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slopes

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tceight - good to hear you are still on the case. I wish this thread was more active. I'm planning to buy some D-Limonine to replace the olive oil in the organic stages. I think that would sneak through as 'kitchen' (food safe) - do you think it would be more effective to use?

Some other experiments over the months:
1) THE SUPER DIRTY METHOD.
I ran two 8mm pipes through a stopper into a test tube to create a rudimentary hookah. The longer pipe ran to the base of the tube and its end was constricted to a 2mm aperture. The shorter pipe ended just inside the tube. The tube was one quarter filled with a distilled water/glycerine mix. I attached a super kingsized cigarette to the end of the long pipe and my vacuum cleaner hose to the end of the short pipe. I lit the cigarette and the vacuum cleaner sucked its smoke content through the bubbling water/glycerine mix (time: around 1 minute). I repeated this with 10 cigarettes. I vaped the yellowy-brown juice. Perhaps unsurprisingly, it had the taste of 'condensed ashtray'. But it had a kick and felt like smoking a cigarette. I guess the juice contained pretty much everything a cigarette would - including all the 'crap'.

2) THE BACKYARD SUPERCRITICAL METHOD
I mixed 25g dampened tobacco with a sprinkling of sodium carbonate. When dry, I placed this into a small stainless steel pot. Loosely covering the top, I squirted in the entire contents of an aerosol can of pipe freezing liquid (used for DIY plumbing). This liquid is pure 1,1,1,2-Tetrafluoroethane - a refrigerant which is also used for the extraction of fragrant oils and flavours (and is claimed to be non-toxic). It has a very low boiling point. I stirred and tamped the mixture for several minutes whilst it boiled (and ice formed on the outside of the vessel). I then tipped the liquid through a filter into a test tube. After 15 minutes the tetrafluoroethane had boiled off completely, leaving a puddle of pale yellowy pink liquid in the base of the test tube.

EDIT: The next batch of this I will try without the sodium carbonate - as I don't think it needs it. I think it is the residue of this power which keeps the end result from being crystal clear. It would speed up the prep and distillation time too - total time (excluding 15 the min boil-off): 5 minutes.

3) THE KITCHEN CRYSTAL METHOD
I boiled up 25g ground tobacco with 2 tsp of sodium carbonate and 250 ml distilled water. I filtered off the tobacco and reduced the remaining liquid down to a stiff brown paste (ie almost dry). I placed an quantity of this material into the base of a test tube (ie filling about 20mm). I heated the bottom end of the test tube (directly over the material) on an open flame. Condensation formed in the upper part of the tube and I wiped this away several times with a rolled up tissue. The theory being that pure nicotine crystals would eventually form on the glass - which could then be scraped off and collected. I chickened out before reaching this point... believing that any powdery plant material left in the mixture might spontaneously combust as it heated and dried.

4) THE CO2 SUPERCRITICAL IDEA
I would buy a small, 3.5oz, refillable CO2 canister of the type used by paintball enthusiasts. I would remove the nozzle and suspend inside the canister a large, sealed 'teabag' of tobacco. With the nozzle bolted firmly back on, I would fill (or partially fill) the canister from a second - larger - source of CO2 (I have in mind a canister supplied for soda syphons or simply a larger paintball canister). After shaking about for several hours, I would release the CO2 into the air, unbolt the nozzle from the small canister, remove the 'teabag' and retrieve whatever pure WTA liquid had collected in the base of the canister.
 
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tescela

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interesting note... I've made some incredibly 'pure' stuff... and even when cut down to 24mg/ml, it has a throat kick like hotsauce and wasabi...but... for some reason it's less satisfying than many of the quick and dirty far less pure batches I've made. I'm wondering now if the alkaloids are the whole answer. There are hundreds of other active molecules in there too, that are not alkaloids.

This is an intriguing comment, tceight. Has anyone else observed this difference in effect (with all other major variables held constant)?
 

BCB

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interesting note... I've made some incredibly 'pure' stuff... and even when cut down to 24mg/ml, it has a throat kick like hotsauce and wasabi...but... for some reason it's less satisfying than many of the quick and dirty far less pure batches I've made. I'm wondering now if the alkaloids are the whole answer. There are hundreds of other active molecules in there too, that are not alkaloids. :p

I got to try some pure stuff from DVap and was able to compare it to my usual snus/e-liquid combo and regular analog cigarettes for effect. (I had been smoking a little bit). My opinion is that WTA is a huge improvement over regular e-liquid. The taste with no additives is delicious and it is more calming than the nic-only stuff. However, I found analogs to provide a better effect than any of the other options. For this reason, I'd venture to guess that the "dirty" stuff is closer to whatever I want that the "clean" stuff is. Just one person's opinion.
 

