aged tincture for comparison. Also great for cleaning bottles and other lab glass, stainless items.
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post #34 of 37
4/25/11 at 11:59am
A vacuum would be ideal (I recommend getting a PTFE diaphragm pump from eBay, either by Vaccubrand or KNF Neuberger, that's what I use in my laboratory).

One could just use a water aspirator, or buy a recirculating aspirator (Brinkmann is a vendor). You need to get a good 24/40 distillation kit to put the extract in there. Or better yet, a rotary evaporator with a dry ice condenser.

I'll work on a tutorial when I have some free time.

Cheers!
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post #35 of 37
5/13/11 at 8:45am
Alright new question: What is the difference between an absolute and an oleoresin?
From my understanding the absolute is made from vanilla concrete which is the final stage of the C02 extraction (using whatever as a medium) and an oleoresin is made from an alcohol extraction and then added to a vacuum to extract the alcohol being left with an oleoresin. The oleoresin is supposedly stronger than the absolute(?). Also, how are their applications different? Which application is food grade vanilla extract made from and which is cosmetic grade (oils) made from?
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post #36 of 37
5/23/11 at 6:33am
I think you are talking about an oleoresin not an absolute. Absolutes are made with a cold extraction. Any extraction that uses heat will destroy part of the vanilla structure. Absolutes are made for aromatherapy and soap production because they are soluble in oil not alcohol. Whereas the oleoresin is used in industrial products.
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post #37 of 37
6/27/11 at 6:35pm
Thread Starter 
Wow, it's seems that everyone is interested in making home-made absolutes! Thanks to everyone, especially for the vanilla absolute recipe, but the "gasy" part really scares me! For the professional material, good to know all the details but it's super technical and costly for me!

Now, talking about oleoresin, my vanilla EO is already an oleoresin type, dark and strong liquid that is NOT oil-soluble... Referring to the other types of oleoresins, it may sound tempting because they are very concentrated liquid forms and are very affordable. But as you said, nakedseewtshop, they are not at all meant to be used for perfumery but only for food industry since they can be very allergic and even though some of them are soluble in alcohol and oil! Also, they need to be tinctured: http://www.newdirectionsaromatics.ca...-vo-p-646.html NDA. Generally, these oleoresins come from spices, so it is really worth to work with this type of material while essential oils from spices are really affordable??
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