Kitchen WTA extraction method.

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tceight;1775588 said:
I can't see anything dangerous in here, short of conventional kitchen hazards such as hot oil, and I would pit the end product against burning tobacco in any safety test one can come up with.

So here it is, a kitchen chemical AcidBase extraction, with no concentration of nicotine to dangerous levels at any point.

Gear
- small metal or glass pot. size determined by the batch you wish to do.
I was working with 20g of tobacco at a time, so a small pyrex measuring cup makes a great 'pot'
- coffee grinder,
- 10ml syringe with a blunt tip needle.
-large turkey baster (60 ml)
-coffee filters.
-spatula

ingredients.
- good rolling tobacco, not 'reconstituted leaf'. or better yet use uncured leaf tobacco if you can get it. (no TSNA's)
-baking soda
-light mineral oil USP
-cream of tartar
-propylene glycol or glycerin
-tumeric (optional)
-salt (optional)
-distilled water

step1.
- boil a few (50) ml of distilled water, and dissolve the baking soda into it until no more will dissolve. This is your alkaline solution to free the salts in the tobacco and is about pH 11
- saturate a few ml of distilled water with cream of tartar. room temperature is fine, this will be used at the very end.

step2.
- measure out 20g of tobacco. this is about 3/4cup loose settled tobacco.
- grind up the tobacco into a powder, and add about 0.5 to 1 drop per gram of the solution in step one. You want the tobacco barely moist and not wet at all. (in my case with 20g I added about 12 drops, depends on how dry the tobacco is in the first place)
-let this moist powder sit for about 30 min. this allows time for the salts to convert, as well as the cell walls to break down, releasing the alkaloids.
-optional to step 2, bake some baking soda at 400F for an hour to convert it to sodium carbonate, and add a gram of this to the tobacco while grinding. Still, ensure the tobacco is moist.

step3.
heat 20 ml of mineral oil to about 212F and add the tobacco powder to it. Let this sit and steep for about 30 min to an hour

step4.
take off the squeeze bulb and stuff a small piece of coffee filter into the small end of the turkey baster. If you can't find a large enough baster, a 60ml HDPE syringe works great. spoon the oil/tobacco mixture into the baster, Set the baster vertically over a small cup to catch the filtered oil dripping out the end. Very little if anything will come out at this point. (caution, remember this is HOT oil)

step 5. heat up another 30ml of mineral oil to about 200F, and pour on top of the oil/tobacco powder in the baster.

step6. Wait....leave for 24hrs or longer. The viscosity of the oil, and the fineness of the powdered tobacco really slows things down. There is an advantage to doing it this way, as we end up with a very concentrated oil, with a minimal number of extractions. The clean oil seems to create an interface and slowly displaces the oil in the tobacco as it drips out. A bit like column chromatography or IX dedeuteration.
***The first time I did this, I didn't heat the oil up first, or mix it with the tobacco. I just poured the oil onto the top of the dry powdered tobacco. It took 24hr's just to saturate the tobacco, and another 4 days to get 25ml back.

you should now have about 25-30 ml of dark amber oil in your catch container. And we will optimistically 'assume' about 200mg of alkaloids. There will also be some very small fines that got through the filter, as well as some carbonates from the baking soda that made it through.

step 7. (optional, but really cleans things up a lot)
take 25ml of distilled water, this to the oil, and shake well for a few minutes. Let settle and separate into layers. (may take 10-20 min) The oil will be lighter in colour now, more yellow than amber. There will be some small loss of alkaloids in this step, but because the water will become quite alkaline from the contaminants it absorbs, the alkaloids should still be preferentially dissolved in the oil.
Keep the oil by siphoning off with a syringe and discard all the water and any emulsions that formed.


step8.
add a tiny 'pinch' of cream of tartar to the oil and shake well.
it won't dissolve in there, but that is not what we are trying to do.
we are just attempting to displace any of the leftover baking soda particulate with the cream of tartar, so that in the next step, the acidic polar solvent won't be neutralized by any remaining baking soda.
Let the particulate settle, and pour off the oil into a clean container.