Sweeper

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Well I took the plunge last night, and I gotta say, you learn by doing!

I went the "hot oil filtering through tobacco" route, and I now know why that's not a current method :) after 24 hours, I still had recovered less than 5ml of the 40ml of oil used. Sooo I got a garlic press and one of those wire mesh coffee baskets, cut the wire mesh, put it into the garlic press, and proceeded to (very messily) extract the rest of the oil, and then filter it. After shaking & separating the PG a few times, I ended up with 10ml of pale yellow liquid that has very little flavor, but is almost clear. I added 2ml of VG and half a ML of coconut, and vaped away. The result is not bad, but the wta I got from vapealicious was definitely more potent.

One significant variation on the hot oil method I used was a double boiler to heat the tobacco. I actually stewed the tobacco in the double boiler in oil for like 20 minutes. my primary complaint is that it's so time-intensive a process, but after re-reading the last few pages of this thread I think I'll try again soon!

Are there any downsides to using mineral oil vs olive oil? olive oil seems like it has so much more "stuff" in it....
 

Bagazo

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I went the "hot oil filtering through tobacco" route, and I now know why that's not a current method :) after 24 hours, I still had recovered less than 5ml of the 40ml of oil used.

I actually posted about a water extract method in this thread. It is an extra step but I think it works well to get rid of the bulk of the unwanted material. It involves soaking the tobacco in acidic water so that the alkaloids bind to the acid and form salts that are water soluble. Filtering the water out is easy. From that point on you just use the regular acid/base procedure.
 

Sweeper

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I actually posted about a water extract method in this thread. It is an extra step but I think it works well to get rid of the bulk of the unwanted material. It involves soaking the tobacco in acidic water so that the alkaloids bind to the acid and form salts that are water soluble. Filtering the water out is easy. From that point on you just use the regular acid/base procedure.

Yea, that's what I was referring to :)

Ok, so here's what I did today:

20g "good stuff red" pipe tobacco, ground up

boiled with 250ml of distilled water, and 2 tsp baking soda. I screwed up here, it was supposed to be calcium carbonate, but I forgot until it was already added. I immediately stuck 200g of baking soda in the oven to bake while I went on, for the future :)

Decided to see what would happen regardless, since I had already put in the most expensive ingredient (tobacco, purchased for $12/lb on the indian reservation)

I boiled for 5 minutes, then used the remaining part of the aforementioned metal coffee strainer to strain out the ..... The tobacco mush was much lighter in color, and the water very dark. I used a spoon to press the mush and get as much water as possible out.

Next, I tried an additional filtration step. This went badly. I initially used a glass cup with a coffee filter rubber-banded to the top. This filtered about 5 ml, and then STOPPED. Filtration rate went from a steady stream to 1 drop per 30 seconds. Needless to say, 250ml at this rate was going to take forever. I tried using the turkey baster method, same results. Somehow the micro-particles that got through the metal strainer are VERY effective in clogging the filter. Since these particles probably wouldn't make it into the mineral oil, I decided to scratch that step.

I had initially recovered 160ml of tobacco/baking soda water, but my failed attempts at filtration lost me about 10ml all in all, so I had 150ml of tobacco water left. I poured this into a wash bottle, and added 30ml of USP light mineral oil. After about 6 hours of occasional shake/separation, I isolated the oil. This was...interesting. I need to grind down some needle tips to make it easier, or get a separatory funnel. I drew off as much as possible of pure oil from my rather wide wash bottle and put it into my graduated cylinder, and then sucked up a bunch of oil/water mix from the top layer, and put this mixed stuff into several test tubes. since the test tubes were much narrower than my shake bottle, I was able to recover about 10ml more oil, resulting in a total recovery of 27.5ml pure oil. If I can find a good way to put a stopcock on the turkey baster, that might be a VERY good replacement for a separatory funnel, since it's narrow and I'll be able to see the separation of phases easily.

