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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. Upinsmoke

    Upinsmoke Senior Member Verified Member ECF Veteran

    Aug 2, 2017
    Suffolk UK
    Just a note of caution .
    Ethanol gets pretty volatile when you exceed 80°C .

     
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  2. thedesbois

    thedesbois Senior Member Verified Member ECF Veteran

    Dec 19, 2012
    Montreal, Canada
    Yeah I've seen it when I removed the bottle cap. Could have been a stronger reaction. Or God knows what if an open flame would have been near. I doubt I'll repeat the experiment in the exact same way. Maybe short ultrasonic bursts or some way of making sure the temperature inside stays below 80C. But if this test doesn't bring something better to the simple 12 hours warm bath... I'll see no reason to pursue further. 12 hours is not a long time when the whole process is taken into account. Maybe a few 2 minutes ultrasonic passes into the 12 hours. But then I'd have to add a timer control to the machine which I have not the skill to put together and code.

    I'll be careful out there! Thanks! :D
     
  3. Str8vision

    Str8vision Ultra Member ECF Veteran

    Dec 26, 2013
    Sallisaw, Oklahoma USA
    Dead accurate statement. :) My posts in this, and other threads, simply chronicle my efforts, experiments, discoveries, successes and failures while seeking the best home made NETs possible. I'll always tinker and experiment searching for additional improvements to the process. I've been on this journey for five years and am pretty happy with where I'm at but there's -always- room for improvement. A labor of love. ;)


    I'm real picky when it comes to flavor and back when I was making traditional NETs (using PG as the extraction solvent) I -had- to re-wick every 4 to 6mls. With the advent of using hot ethanol for the extraction followed by freeze filtering condensed extract I go three to four days between re-wicks which for me is 30 to 40mls of NET. Took almost five years to get to that point but it was time well spent IMHO. I certainly wouldn't want to go back to vaping the gunky stuff, it tasted good but having to re-wick twice a day would be a major PITA for me.


    I have considered slowly but constantly stirring the solvent and tobacco during the hot extraction process but have yet to built the apparatus needed to do so. I haven't experimented with ultrasonic cycling during a hot ethanol extraction but feel it could be advantageous to the process. Like stirring, I believe ultrasonic cycling might help circulate the solvent around and through the tobacco enhancing the flavor extraction. I'm interested in your observations/opinions, be sure to comment on your results. ;)
     
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  4. Str8vision

    Str8vision Ultra Member ECF Veteran

    Dec 26, 2013
    Sallisaw, Oklahoma USA

    FlippantSpiritedCoot-size_restricted.gif

    So... instead of enjoying home made NET, if not careful, a person could end up smoking again??
    :evil::)
     
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  5. thedesbois

    thedesbois Senior Member Verified Member ECF Veteran

    Dec 19, 2012
    Montreal, Canada
    Reporting back after my experiment with fast ultrasonic/heat extraction. Same steps as usual, only difference was that I replaced the 12 hours in warm bath by a 60 minutes ultrasonic blast and heat.

    Obviously I was lucky as when I removed the cap of my reagent bottle, some gas exited and the liquid inside bubbled like champagne when popping the cork. Probably lost some ethanol there from gas loss. No bubbles exited the bottle and they quickly went back down.

    Ethanol was most certainly heated above 80C inside the bottle. Warm water bath was set at 70C. But the constant ultrasonic cavitation effect probably heated the ethanol close to or beyond it's boiling point.

    That higher temperature might have played a role in the extract quality.

    I have mixed some e-liquid using this extract. And compared the taste with the same tobacco (Mac Baren Vanilla Cream) extracted in same manner except with a normal 12 hours warm bath. Identical PG/VG ratio, nic content, extract % etc.

    In a blind test, using two identical mods and atties (Snapdragon same builds and 2 Floris Orca's), I could not notice any difference. I tried. Really. My palate might not be the best. But for me, no noticeable difference between the two.

    Will I use this technique again? No. I have no way of controlling the inside temperature of the bottle. I don't like having ethanol do what it did on me. To save what, 10 hours? Not worth it for me.

    However this experiment indicates that 60 minutes of ultrasonic action plus warm bath yielded a similarly good extract to the one with warm bath only for 12 hours. So ultrasonic waves do play a role.

    If I could I would test a 12 hours warm bath with a programmed ultrasonic "zap" of maybe one minute at regular intervals during the 12 hours for a total of 60 "zapping" minutes. But I don't have the electronics skills to modify my ultrasonic cleaner to add this feature. Yes I could manually do it but that'd be a long 12 hours.

    I'm sure someone better skilled than me will be able to conduct such a test. Or someone that already owns some kind of programmable ultrasonic probe. They're expensive but that would be the best tool to use.