Step 9.
add a drop of the cream of tartar water you made in step one to your PG or glycerine, 1 or 2 drops per 10 ml is enough.
- add 10ml of the PG to the oil, shake well, let separate, and extract the PG with the syringe.
- add 10ml, shake well, let separate, and extract the PG with the syringe.

- assuming there is 200mg of alkaloids in the oil, you would add 10ml of PG to get 20mg/ml.
This stuff is way stronger than any nic juice i've tried, so I kept adding 10ml at a time, until I had 40ml. (5mg/ml assuming)

So, either I am way off in my guestimates of extraction efficiency, or the WTA is Very synergistic.
- next batch, I will just add the 40ml of pg to the 25ml of oil all at once and simplify this step further.

Step 10... dripped my homemade WTA into a fresh atty and ... wow. Warning... going back to straight nic is going to be tough.

this whole process is just an age old "acid/ base extraction", but with the advantage of using the PG as the final solvent, one avoids ever having to concentrate nicotine to dangerous levels.
Nonetheless, there is NO recommendation on my part that anyone try this themselves. This is just a writeup of my own experiments and results.

Extra stuff...
Step 7, 9 and step '11', can be 'monitored' for accuracy by the use of Turmeric (curcamin), It will change from yellow to red at pH 7.5-8.5.

Step 11, if you so choose (I think it unnecessary) is to add baking soda to your WTA juice to neutralize it. Take 1/2 ml (10 drops) and add to a few ml of distilled water and turmeric.
Dilute some of the baking soda solution from step one 10:1 and add it drop by drop until it turns red. (one drop did it for me so maybe try 20:1) Then use that ratio to neutralize the PG/Glycerine. Or, if you like curry flavoured juice, add the Turmeric to the juice, and add the sodium carbonate until it turns red.

Play safe, and use common sense. :)
Click to expand...
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Comments

D
Has anyone tried this? After reading about WTAs it sounds interesting. I was always better in physics than chemistry. It seems logical - I vaguly rember doing acid/base extractions, but I also don't want to make something that is not safe.
 
Tgoode
kcos;bt3554 said:
sounds good BUT mineral oil ? I don't think it's safe to vape?
Click to expand...
This process results in pg containing WTa, and the final product doesn't contain oil. The basic water frees the alkaloids from the tobacco and makes them oil soluble. Putting the basic tobacco mash in the oil extracts the alkaloids and boils off the water. When you filter the oil, you get oil with alkaloids and no solids. Adding the tartaric acid to the pg makes it acidic. This, when mixed with the alkaloid oil causes the alkaloids to migrate into the acidified pg, and neutralizes the base. The pg and oil don't mix, so when they separate you siphon off the pg.
 
kinabaloo
WTA seems to be high in the 'other' alkaloids relative to nicotine (a different profile to that in smoke, and in my eyes, preferred). My extraction using a very similar method was around 4-5 mg and had little nicotine that I could notice, but a big effect in terms of a 'wave of calm' that becomes apparent after some minutes.
 
Lastlokean
It would be interesting to hear DVaps opinion on this... If it 'counts' as being WTA... Being as it is using a very basic A/B your resulting purity is obviously questionable. I do completely agree you have isolated tobacco alkaloids with this process. I only bring this up as my process that brings about the tobacco alkaloids in a currently unknown % has been shut down as not being WTA. Apparently anything other than 99% tobacco alkaloids cannot be WTA...?

I personally prefer a simple cold ethanol soak - filter - evaporate - dilute process... As it will also have impurities but comes with a nice tobacco flavor.

I know its all food grade but are there no concerns about trace mineral oil, cream of tartar, salt?, plant products as apposed to just doing a simple extraction and minimizing/living with the plant bi-products? :2c:
 
kinabaloo
Having thought more about it, DVap is welcome to the WTA term, as the creator of the aronym.

