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Tobacco extraction using heated Ethanol

Discussion in 'Liquid Extraction From Tobacco' started by Str8vision, Apr 10, 2015.

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  1. brewbear

    brewbear Ultra Member Verified Member ECF Veteran

    Jan 9, 2017
    Wait a minute here, will ya'? Wait another month, you say? No shake 'n vape here?
    Just kidding, really. I actually bought a sampler set of six different net juices so I can try them. Not too bad. I guess that once I gather all the toys (temp controller, ....et. al) and get a little time, I will embark on this endeavor.
     
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  2. leftyandsparky

    leftyandsparky Vaping Master Verified Member ECF Veteran

    Nov 22, 2015
    Somewhere in the South
    I’m so use to shake n vape menthol, it’s driving me crazy waiting!:lol:
     
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  3. kbriggs

    kbriggs Senior Member ECF Veteran

    Jul 24, 2014
    Houston, Texas
    I just mixed up two batches of Voodoo Queen, one with extract made from 190 proof PGA and the other with 200 proof PGA that was made by drying 190 with molecular sieves. After shake and vape, they taste the same to me. I'll try them again after they age a couple of weeks. I also have two batches of "Black XX" still in the freezer that I'll be doing the same test on.
     
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  4. Str8vision

    Str8vision Ultra Member ECF Veteran

    Dec 26, 2013
    Sallisaw, Oklahoma USA
    That's good news @kbriggs I've been hoping the 4% to 5% water content of 190 proof PGA wasn't enough to cause a perceivable impact to taste/flavor. However, now that I'm set up to remove the water and produce 100% pure ethanol I'll likely continue doing so for the sake of purity.

    At this point in time I certainly don't recommend others burden themselves with the concentration process unless they have no other way of obtaining 190+ proof ethanol. I don't recommend using less than 190 proof for tobacco extractions. My experience using 150 proof PGA (75% ethanol 25% water) for extracting flavor from tobacco was a disaster, tasted terrible.

    I'm currently in the process of converting my first 1.5 liters of 190 proof PGA into 200 proof (100% pure ethanol) using 3a molecular sieves. I'm using 500g of 8-12 mesh size beads, they're quite small. Might end up being a mistake but I'm using a glass 1.75 liter Everclear bottle for the conversion, with 500g of beads the bottle still held around 1.5 liters of PGA (which surprised me) even with leaving ample head-space for stirring/mixing. The sieves don't seem to displace very much ethanol at all. After adding room temperature PGA (70F) to the sieves the bottle became warm to the touch, around 90F, a 20F rise in liquid temperature. It stayed this warm for about 30 minutes. I also noticed small bubbles rising from the sieves, every time I touch the bottle it releases dozens more bubbles.
    Conversion.jpg


    I've also tried the new temperature controller and so far it works great. What I really like about it is the temperature probe fits through the small steam vent on the crock pot's glass lid, my old one wouldn't. With the crock pot set on high and plugged into the "heating" outlet the controller turns it on/off to maintain the set temperature. According to my candy (mercury) thermometer the controller is dead accurate on temperature so no need to calibrate.
    Controller.jpg
     
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  5. Upinsmoke

    Upinsmoke Full Member

    Aug 2, 2017
    Suffolk UK
    Hi Str8vision how are you?
    Been reading this thread with interest.
    A few questions come to mind.
    Why 12 hours?
    Why 160 °f ?
    Have you arrived at these time and temps by chance or by reason.
    I definitely think the purest alcohol is the best method.
    Due to the hygroscopic nature of alcohol and glycerine, keeping water out of your juices is impossible but intentionally adding water does not make any sense if you want pure flavour.
    As you probably know medicinal herbalists have been making extracts for years. When I discussed this with my herbalist he was not keen on the idea of heating the herbal matter. He said the alcohol serves to break down the cell wall of the plant material. Perhaps there is something else going on besides just speeding up the process.
    If it were heated in a pressure vessel to an even higher temperature it might produce unexpected delights. Conversely just warming the alcohol to aid the process.
    I noticed the tabacco when soaked in alcohol becomes hard and brittle to the touch, whereas in VG it is softened.
    I tried softening with VG before drenching in alcohol. Not a raging success.
    My favourite mix to date was tabacco soaked in VG heated to around 180°f and left to sit for a few weeks.
    Now I have vacuum filtration I no longer have a problem filtering thicker liquid.
    For UK readers there is a guy on EBay selling 95% PGA wheatgrain 190°proof food grade for just over £20 per litre.
     
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  6. Str8vision

    Str8vision Ultra Member ECF Veteran

    Dec 26, 2013
    Sallisaw, Oklahoma USA
    Hi @Upinsmoke I've been doing quite well, just busy getting things around the homestead ready for winter.

    12 hours @ 160F was the result of exhaustive experimentation. I'm not a big fan of using excessive heat for flavor extractions but lower temperatures for a longer duration just didn't yield adequate flavor depth. Longer durations at 160F didn't provide perceivable benefits either. Higher temperatures are beneficial but for most people too hard to control since you're at the threshold of actually boiling the ethanol off. -If- you can accurately control the temperature (+ or - 2F), 170F is ideal. I have been able to obtain outstanding flavor from six month cold soaks but the results simply weren't as good as a 12 hour hot extraction followed by a few weeks cold soak, my current personal favorite method.

