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DVap

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Having trouble buying this.... first, that nicotine hydrochloride would form, and second that nicotine hydrochloride which is highly soluble in water would become insoluble at fridge or freezer temperatures.

Having trouble with this one as well. Nic.HCl is hygroscopic after all.
 
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Yes, that's the exact paper I was thinking of. Thanks!
The same multi step process could also be done using oil, to maximize yield.

"a clear colorless liquid, b.p. = 110°-117°C/12 mm. The 21g (88%) of product was >99% pure by G.C. and turned pale yellow within 3 days at room temperature. [...] It was interesting to note that when the lye and the dark nicotine sulfate solution was mixed the color was black. Upon distillation the clear nicotine distilled and the sodium sulfate residue was left as white crystals. This suggests that it is not possible to determine the purity of these nicotine sulfate solutions based entirely upon the color of the mixture."
 

tescela

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It doesn't feel like the ecigs provide a "hit" to the brain the way that analogs did. I'm still sticking with ecigs - no analogs for over one and 1/2 years - but it still does seem like "something is missing". Maybe it is the beta carboline MAOs. I really don't know what I'm talking about, but I'm curious so I thought I'd ask what you guys think. Thanks. (is there a better place where this should be posted?)

Welcome, hgielm1! You have come to the right place. Congratulations on having the self-discipline to stay off of analogs despite recognizing that your needs are not being fully met by nic-only eliquid (while simultaneously recognizing that those your situation is not sustainable indefinitely, and going back to analogs is not an acceptable option). People like you are the reason the great people here are pursuing this issue relentlessly :)

It appears that my strong reaction to the simple snus water extraction liquid was due to the fact that I had already removed the MAOIs from my system and had no tolerance to them at all. Now that I've used this simple WT(A) for several weeks I no longer get this reaction.

I still get a sufficient "calming" effect but I can definitely tell now that I've built up a tolerance already. Key words here to me are 'sufficient' and 'tolerance' oh, and of course, 'simple' - this process is performed very quickly and gets the job done.

I vape less often still but now I am pretty sure I crave the wta rather than the nicotine. Going to drop the wta for a few days and see if I go insane with withdrawls.

At first glance, this struck me as the feedback scenario I feared. After reflecting on your words, though, it appears that you have made a point of emphasizing that your simple WTA eliquid is still calming you and satiating your desire for analogs, and that is the primary objective.

Please continue sharing the details of your experience as the days pass.

a 'designer vape' sounds fantastic, if you have the means and wherewithal to do it. Suggest an MAO-B like selegaline as a place to start that could make vaping a neuroprotective and nootropic tool as well.
Save yourself some time, and do a search on here to see what has already been attempted. Then be sure to let us know how things work out with that approach. :)

Seeing the relatively obscure term "nootropic" pop up in this thread has got my attention, and triggers a twinge of concern.

Perhaps tceight's comments should be interpreted as follows: we are not recommending that you try adding specific substances to your eliquid. If, however, you choose to do so, then please share the details of your experience. :)
 
On the slopes method (ethanoic acid / sodium chloride) :


Maybe this method will extract the harmalas but not many of the other alkaloids, as tceight and DVap suspect).

~~~

Later :

The rationale seems to be this :

"I think the driving force for this reaction (the converting to the HCl salt) is the fact that the HCl salt is insoluble. Thus it seems to "disappear" from the right side of the harmaline-acetic salt <--> harmaline-HCl salt equation. So even if the dfisplacement of the acetate by the Cl is not favorable, giving an equilibrium concentration favoring the acetate, as the HCl salt crashes out of solution, the equilibrium will try and be maintained, forcing more of the HCl salt to be formed"

It all depends on wether the alkaloid-HCl is indeed insouble at cold temps. And which ones.

~~~

While ~5% Rue is harmalas, in tobacco it is <0.01% (from memory). An amount too small to see perhaps. If there's more, and it's not table salt (NaCl), this could be interesting.

~~~

If this method works, and is WTA not just harmala alkaloids (and maybe a few others), then although there is a point of concentration, it is of a solid and need not be manipulated at all; once the liquid is drawn off, PG can be added. So while caution and respect must be stressed, it is not a no-go in my eyes.

If it works and is WTA, it is neat; less messy and no oil. And it should present only alkaloids in the crystals that salt out (so long as the NACl was not saturated).

If it works, then because of the way it works, the yield should be very good - no partitions, plus the insoluble salt one side of an equilibrium. I can see the idea well enough. But will it work out in practice ???

~~~

Need to sleep now, but slopes: if the cooling produced nothing, try this: just set it aside to slowly evaporate and just maybe the alkaloid-HCl will salt out first as the solution becomes ever more concentrated. Or rather than waiting for days, simmer it down by say 20% and then cool again.

~~~

The nic-HCl in a ptach is realeased only slowly. I know there are binders and such, but it is suggestive of nic_HCl being only slightly soluble, even at body temperature ...