    Now back to the regular warm bath method for me. I might give my extracts some 2-3 minutes zaps during the 12 hours whenever I pass by the bath or think about it. ;)
     
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  6. Boscovlle

    Boscovlle Full Member Verified Member

    Feb 14, 2018
    Just scrolling through the post and saw your comment. Daughters & Ryan still sells NET's. I went to my local vape shop and they had 30ml samples. I took a couple home and tried them out. The Picayune, I believe it's a perique blend is STRONG. I don't know their process but it made me tear up. I called them because I thought it was a concentrate and they said it wasn't. I don't see how anyone could vape it straight.

    Sent from my SM-N950U using Tapatalk
     
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  7. Str8vision

    Str8vision Ultra Member ECF Veteran

    Dec 26, 2013
    Sallisaw, Oklahoma USA
    I'm glad Daughters & Ryan (D&R) stayed the course but they don't actually make their own tobacco extracts, turns out Purilum LLC (Nicotine River) does it for them. Purilum is a state of the art manufacturer, a laboratory and manufacturing facility rolled into one. By your description I'd guess they're producing extracts for D&R using Supercritical CO2, I know Purilum has the equipment on-site. Purilum also purifies their extracts although I don't know their methods for doing so. It could be that Daughters & Ryan NETs will be as clean as Heather's Heavenly Vapes (HHV) NETs the only other NETs I know of made using the Supercritical CO2 extraction method. I don't believe HHV makes their own tobacco extracts either but I've not heard who actually does it for them. I wish Cornell & Diehl, Samuel Gawith, Sutliff and others would follow D&R's lead.

    Suggestion; if you find D&R's NETs too strong do like I did with HHV's NETs, use it as a flavoring and dilute it down. When I tried HHV's "Shadow" (back in 2013 or 2014) what I received was -way- too strong, 30ml of Shadow ended up making/flavoring 90ml of vapable NET. ;)
     
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  8. Boscovlle

    Boscovlle Full Member Verified Member

    Feb 14, 2018
    This is their line up [​IMG]

    Sent from my SM-N950U using Tapatalk
     
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  9. thedesbois

    thedesbois Senior Member Verified Member ECF Veteran

    Dec 19, 2012
    Montreal, Canada
    I've been reading about freeze filtering with regards to dual process, reduce before or after etc.

    As I see it these are the options, after the 12 hours hot extraction and warm filtering:

    1- No reduction then Freeze filtering. (This is what I've done until now)
    2- Reduction then Freeze filtering.
    3- Freeze filtering then reduction.
    4- Freeze filtering, reduction, 2nd freeze filtering
    5- ... there may be other options... like multiple reductions and freeze filtering passes like Reduction/FF/Reduction2/FF2 etc. But I guess the extra ones will yield diminishing returns in terms of clean extract and flavor.

    In your opinion, not taking into account the amounts of loss to the filter, which step provides the :
    A Best Flavor
    B Cleanest extract ?

    Maybe they all provide similar flavor but the added steps only help in getting a cleaner extract? Or a cleaner extract with a slight loss of flavor? Then it would become a balancing act depending on one's preferences.

    I will try my next extract with a split to compare option 3 and 4. But I'd love to know if any of you who tried those coud chime in. :)

    Thanks!
     
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  10. happy valley

    happy valley Ultra Member ECF Veteran

    Nov 7, 2016
    Up on Bear Mountain
    Hello again all, got my hay fields first cut in, so time for a breather and to take a look to see what my ECF NET friends are up to. Also found time to bottle 8 varietal tobacco extracts I've had, they were first heat assisted in 190 PGA and then allowed to steep for 5 additional months. I'm decidedly no expert, only doing this for not quite 2 years, so final bottling and filtering is always a ponder, especially with the patience this hobby can require. ;-)

    The challenge I've had in making DIY NETs, as a heavy smoker for years, is having them finish up robust enough to keep me from wanting to smoke those darn lovely tobaccos I'm brewing. Hence I've sought to find a balance between getting a clean enough extract and filtering away too much of the particulate that contains essential flavor.

    I have come to realize that no amount of vape is ever going to replace the combustion experience with tobacco. So as I continue to remain disciplined and stay away from smoking, I've tempered my ideas on over filtering my NET extracts.

    This last batch of 8 tobaccos I'm mostly satisfied with strength wise, filtered once with a paper coffee filter to remove the tobacco, then into clean jars and into the freezer for 48 hours, then cold filtered a second time again with a paper coffee filter before final reduction. I've put aside the box of 1 micron lab paper filters I have, for the time being anyway. (a side note on filters, not that I think it makes a huge difference, but I'm using Chemex paper coffee filters and following a trick from a coffee brewing fiend I know, rinse the filter with a bit of distilled water before using it damp)

    That's where my NETs are at the moment. I'll continue to gauge my satisfaction with the process, and monitor the line between too much gunk vs achieving sufficient flavor.
    As usual, YMMV, hope all is well and best to all.
     