    I don't mind a little water in my mixed NET just not in the extraction solvent. During the actual extraction process excess water will muddy the flavor that is extracted from tobacco. 190 proof PGA already has a 4% to 5% water content and that amount seems to be acceptable but lower proof PGA (i.e. 150 proof PGA) is not well suited for use as an extraction solvent because it contains 25% water, far too much. Unfortunately, many people around the world don't have access to 190 proof PGA which is why I'm experimenting with the use of molecular sieves, to convert watery alcohol into pure ethanol.

    Medicinal herbalists have been my greatest source of information, it's where I got the idea of freeze filtering the extract to precipitate out unwanted gunk. People have been making tinctures since the dawn of mankind, lots of experience/wisdom out there.

    It does. ;) I just don't share my experiments/experiences when they involve potentially dangerous methods and or using toxic solvents. For a public forum I stick to discussing the use of non-toxic solvents and safe/easy extraction methods.

    Before switching to ethanol my favorite extraction solvent was a 70/30 PG/VG blend. Four hours @ 170F followed by a six week cold soak. VG does make it more difficult to filter but vacuum filtration remedies that. VG has long been used by herbalists as an extraction solvent with good reason, it's effective. I followed an herbalist's instructions for making vanilla glycerite (60/40 VG/water extraction solvent) and was amazed by the results, an outstanding vanilla extract. I even took it a step further, using high vacuum and low heat I was able to successfully remove most of the water once the flavor extraction process was complete. :) Two years later and I'm still using that extract, much better tasting than store bought.
     
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  7. Str8vision

    Str8vision Ultra Member ECF Veteran

    Dec 26, 2013
    Sallisaw, Oklahoma USA
    As you can tell by the first picture in post #1304, the molecular sieves deposit a very fine "dust" in the ethanol making it appear somewhat hazy. This dust is comprised of particles that are around 2 microns in size so they're pretty small. After some experimentation I finally ended up using a 1 micron glass microfiber filter and it worked beautifully. One thing I didn't like was the slow flow rate, it took well over an hour (twenty minutes per pint) and required two 5.5cm filters to clean 1.25 liters of pure (100%) ethanol. Next time I'll set up for vacuum filtration to speed up the process and pre-filter the ethanol through a 2 micron glass filter first. Here's what the fourth and final pint of finished product looked like;

    DUST FILTER.jpg
     
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  8. PeterRamish

    PeterRamish Account closed on request

    Jun 17, 2017
    California, USA
    After using 3a sieve to break the azeotrope Ethyl alcohol must be handled in a closed system.
     
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  9. brewbear

    brewbear Ultra Member Verified Member ECF Veteran

    Jan 9, 2017
    Digital temp controller - ordered,
    Busy Liz set - ordered
    Now, the hardest part, finding a little time!
     
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  10. Brad P

    Brad P Full Member Verified Member

    I think you will find the Busy Liz setup very useful. As far as finding time, good luck! ;)
     
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  11. happy valley

    happy valley Ultra Member ECF Veteran

    Nov 7, 2016
    WMass
    Uh-oh, now you've done it Str8vision, given me license to go off-topic!;)

    As of late I've been musing about brewng vanilla extract for mixing. Prompted by less than satisfactory attempts at cloning NT's ACB (RIP), I had been poking around some forums and it was suggested that one reason that recipe might remain elusive is because Kent made his own vanilla and it's quality and proprietary nature was perhaps going to be hard to duplicate with store bought options.

    I wonder if you'd care to elaborate a bit on your experience with vanilla?
     
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  12. brewbear

    brewbear Ultra Member Verified Member ECF Veteran

    Jan 9, 2017
    The digital thermostat arrived on Friday. It's getting close now!
     
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  13. brewbear

    brewbear Ultra Member Verified Member ECF Veteran

    Jan 9, 2017
    One step closer, my Busy Liz funnel arrived!
     
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  14. Str8vision

    Str8vision Ultra Member ECF Veteran

    Dec 26, 2013
    Sallisaw, Oklahoma USA

    :) My favorite NET is a vanilla tobacco hybrid with the tobacco up front, the star of the show. I lose the ability to "taste" vanilla after two dripper loads so I don't get to enjoy it very often, just once a week or so. The problem IMHO is that -all- concentrated vanilla flavorings fall short in flavor, most taste nothing like vanilla and the few that actually do lack any depth. I know this because in 2012-2013 I bought and tried every single concentrated vanilla flavoring that was available (dozens). Disappointed, I experimented with making a DIY vanilla extract and found that "real" vanilla extract doesn't translate well into vaping, at least not on its own. Smells and tastes wonderful and is outstanding for baking/drinks -much- better than store bought. Unfortunately, real vanilla flavor is quite fragile and when atomized (vaping) it loses its higher flavor notes due to the heat that's involved (my best guess). It does however impart a deep earthy vanilla nuance that the artificial vanilla flavorings all lack, a flavor very similar to that found in Frenilla and NT's vanilla base.....