But I'm not interested in his opinion on this method as it is clear from years of silence that it would be considered 'competition' and slighted. No problem with commercial enterprise, just done fairly.

Oil and water absolutely don't mix, so if done with patience (separation) and care, there will not be any oil left in the final product.

Flavanoids are alkaloids too - it does have the tobacco flavors.

This method produces ATA (All Tobacco alkaloids). The efficiency is pretty good (potentially 90%+). The purity even better (99%+ only alkaloids).

If you're happy with cold ethanol, I've no real issue with that. I will try it someday to compare.

You call it a 'basic A/B' but that is misdirection. Basic in equipment, but a fully proper A/B !
 
Lastlokean
Your right DVap can have the term WTA. However, I would like the public to become aware of the fact that this 'WTA' is not the only way one may benefit from the synergistic minor alkaloids found within tobacco.

Actually oil and water do mix, it is just to a relatively negligible amount. Most vegetable oils hold 200 to 1000 ppm H2O, and H2O can hold a few ppm of most oils. This is one of the reasons it is necessary to recrystallize at the final steps of an A/B extraction.

I call a full proper A/B a little more thorough. Where this process stops is with PG with an unknown concentration of alkaloids, trace mineral oil, possible contaminants from mineral oil, Potassium bitartrate(cream of tartar),sodium bicarbonate, salts from the latter 2 neutralizing, other unknown contaminants.

Usually, from an o-chem standpoint, an acid/base process usually involves an initial extraction, wash, phase transfer, separation, phase transfer, wash, recrystallize. This being minimal and commonly going to quite further extent and/or involving distillation at some point.

This process is quite promising to me. It just might be in need of some tweaking. I have a few concerns. If your going to 'consume' something you should be pretty thorough about its contents in even trace quantities. I'm all for achieving a safe feasible at home / OTC method of creating high purity ATA.

#1 Vaping cream of tartar... and various salts, I have no idea if this is a good idea; most likely not.
To clarify, tartaric acid and cream of tartar are not quite the same thing, cream of tartar is made from tartaric acid. Cream of tartar is made by combining tartaric acid with potassium hydroxide. From what I am understanding of this process you definitely have this in your final product.

#2 impurities in food grade mineral oil. Have to to do some in depth research on the subject before I use anything other than pharmaceutical grade for consumption. You could easily be extracting/concentrating impurities in this process. If your gonna accept unknown petroleum impurities why not use a volatile(ether,hexane,mek,dcm,etc.) oil phase to collect and evaporate the base?

Mineral oil itself, is any of various colorless, odorless, light mixtures of alkanes in the C15 to C40 range from a non-vegetable (mineral) source, particularly a distillate of petroleum. Food grade mineral oil has an E number of E905a, although it is not approved in food products in the European Union, and incidental amounts in foods are carefully regulated. Basically the stuff is questionable.

#3 Unknown yield. Some people may be comfortable with assumptions, but in my opinion this is playing with fire. It is quite possible to have one tobacco be .6% and the next be 3.6%. Using a process with no quantification of yield is quite dangerous when the resulting product has an LD50 of 50 mg.

Solution #1: Switch to high grade d-limonene, linseed oil or the cleanest oil you can find instead of generic mineral oil. In either case I would strongly recommend the highest purity / grade one can get. All 3 of these things, along with vg/pg have 'grades' based on the level of contaminants. Being as we intend to regularly inhale this product, this is a serious concern, don't skimp on the grade of solvent used.

Solution #2: Extend the process using the same methodology.
Replace the PG in step 9, with just distilled water with cream of tartar added and separate:
10) Add baking soda to the collected water. Enough to neutralize.
11) Add oil to water. Separate, collect oil. Repeat.
12) Wash oil with dilute baking soda water. Repeat until water does not pull crap out.

Now you should have oil, of some type, with freebased alkaloids and minimal water soluble contaminants, hopefully free of baking soda.

