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PLANofMAN

How to do a Cold Ethanol Tobacco Extraction in a home environment

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by , 01-07-2014 at 11:37 AM (1803 Views)
If the worst should come to pass, and the FDA criminalizes or bans vaping, or if nicotine vendors are no longer able to sell nicotine, vapers will need a fallback plan. Everything used in vaping is easily accessible, with the exception of raw nicotine. This may also be helpful to vapers in countries that restrict importation or distribution of liquid nicotine products like e-liquid.

If you came here looking for a recipe for WTA e-liquid, this isn't it. This is just a nice clean NET extraction. For the best WTA, go here: Aroma Ejuice Manufacturer of WTA Whole Tobacco Alkaloid Eliquid

Vaping items recognized as "easy to obtain."
Batteries: originally used by the high-end flashlight modders.
Personal Vaporizer: can be cobbled together by anyone with basic construction and tinkering skills
Atomizer: With easy access to both heating wire (Kanthal A-1) and organic cotton, anyone with a rebuildable atomizer will be set for life
Vegetable Glycerin: used as skin protectant and laxative. Can often be found at grocery stores and pharmacies.
Propylene Glycol: is commonly found at animal feed stores. Used as a food additive for cattle and dogs.
Flavorings: The flavorings we use now are primarily used by the food industry and are already FDA approved

The only thing that the FDA can do to stop vaping is to stop the sale and/or import of liquid nicotine.

In this situation, it is important to be able to create a personal supply of nicotine that is easy to make, relatively clean, and inexpensive.

So we must turn to Cold Ethanol Extraction. This method was first proposed by Lastlokeon as an attempt to produce a WTA extraction. In this, it failed. It did, however, result in the cleanest solvent tobacco extraction (NET) available. As a bonus, it also contained a spread of the nicotine alkaloids as well, though much reduced from what one would find in WTA.

The following method is Lastlokeon's, with a few refinements by myself (following suggestions made by jbbishop) and interspersed with comments and observations by Dvap as he reproduced Lastlokeon's method to determine alkaloid extraction percentages. (Note: Dvap does not endorse or recommend NET extractions).

EDIT: there have been some major changes to this procedure, based on additional input from Lastlokeon. I don't know what this has done to the numbers that DVAP came up with from his testing, so I will let them stand, for now.

If you see *Why this works! followed by a paragraph in italics, you can skip reading it. It's just there to provide further information.

Necessary items:
Tobacco. Any dried form will work. The tobacco used by Lastlokeon and Dvap was ordinary shag cut roll-your-own. Ideally you would want to use air cured low-nitrosamine whole leaf tobacco that you shred yourself. Whole Tobacco Leaves by the Pound, Buy Tobacco Leaf, Bulk Tobacco, Fronto Leaf, Cigar Wrappers, Binders, and Fillers This site has been recommended for purchasing cured leaf tobacco.
Ethanol. Any unflavored spirit will do, the higher the proof the better. Vodka in a pinch, but 190 proof Everclear (PGA) would be far better. This is what we are using as the solvent. If you decide to use Vodka, it will need to be dried and this process is covered later.
Freezer. You will need to freeze this tobacco cocktail for 4-12 hours. Lastlokeon did so for 6 hours. This is a catch 22. The longer you extract, the more nicotine you will get, but you will also pull more unfilterable organic solids and flavonoids.
Molecular Sieve. These little beads are properly called "A3 Molecular Sieve 4-8" and go by the commercial name Zeolite. They can be purchased on eBay.
Syringe and cotton ball.
Large glass container (x2).


Step 1. First things first. You will want to use 190 proof Everclear (PGA) or at most, bring it close to being anhydrous ethanol. Because pure ethanol absorbs water from the atmosphere, we will not be able to get it to a pure (200 proof) state, nor is this desired. In order for the extract to work properly, some water is needed. 190 proof is good, 195 proof is better, anything above or below those two numbers is not good. The ideal alcohol to use is about 95% pure with a 5% water content (195 proof).