    So far the best vanilla flavoring I've made (what I currently use) is a "hybrid". Homemade vanilla glycerite (dried) with "Holy vanilla" and/or "French vanilla" concentrated flavorings added in. When vaped the vanilla glycerite provides a deep earthy vanilla base while the Holy vanilla/French vanilla add the higher spicy notes, a winning combination for my taste preference.

    Problem is vanilla glycerite isn't an ideal extract for vaping, it has far too much water in it. To make vanilla glycerite you cold extract vanilla beans for a few months in a 60/40 VG/water solvent. Unfortunately, you can't simply evaporate the water off because VG is hygroscopic. I ended up gently heating the vanilla glycerite (~140F) while subjecting it to a high vacuum. This removed most of the water but it required a lot of specialized gear. The aroma was incredible, my shop smelled like fresh vanilla. :)

    PG also works as an extraction solvent for vanilla beans but not nearly as well as VG/water does. I haven't extracted vanilla beans in ethanol yet but the alcohol based vanilla extracts I bought didn't impress me at all. I also haven't tried using pure VG without water. Chances are next time I'll try using a 70/30 PGA/VG blended solvent (for the freeze filtering benefit) and just evaporate the ethanol off in the end leaving a 3-fold VG based vanilla extract. A lot of trouble to make but, for me, pursuit of the best is always worth the effort involved.

    Worst case scenario, if all else fails I'll end up making another batch of vanilla glycerite and break the vacuum/distilling equipment out again. The last batch has lasted nearly three years so far and I still have some left in storage....

    I agree, you'd need an earthy vanilla nuance to make a good ACB clone. ACB also had a bit of tobacco extract in it, not sure many people knew that. NT supposedly made their own tobacco extract but I suspect they just bought a commercial tobacco absolute and reconstituted it in-house, that's what it tasted like to me. Years ago I would make hybrid NET by adding tobacco extract to ACB. Ultimately, I replaced the ACB with a combination of Flavor West's "Caramel Candy", TFA's "Caramel Original" (in equal amounts) and my hybrid vanilla flavoring. Sometimes I replace the "Caramel Original" with Medicine Flower's (Lotus label) "Caramel" using it at around 1% since it's so highly concentrated. Caramel is my second favorite flavoring for making hybrid NETs.
     
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  15. happy valley

    happy valley Ultra Member ECF Veteran

    Nov 7, 2016
    WMass
    Yes, and for myself anyway, perhaps after too many years smoking exceedingly strong tobaccos, lamentedly that goes for almost all flavor concentrates I've tried. I guess that's why I am constantly tinkering with small batches, and why my flavor stash now numbers in the hundreds (much to the puzzlement of my non-smoking/vaping better half ;-)
    I did and think that's one of the reasons I like it, either straight or mixed in a hybrid. Frankly, much of my messing around extracting and mixing is in search of something, a NET based hybrid ADV, something like an RY4 but a DIY version, not the store bought variety, at least the one's I've tried.

    BTW, your version suggested earlier in this thread (or the other one on Best Tobacco) has been as close as I've come so far and remains a template on file in my recipes page, IE:
    I believe I'll experiment with extracting vanilla over the winter. I'd like to try vanilla beans in PGA and chime back in on that if and when appropriate.
     
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  16. Str8vision

    Str8vision Ultra Member ECF Veteran

    Dec 26, 2013
    Sallisaw, Oklahoma USA
    :thumb:
     
  17. Rickb119

    Rickb119 Ultra Member ECF Veteran

    Jul 20, 2013
    Greeley, CO, USA
    I've had good luck making RY4's from the following.

    H&H Louisiana Red
    PS Luxury Bulls Eye Flake
    C&D Orion's Arrow

    All similar profiles (VA/PER), but each one noticeably different, and very good. :)
     
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  18. Rickb119

    Rickb119 Ultra Member ECF Veteran

    Jul 20, 2013
    Greeley, CO, USA
     
  19. Rickb119

    Rickb119 Ultra Member ECF Veteran

    Jul 20, 2013
    Greeley, CO, USA
    @leftyandsparky

    It's been a month. Inquiring minds want to know. Is it any better?
     
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  20. brewbear

    brewbear Ultra Member Verified Member ECF Veteran

    Jan 9, 2017
    Was just wondering if a fining agent would work in removing the haze left by the molecular sieves. Sparkolloid and Bentonite come to mind. Since micro filtration systems are not easily found and a vacuum setup is not something everyone has handy, using a fining agent would be a rather inexpensive alternative....if it works.
    Bentonite clay powder is about $7 / pound and for our batches we'd use something like a teaspoon per gallon.
    Sparkolloid is $14 / pound, mix 1 tablespoon in 1 cup of hot water, good for 6 gallons!
    These are "memories" from the days when I had enough time to brew mead and beer:cry::(
     
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