13) Many Choices... Essentially ways to collect the goods.
a) Add acidic PG to the oil to collect the alkaloids for direct vaping. Would want to add the minimal acid needed. Still has the downside of leaving you with an unknown strength, but at this point it should be minimal in various salts and water soluble mineral oil contaminants. AND DVaps nicotine test will not work at this point as the alkaloids are in salt form.
b) Add acidic water, evaporate it down, preferably under vacuum. May lose some nicotine in evaporation without nicotine (need to do more research on this). Same as A) with the added benefit of being able to weight it. This can be done without 'directly' handling.
c) Precipitate acidic alkaloids from oil phase. Fumaric acid and acetone come to mind as a strong possibility. So you would add acetone saturated in fumaric acid. The acetone will be oil-soluble and turn the freebase alkaloids into salts that are acetone and oil insoluble crashing out. There is likely a more food-safe way to do this, however the resulting precipitate can be washed to remove trace acetone/fumaric acid)
d) If using a volatile oil phase simply evaporate it to collect the freebase. Preferably under vacuum.
e+) haven't thought of it yet... working on it. Hopefully food safe.

I prefer the tobacco absolute via cold ethanol because it is flavorful, simple, and safe. I have confidence regularly consuming the 2 ingredients involved: tobacco and ethanol. If I was going to go through more work on tobacco it would not involve petroleum contaminates. But really, with all the trouble an A/B extraction requires for isolation of tobacco alkaloids why not go all the way to a distillation process?

"The alkaloid is obtained from an aqueous extract of tobacco by distillation with slaked lime, the distillate being acidified, concentrated to a syrup and decomposed by potash. The free base is extracted by ether and fractionated in a current of hydrogen. It is a colorless oil, which boils at 247 C. (745 mm.), and when pure is almost odorless. It has a sharp burning taste, and is very poisonous. "

Obviously one could stop at extracting the free base alkaloids with ether, then stripping the solvent to recover the pure alkaloids as apposed to isolating the nicotine from the other alkaloids.

Edit:
Unfortunately I believe freebase nicotine and water form an azeotrope at 2.45% nicotine BP 99.988 C. I believe this implies one cannot evaporate a water-nicotine solution in atmosphere to achieve pure nicotine, as the nicotine will evaporate. Nornicotine, anabasine and other various alkaloids do not form this azeotrope. There is literature on how to isolate nicotine in such a manner. Fortunately at a vacuum of only 400mmHg and lower the azeotrope does not exist. Making it possible to vacuum concentrate nicotine. I am not sure to the extent this is impacting evaporating an ethanol solution. It may be removing the nicotine and leaving only the alkaloids that do not azeotrope with water. Notice in the above lab process, they acidify the distillate, then evaporate, then re-base, then extract with ether. This is because they know of this detail.

Also at some point of concentration, slightly beyond 5% aqueous nicotine solution, the solution will separate. One layer will form of ~80% nicotine and the other remaining at the saturation point around 5%. I have witnessed this personally in evaporating tobacco distillate under vacuum, as have I read of it within tobacco institute literature. If you do not notice this effect when evaporating aqueous nicotine solutions to dryness, its because your nicotine is going with the water in a 2.45% azeotrope.
 
kinabaloo
Quick reply; maybe more detailed later.

It is great that you are thinking of improvements - that's the whole point, although I think it is very good as is.

Re 'unknown concentration of alkaloids' - yes, tobaccos vary but one can look up the tobbacco one is using and be pretty sure of the maximum yield.

Re ppm organic solvents - mineral oil will certainly be better than vegetable oils (which I have also tried). I think that at this level we are in background noise levels - there are petrol fumes and all sorts of other contaminants in the air (especially in cities / the home, which are largely unavoidable. And further, this is at the end of the day an alternative to smoking - parts per million or pp hundred ?

Finally (for now), this was meant to be 1) an easy at home method, 2) avoid concentrated alkaloids (not a big danger if know the danger and sensible about it).
 

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