*Why This Works! The reason we don't want much water in our alcohol solution is because water catches tars and resins that the ethanol won't. This is not a "clean" extraction, but anything we can do to avoid organic sludge being added to the extract is good. This is why Vodka, with a 60% water content, is a very poor choice for this extraction.
Quote Originally Posted by DVap View Post
Ethanol is going to pull out a lot of crud, even ice cold.
You will need about 10 grams of Zeolite per ml of water you want removed. a full fifth (750 ml) of Everclear contains about 38 ml. of water, and we want to remove half of that, so you would need to add about 190 grams of Zeolite to the bottle and let them absorb water for 24 hours. The Zeolite beads are infinitely reuseable and can be spread out on a baking sheet and cooked under a broiler at 140c to remove absorbed water. They can then be stored in an air tight jar for further use. This process can really be skipped if one is using 190 proof alcohol. If all you have available is Vodka, then this process becomes very necessary. When using Vodka, you stop the process when the bottle is just under half full.
*Why this works! The reason we use A3 Zeolite is because it has holes of 3 Angstrom (one Angstrom is one ten billionth of a meter) and can separate water (which has a diameter of 2.5 Angstroms) from ethanol (which has a diameter of 4.5 Angstroms).

Bake the beads first, then add them to the Everclear or vodka. Seal the bottle and then remove the beads after 24 hours. Re-bake the beads to remove the absorbed water and then store them in an airtight container or repeat the procedure as needed. I'm sure it goes without saying, but DON'T DRINK THE ALCOHOL! This method of creating anhydrous ethanol is courtesy of jbbishop.
Quote Originally Posted by DVap View Post
If I were interested in this sort of thing, I would definitely go with the previously suggested drying of the ethanol to remove the 5% water. Water is very aggressive when it comes to pulling gunk out of tobacco and ethanol far less so. I haven't exhaustively consulted the literature, but I believe that 100% ethanol should be effective for the extraction of alkaloid salts.
...
An additional comment I'd like to make is one that should be obvious, but perhaps is not to some. NEVER use denatured ethanol in a NET extraction (hashtag: #stupid). It's 190 proof from the liquor store or nothing unless you have access to anhydrous un-denatured ethanol (which is fairly unlikely).
Step 2. Shred the tobacco and use some of the 190 proof alcohol to dampen it thoroughly. Freeze and thaw this tobacco three time to ensure cellular disruption.
*Why This Works! Freezing and thawing the tobacco ruptures the cellular walls, allowing the oils to be extracted more efficiently.

Step 3. Put 100 grams frozen tobacco into the container, add chilled ethanol until the tobacco is saturated and covered. Place in freezer for 9 hours.

Step 4. Filter the contents through a sieve without compaction into a new container. A "permanent" mesh style coffee filter will probably work best for this. Discard the tobacco solids. Evaporate 70% of the remaining liquid. This can be done via natural evaporation, low heating of the solution (CAUTION: FIRE RISK) or through distillation. Refreeze for 24 hours. At this point you can choose to complete the evaporation process and then proceed to Step 5, or you can choose to follow the alternate Step 5a.

Step 5. Filter using the cotton ball and syringe method.

Step 5a. Alternate method: A
dd a few chips of dry ice (CO2) to the solution to cause additional solids to separate. While the extract is still almost frozen, filter using syringe micron filters for extra purity and clarity. Warning: Do not handle dry ice with your bare hands.

Step 6. You should have about 2-6 grams of a pale to golden yellow viscous liquid with a high nicotine content. Wear rubber gloves and handle this liquid as though it were pure nicotine.That means you need to dilute it with VG and/or PG before vaping it! Adding 240 ml of PG/VG should bring the nicotine content down below the 24mg mark.

The standard method of titration to determine nicotine content will not work on this product.
*Why this works! The nicotine and alkaloids produced in this manner are salts, not a purified freebase. Titration is designed to measure free base nicotine and won't detect nicotine alkaloid salts.