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  11. Str8vision

    Str8vision Ultra Member ECF Veteran

    Dec 26, 2013
    Sallisaw, Oklahoma USA
    Good to hear from you. I remember hauling hay for my grandparents in the simmering summer heat back when I was a young man, wasn't much fun.

    I haven't extracted anything lately, I have enough condensed extract in the freezer to last for decades. I've been working on my home and property which was (and still is) my retirement hobby/project.
     
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  12. Str8vision

    Str8vision Ultra Member ECF Veteran

    Dec 26, 2013
    Sallisaw, Oklahoma USA
    From what I can tell a second round of freeze filtering rarely yields any tangible results, if done properly the first round gets it all.

    IMHO freeze filtering reduced (concentrated) extract is only feasible/practical when larger extractions are in play (well over 1 oz of tobacco). It yields a slightly cleaner extract but filtering losses are greatly increased since the extract lost to the filters is "condensed". My last extraction (4.5 ounces of tobacco) yielded 900ml of extract which when reduced by 70% ended up being around 250ml of condensed extract. I then freeze filtered that 250ml of condensed extract and removed about 10ml worth of gunk and lost perhaps another 15ml to filters (absorption). 15ml doesn't sound like much but it's equal to 60ml of "regular" (un-reduced) extract and I have specialized filtering equipment that minimizes the amount of extract lost to filter absorption, most people don't. For people extracting small amounts of tobacco, freeze filtering extract before it's reduced is likely the best choice.

    There is an interesting but wasteful experiment that can demonstrate the difference between freeze filtering regular extract and condensed extract. Extract 1.5 ounces of tobacco in ~320ml of ethanol. Freeze filter the results. Reduce the freeze filtered extract by ~70% and then freeze filter the reduced extract. The gunk you'll see in the filter is what regular freeze filtering couldn't separate/remove before the extract was condensed/concentrated.
     
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  13. thedesbois

    thedesbois Senior Member Verified Member ECF Veteran

    Dec 19, 2012
    Montreal, Canada
    I see... so I shall not do the wasteful experiment with this batch. I'm still making tiny test batches. The one that's running is 0.4 ounce. Not a good candidate for a test. :) Will test once I've found a tobacco worth doing a large batch of.

    Thanks Str8vision !! :D
     
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  14. happy valley

    happy valley Ultra Member ECF Veteran

    Nov 7, 2016
    Up on Bear Mountain
    True enough, we used to put up 6000 square bales until we got the round baler, that now equates to 200 bales but we no longer toss'em, that's what the front loader is for ;-)

    And I've still got 49 lbs of aged pipe tobacco to extract, heh. Seriously, thanks for all the help, without it I would have given this up by now. Best of luck on your property project, I think I remember correctly you once mentioning it was a historic landmark, gotta be a labor of love.
     
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  15. Str8vision

    Str8vision Ultra Member ECF Veteran

    Dec 26, 2013
    Sallisaw, Oklahoma USA
    That's nearly triple what we had to haul each year! My grandparents were cattle ranchers and raised/stored their own winter feed. They eventually bought a hay wagon with auto loader which helped immensely, round bales became all the rage a decade later when I was gone attending college. Unfortunately, both my grandparents had passed by then and the ranch divided/sold. I'll never forget the years I spent with my grandparents, the fondest childhood memories I have. :)

    Built back when wagons/horses were the mode of transportation and most modern homes had only a few electric lights, it is indeed quite historic. The house predates the town and was once a sprawling dairy farm, I found crates of glass bottles and wooden bottle caps in one of the out buildings along with antique veterinarian gear a turn of the century cattle ranch might have had on hand. In the attic I found a treasure trove of antiques, too many to list. Many books from the 1800's and early 1900's. I have the very first addition of "Reader's Digest", stacks of old newspapers including one that announces "full page" Pearl Harbor was attacked. In addition to the dairy farm, the man who built the house also owned a hardware store, lumber yard and some sort of clothing shop. I have many of the displays used in those stores including the entry doors and signage. One of the people who eventually owned the house (a fellow engineer) graduated from Oklahoma State University located in the "Oklahoma Territory", found his diploma in the attic. Many, many stories about this house and its history, I'm absolutely enamored by it. A retired engineer, my goal is to modernize the house (and property) to ensure it thrives for another hundred years. I'm not just concerned with aesthetics but also want it be functionally and technically a step ahead of new house construction without losing its old world charm. A challenging project but yes for me it's truly a labor of love. I bought the house anticipating my retirement, to provide me with never ending projects and challenges. Some people plan to fish, others to hunt/camp and travel, I plan to create and build during my final years it's what I enjoy doing. ;)

    I had a lot of my favorite pipe tobacco on hand when I started vaping and making extracts but, unfortunately, that tobacco didn't make good NET. What I loved to smoke just didn't translate well for vaping, ended up getting rid of it all. That's what started my search (and thread) for "the best tobaccos for flavor extraction". For me, the tobaccos that make the best NET aren't anything I would ever have smoked.....go figure. It was difficult at first because the tobaccos I wanted to select were based on what I liked to smoke, I had to force myself to think completely differently which actually took a year or two to accomplish. Experimenting with different tobaccos/blends was a lot of fun, became a hobby for me. I'll likely still sample new blends during the winter months, you never know I might just stumble across a new favorite. Best of luck to to you and have fun!
     