right now I'm going to let this "pure" oil sit for a while and see if any more water separates out. There's maybe a drop in the very bottom of the graduated cylinder, so I want to be very sure everything is completely separated. The mineral oil is a yellow cloudy liquid, kinda like pus, so something came out of the tobacco despite using baking soda instead of calcium carbonate. I think adding calcium carbonate to water probably does the same thing as baking soda in terms of making it basic, but less so because the extra water hasn't been baked off? Or oxidation or something. been a while since AP chem :)

Plan for tomorrow is to take a 70/30 PG/VG mix (my preferred vaping mix) and acidify it. Not quite sure how much I should acidify it, but I've got white vinegar, and I want there to be a perceptible change on the ph strips, so I can tell if the PG/VG goes basic. I'll just have to play with it a bit until I'm confident I'll be able to see the change after the second step of the extraction. Last time, I used 5 drops for 20ml of pure PG (I think, hadn't started taking notes), and there was definitely *something* extracted, so I'll start there.

Assuming 200mg of alkaloids in the whole tobacco, I recovered 60% of the water. I highly doubt much of this actually boiled off, I'm going to assume it was lost in the remaining expanded mush, giving me 120mg of alkaloids in my mineral oil (assuming 100% transfer). I recovered 27.5ml of the oil, netting me 110mg of alkaloids. I'm going to do 2 5ml "washes" of acidified PG/VG, and measure the PH of each wash to determine how much alkaloids I'm getting. If I had some Bromothymol Blue, I could accurately calculate the ph, but for now it'll have to be ph strips. There's probably crazy math I could do with molarity and ph as well to get a good read on final alkaloid levels... but that will have to wait until a) I get some blue b) my wife settles down enough to let me brew a bigger batch...
 

Bagazo

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Sweeper, baking soda is alkaline and would make the extraction less effecient. What you want is to make the water acidic by adding some acid (citric, malic or even hydrochloric). Lemon juice or vinegar would work.

Theres no need to boil and actually this may actually be destroying the nic. I have read that freebase nicotine degrades at around 70ºC. Freebase nic is what you are getting when you add an alkaline to the tobacco.

You need to go back and forth between water and oil at least a couple of times. So:

Step 1 - water extract with acid (Nic and acid form salt that is soluble in water)

Step 2 - raise pH of water with alkaline and add oil (Nic becomes freebase that is soluble in oil so moves from water to oil)

Step 3 - lower ph of oil with acid and add water (Nic again forms salts that are soluble in water so it moves from the oil to the water)

Step 4 - take water and reduce and add PG/VG/Flavors
 

Sweeper

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ok, log for today (yay weekends):

Baking soda extraction is pretty much on standby until the PG/VG separates further from the oil. basically there are bubbles of PG/VG laced with detritus that are taking forever to "pop" and settle. We'll see tomorrow. I made a ghetto test tube stand by taking two snus cans, gluing them together, and drilling holes all the way through, holds 5 test tubes just fine.

Meantime, I started a larger batch, since I'm losing a few ml each time I transfer, so I'd rather lose a lower percentage of the batch. Losing 2ml when your final product is going to be 10ml is a lot worse than when your final product is going to be 50 ml :)

On that subject, I took a valve from my set of spares for low-pressure irrigation, and used plumber's epoxy putty to attach it to the end of my 2oz turkey baster, resulting in a passable separatory funnel. The putty is the same I use for juicebox mods, supposedly good for potable water piping. I *hope* nothing bad happens to it...we'll see. The valve's end fills most of the end of the baster, so there's not much putty in contact with the liquid....hopefully that will cut down on transfer and separation losses. Need to fabricate some sort of stand for it, but that can wait till tomorrow.

So, this bigger batch. 50g of ground tobacco, 500ml distilled water, 25ml of 5% acetic acid (i.e. vinegar). It'll steep overnight, and then I'll filter out the mush tomorrow. What kind of maths should I be doing to calculate the amount of acid to be using? Probably something to do with the amount of freebase nicotine present in the tobacco? Any benefits to using HCl instead of acetic acid?
 
No time to check into this thoroughly, but intriguingly DeKang says its e-liquid is direct from tobacco and is 'the only natural e-liquid'.

Could it really be the WTA we've been hoping for? Is this a new thing/line for DeKang (the oldest e-liquid manufacturer afaik) ?

If anyone has time to ask them about alkaloids in their liquids that would be very interesting.

"Unlike many players in this industry, Dekang has never use any chemical combination to create the “tobacco essence”, inhaling Dekang, means you are inhaling just real tobacco."