Like Dvap, I don't recommend making this, but if there is no other option, this is one of, if not the, best way to make a NET. I recommend that you print this off and store it in your "bug out bag," in case WTA e-liquid or commercial nicotine become unavailable. Vaping this is better than smoking...but not nearly as safe as vaping regular e-liquid.

Quote Originally Posted by DVap View Post
I happen to like the cold ethanol extraction as compared to other soak procedures when it comes to not making complete gunk.
Dvap won't vape this stuff. So let that roll around in your thoughts for a minute.

Folks in Australia and Canada might want to give this a try (because nicotine e-juice is restricted in those two countries...among others).

I have not made this, and will only make it in an emergency situation. You can do as you wish. I posted this here in hopes that it would be helpful to vapers with no access to liquid nicotine.
spdy and Mr.Mann like this.

Updated 02-14-2014 at 09:04 AM by PLANofMAN

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Comments

  1. names's Avatar
    Thanks for this useful post. How laborious is the desiccant process? Are there other adsorption means for the water on the ethanol? Would a low-temp distillation be effective to get the water percentage down?
  2. PLANofMAN's Avatar
    Quote Originally Posted by names
    Thanks for this useful post. How laborious is the desiccant process? Are there other adsorption means for the water on the ethanol? Would a low-temp distillation be effective to get the water percentage down?
    I used the desiccant process as the easiest example because you can buy $20-30 worth of molecular sieves and reuse them indefinitely. Adding 12 oz of desiccant to a 750 ml bottle of 190 proof alcohol makes it a one step process. All that remains is to strain the beads out before using the ethanol.

    I'll post some other methods (courtesy of jbbishop) but all either require distillation, or have the potential to leave unwanted residue behind.

    DISTILLING

    Alcohol can be distilled to 99.6% pure using a valved reflux still
    , but in some countries, notably America, distilling is illegal unless you have a license to run a distillery.

    DRYING WITH SALTS

    One method takes advantage of the fact that water will dissolve in most salts, but ethanol will not. Therefore, water can be removed (although not entirely) by filtering the alcohol/water through dry salt. Almost any “hygroscopic" (water absorbing) material such as calcium salt, various sulphates, phosphates and similar materials will work. However, common rocksalt, such as used in water softeners is cheap and available. Fill a drum or container with rocksalt. The alcohol/water is poured in at the top and filters down through the salt. Relatively water-free alcohol is collected through holes or a valve at the bottom of the container. Remember that the salt must be dry. After absorbing water from a certain amount of alcohol, the salt must be re-dried either in an oven or by spreading it out in the sun. Drying the NaCl out in an oven is very fast at 300 F. This is a popular method for those making their own gasohol. Cool in a closed jar.


    Don't expect salts working fast in drying, also with strong stirring it will take at least a day until the job is done and often it will be necessary to replace the salt with freshly dried one at least once. Distilling the dried solvent is advised as the salts are ALMOST insoluble in alcohol but not completely.


    You get EtOH to over 99% anhydrous with CuSO4 - time and changing the salt are necessary though. This 99%+ alcohol can be made completely anhydrous with NaOH - also time, weeks are needed here but it works. For drying alcohols CuSO4 is often used, it has the advantage that you can see if its wet as it turns blue then, anhydrous it is white/greyish.


    Anhydrous magnesium sulfate is commonly used for drying alcohols.... just don't use CaCl2, addition products will form. It probably won't work very well, but the idea is that upon heating magnesium sulfate in a dry environment, it gives up some of its H2O molecules... If put into a wet environment, it will then absorb those water molecules. Cool in something you can seal to stop the Magnesium Sulphate from reabsorbing too much water vapor from the atmosphere. Not a very efficient or easy process, but if you absolutely need to come up with a drying procedure, it might work.