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  16. Str8vision

    Str8vision Ultra Member ECF Veteran

    Dec 26, 2013
    Sallisaw, Oklahoma USA
    When I sampled new tobaccos I too performed small extractions. Ethanol is pretty inexpensive where I live but even so considering that only one out of ten tobaccos made a good NET I didn't want to waste a lot of ethanol on bad extractions. A quarter ounce of tobacco in ~50ml of ethanol was a decent sample size for me. After purification, filtering and reduction, I'd end up with about 8ml of condensed extract to sample. Most ended up tossed because I only kept the ones that truly impressed me. Those I'd extract larger batches of.
     
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  17. Upinsmoke

    Upinsmoke Senior Member Verified Member ECF Veteran

    Aug 2, 2017
    Suffolk UK
    Hi @Str8vision and @happy valley .
    Well they say birds of a feather flock together.
    As a kid I loved hay making , my dad would cut and turn the hay with an old Massey Ferguson and a 5 ft finger bar mower. The neighbouring farmer would come and bale it. Us kids would stack it all while dad drove the tractor . We'd all climb on the trailer sitting on the big stack of bales acting as a human net to hold any bales that might fall.
    After years of property development in London we bought a run down village school and 20 acres of land.
    Over the last 12 years we have been slowly getting the place in shape. The school and teachers house attached are now one with the main school room being our living room.
    We run a small herd of red poll cattle .
    In the early days I would make hay on some local meadows. My baler was just a few years younger than me , a Massey Ferguson 20/8. Fun for a while now I have a contractor do all the work. What with the cost of maintaining the equipment it's only marginally more expensive than doing the job myself.
    He makes 4ft round bales which are about 9 conventional bales by weight .
    This week we have the 4 yearly TB testing which is always a stressful experience .
    Pasture cattle get spooked having to go through the race. They have been getting training all weekend. Not worried about the TB , just getting them all safely through the race. Followed by doing it all again 3 days later. They get a couple of shots under the skin of TB serum which if they are carriers come up in raised lumps after 3 days.

    Haven't made any NET'S in a while.
    I liked the Dunhill Nightcap might do that again. Are there other Latakia blends you recommend?
    When I started I used to mix the NET'S very strong, now I'm finding less is more.
    I tend to mix and drip as I go.
    I have 4 drops of NET 4 drops of 20mg/ml nicotine and 10 drops of VG.
    I switch to another flavour or flavourless every other time.
    I find I lose the flavour if I keep hitting it.
    Trust you are all keeping well.

    Back when it was still a school , picture is about 100 years ago.
    Place was built around 1836.
    image2.gif
     
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  18. Str8vision

    Str8vision Ultra Member ECF Veteran

    Dec 26, 2013
    Sallisaw, Oklahoma USA
    :thumb:

    You might try C&D's "Constellation", for my taste it's better than Nightcap but YMMV
     
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  19. Upinsmoke

    Upinsmoke Senior Member Verified Member ECF Veteran

    Aug 2, 2017
    Suffolk UK
    Thanks I'll have to search for it.
     
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  20. MokumMan

    MokumMan New Member

    Sep 13, 2018
    NL
    This thread is a treasure trove! Before anything I need to say thanks to @Str8vision for sharing his journey for all to learn.

    I've read the entire thread during the past few weeks and meanwhile started to gather the needed gear to start trying out my own extractions. Also decided to sign-up to ECF to share the experience and hopefully learn some more going forward.

    I already have a few PG based cold extractions going (6 weeks and counting) and just started my first hot PGA extraction. Really looking forward to the results!

    Currently in the pot:
    - Dunhill Nightcap
    - Solani Aged Burley Flake
    - Samuel Gawith St. James Flake
    - Mac Baren Virginia #1

    I got the tobacco a bit sooner than some of the gear and was eager to start so the tobacco has been sitting in PGA for 7 days at room temperature before it went into the slowcooker. Still intending to let them sit for 12 hours but not sure if I should shorten the duration since they've already been in cold extraction for this long. But for now it is T-minus 12 hours!

    PHOTO_20180915_115530.jpg
     
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