Company Profile - Dekang Biotechnoly Co., Ltd
 

Rocketfish

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Been following this with interest. Has anyone looked at TastyVapor's tobacco liquid as a potential source instead of dekang?

IIRC it's made by soaking good tobacco over a long period of time, and I'm sure Geoff is willing to share more information on the process than Dekang would be.
I don't know if the soaking method used would likely have the alkaloids present as well, and I haven't vaped it straight for any length of time to notice.

Though I don't want to win a dead thread, I too am wondering about the passionflower extract as an interim solution:

Kinabaloo you recommend against it, and other people find it effective. I'm not sure what to decide, I do know I feel that I'm missing the calming effect from smoking, and wondering if adding a little bit would be safe/effective.
 
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Been following this with interest. Has anyone looked at TastyVapor's tobacco liquid as a potential source instead of dekang?

IIRC it's made by soaking good tobacco over a long period of time, and I'm sure Geoff is willing to share more information on the process than Dekang would be.
I don't know if the soaking method used would likely have the alkaloids present as well, and I haven't vaped it straight for any length of time to notice.

Though I don't want to win a dead thread, I too am wondering about the passionflower extract as an interim solution:

Kinabaloo you recommend against it, and other people find it effective. I'm not sure what to decide, I do know I feel that I'm missing the calming effect from smoking, and wondering if adding a little bit would be safe/effective.

Huh !?

I don't think that I ever de=recommended it; but it is not ideal. One has to post with caution; yet there is reason for that caution.

-----------

Liberty, not facism; Ron Paul 2012.
 

nopatch

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I will try this method with sulfuric acid and lime for the last step.Obtaining alkaloids in water in the final step is quite useful for DIY;Not for amateur chemists, though.

I have just made another batch of WTA liquid, using an adaptation of this method. Done well - and with patience - it certainly works and provides a juice that reaches parts other juices can't (with apologies to Carlsberg).

Firstly I invested in a very cheap booklet of Ph level papers. This has been a huge help in getting the various stages right.

PREPARE
1) I boiled up 25g of ground rolling tobacco in about 250ml of water and 2 teaspoons of sodium carbonate. After 10 minutes simmering, I cooled the mix and filtered it through some cotton cloth. This was easy as the mix was creamy in consistency.

2) I returned the filtered liquid to the pan and reduced it further... till it began to stiffen. I diluted this a bit with fresh water and - using a Ph paper - made sure it tested blue (alkaline) before pouring the mix (about 25ml) in a glass jar.

SEPARATE
3) To the water solution I added a similar amount of olive oil. I shook it and let separate three times over an 8 hour period.

3) I syringed off the oil into a clean bottle and added more oil to the old water solution - shaking and separating it twice over an hour. I then syringed off this oil adding it to the first lot. I discarded the water solution.

4) I took some fresh (ie distilled) water mixed with a few drops of white vinegar to about 20ml and tested to ensure its acidity (paper turns red). I then added this to the oil and shook.

5) After several shakings over 3 hours, I drew off the water solution with the syringe. I placed 10ml more of the water/vinegar solution into the old oil and repeated the process - adding the (now, lighter-coloured) water to the first amount. I discarded the old oil.

6) I then tested the water solution with a Ph paper and it showed a reduced acidity. I added a couple of small pinches of sodium carbonate to the water until it tested blue (alkaline) before mixing in with an equal amount of fresh olive oil and repeated the shaking/settling routine over a few hours. I drew off the oil into a clean bottle. I placed about 10ml of fresh oil into the old water solution and repeated the shake/separate routine several times before drawing off this oil and adding it to the first amount. I discarded the old water solution.

7) I repeated steps 4 to 5. I ended up with about 12 ml of light, strawberry blonde water solution. It wasn't crystal clear... but not far off!

REDUCE
8) I tested the solution with a Ph paper and added a few grains of sodium carbonate to equalise it. I placed the solution into a small stainless steel pot (a tiny milk jug) and reduced it down over a flame to about 3 - 4ml. By this stage I was wearing rubber gloves! I bottled this.

I added about four drops to about 7ml of 24mg commercial juice and vaped. I can feel it works very well. The effect is completely different to the commercial juice alone.

This may sound complicated, but it's not. I'm trying to work out a simple way of remembering the routines - like a short rhyme or something.
 
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