    DRYING WITH LIME


    The oldest method of drying alcohol is dehydration with lime. This process is still used on a laboratory scale. It is similar to the salt absorption method just described except that, with this method, water is removed by a chemical reaction. Ordinary lime (calcium oxide, formula CaO) reacts with water to form calcium hydroxide (formula Ca(OH)2). The process is simple. The water-containing alcohol is mixed with lime at a ratio of about 35 pounds (or more) of lime for each gallon of water to be removed (as determined with a hydrometer) and allowed to “slake" for 12-24 hours with occasional stirring . The lime reacts with the water to form calcium hydroxide. The calcium hydroxide is insoluble in the alcohol and so the relatively pure (99.5%) alcohol goes to the top of the container and the calcium hydroxide settles to the bottom.


    The usual method of separating the lime and calcium hydroxide from the alcohol is by distillation. Alternately, but less desirable, the alcohol can be carefully drawn off (decanted) and filtered to remove any suspended particles that give it a milky appearance.
  3. Lastlokean's Avatar
    I have well documented information and personal experience demonstrating that 100% pure ethanol is not good for extracting nicotine. 95% and less pure is fine. The water is actually good for doing the dissolving. The ethanol allows it to exist as a fluid in the very cold environment. This 'critically cold' water azeotrope has a very selective solubility profile. Even if you bring alcohol beyond 95% it quickly absorbs water back from the air.

    I've had really good results lately with a slight change to my process for even less tar/coil gunking suggested to me in a PM by 18350.

    After filtering off cold alcohol from the tobacco only evaporate down to say, for example, 30% of initial. Freeze again and sit for 24 hours. This precipitates a bunch more plant waxes/fats/chlorophyll giving an even cleaner final product. But this can be taken even further with some dry ice. Drop in a few flakes of dry ice and watch even more gunk crystallize out. While it is still extremely cold, quickly push it through a high quality micron filter, and observe the purest NET possible.
  4. PLANofMAN's Avatar
    Thanks. That simplifies and streamlines the process even more. I'll update the OP with this info in the next day or two.

    I know I've given you a hard time in other threads, mostly due to confusion over the precise definition of WTA, but I really do feel that your process is a major contribution to DIY self sufficient vaping, and especially to vapers who have no access to liquid nicotine. I've never lost sight of that, even at my snarkiest.
  5. PLANofMAN's Avatar
    http://www.e-cigarette-forum.com/for...l-reserve.html
    Not really related, but worth looking into. DIY oak barrel aging might be a perfect complement to this process.
  6. Bagazo's Avatar
    The reason we don't want much water in our alcohol solution is because water catches tars and resins that the ethanol won't.
    Everything I have ever seen indicates that this is incorrect and that tars and resins are insoluble in water.

    It might help with other plant matter but as Lastlokean posted earlier, the cold actually helps with precipitation and it could be that the alcohol just helps in keeping the batch from freezing into a solid.
  7. PLANofMAN's Avatar
    Quote Originally Posted by Bagazo
    Everything I have ever seen indicates that this is incorrect and that tars and resins are insoluble in water.

    It might help with other plant matter but as Lastlokean posted earlier, the cold actually helps with precipitation and it could be that the alcohol just helps in keeping the batch from freezing into a solid.
    Um...I'm going to believe Dvap instead of you, but I'll leave your comment up. Everything I have ever seen indicates that Dvap generally knows what he is talking about.

    As far as the rest of your statement, of course the cold helps with precipitation. I get to see cold water precipitate out plant matter every time I properly louche an absinthe before drinking it.
  8. Bagazo's Avatar
    Quote Originally Posted by PLANofMAN
    Um...I'm going to believe Dvap instead of you
    Nothing wrong with that but I don't remember Dvap saying water was pulling out tars and resins.
  9. PLANofMAN's Avatar
    ...Water is very aggressive when it comes to pulling gunk out of tobacco and ethanol far less so...
    Tars and resins = "gunk"
    You can say that is my interpretation of what he said, if it will make you feel better, but I've read enough of Dvap's posts to understand that when he talks about gunk or crud, he is talking about vegetable solids/plant matter, which includes tars and resins.