~~~

A temperature controlled fractionalisation of a multi solute solution by different crystalisation potentials/likelihoods

~~~

The dissolved NACL will lower the freezing point of the water. By this temp, the alkaloid-HCl might be insoluble even though it is soluble at room temperature. The temperature therefore is a key in the method (adresses DVaps' point) and the unfavorability is mooted by the salting out (crystalisation/removal from solution) to answer tceight's point).

Can hardly wait to get the results !

So slopes - you might need to go lower than a fridge (~4-5C) to just below 0C
 
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slopes

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kinabaloo - "you might need to go lower than a fridge (~4-5C) to just below 0C"

I left it in the fridge overnight and nothing much seems to have happened (ie: the mixture shows little sign of any separation). However, yesterday I placed it in the freezer for a couple of hours where a sludge formed at the bottom of the glass container and what looked like ice lumps formed and floated on the surface.

I will return it to the freezer and rescue the sludge. I will reheat this with fresh distilled water and dissolve in more salt before returning it to the freezer once again.
 
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kinabaloo - "you might need to go lower than a fridge (~4-5C) to just below 0C"

I left it in the fridge overnight and nothing much seems to have happened (ie: the mixture shows little sign of any separation). However, yesterday I placed it in the freezer for a couple of hours where a sludge formed at the bottom of the glass container and what looked like ice lumps formed and floated on the surface.

I will return it to the freezer and rescue the sludge. I will reheat this with fresh distilled water and dissolve in more salt before returning it to the freezer once again.

Interesting. Keep me posted :)

~~~

any news ?
 
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I'm tentatively calling our experiments this weekend a success, but there is definitely room for improvement. I wish we had time to do another batch because all I ended up with was about 70-80ml of liquid from extracting 10g of tobacco. You guys are turning something like 20g into 20ml right?

My alkaloid solution looks somewhat right, a light golden color, and I am assuming that it is less concentrated. I just finally vaped some of it after getting home but I can't really tell if it worked or not. Before leaving this morning I put 12 drops into a bottle with ~3ml of a low nic ejuice (probably about 6mg when all was done). I took about 10-15 puffs around 12:45 and I started to feel a little foggy and tired, though I normally don't go to bed until 2AM or later. Just as I sat to write this at 1:30 the foggy relaxedness began to clear a little, and I had been vaping my normal ~20mg, non-WTA juice. After a few more puffs, I might be feeling the WTA effects, or I might just be getting sleepy from a busy day including travel.

Is this in line with others' experiences? I think I read that cigarettes have both stimulant and depressant effects, but I am not sure if the stimulant effects are solely from nicotine. I don't do other drugs and rarely even drink alcohol, but I do take 5-HTP regularly, so I don't know if that might mess with how the WTA affects me.

Anyhow, I had fun being in a real lab and taking part in making something. I really didn't do much besides wash beakers and try to find stopcocks that fit the sep funnels, but it was fun to watch. The only severely dangerous thing my brother used was NaOH and sodium carbonate should work just as well. At first we were way too conservative with the amount of tobacco and overdid the base, so it just obliterated everything. I don't think the base solution was very strong in the end though, so I ought to be able to replicate the procedure on my own. I think I will need a different acid though because all I own is malic acid from trying to make sour ejuice, and that seemed to make PG thick. I'm not sure about water though.

I wouldn't even consider doing this without a sep funnel, but more than that I can't imagine not having a vacuum filter. This stuff was nasty goop before it got washed out. I do have an almost-finished batch of oil that I will eventually try to work on. It seemed like it was almost completely separated, then overnight the emulsion/water layer increased to like 2mm thick. Now after all day in the trunk of my car it is about 5mm, so this definitely can take more than just a few hours to do.

Between borrowing a couple from my brother and the "free bookstore" nearby I came away with two organic books, one general intro chemistry, and one on techniques in organic chemistry with a lot of info regarding safety. I just got through the parts about Lewis and resonance structures, so a long way to go. Now it is 2:05 because I am a slow and easily distracted writer, and that little bit of fogginess I got again from the 2nd WTA session seems to have cleared and I am mostly wide awake. Guess it is time to hit the books more =)
 
I'm tentatively calling our experiments this weekend a success, but there is definitely room for improvement. I wish we had time to do another batch because all I ended up with was about 70-80ml of liquid from extracting 10g of tobacco. You guys are turning something like 20g into 20ml right?

Tobacco is say 2% alkaloids; call it 1% after extraction deficiencies. So 20g would give 200mg. so 10ml of 20mg/ml would be a good target for 20g of tobacco. So fr 10g you;d aim for 5ml rather than 70-80ml ;)

But thanks for getting back - nearly gave up on you !

Congrats though on getting your feet wet. Appreciate your commotment :)

~~~

Malic acid is too weak. And the hydroxide as the base could easily be overdone (to possibly harmful extent); carbonate is just perfect (even that is a bit more than necessary but seems to work very well, even at saturation).

@@@

So : your base maybe too strong (go with Na carbonate). and (most importantly) your acid was too weak.
And your end -product too weak = too dilute (if you gave correct figures)

~~~

one can't stress enough safety with chemcals, but the big issues are when you get in your car or cross the road. And need to lock up your e-liquids no matter it is only standard liquid from store"

~~~

to sum up, go with carbonate as the base -it is proven efective, and unlees you have 0.1M HCl, go with citric acid and afer neutralise with calcium hydroxide or Ca carbonate. Aim for about 0.5 x toabicci weight x ml (for ~20mg/ml alkaloids (max)).

10g tobacco : aim 5ml of 20mg/ml
20g : 10 ml of ~20mg/ml
50g : 25ml of 20mg/ml, etc

the actual strength is probbaly less than 20mg/ml but might be as high as that

~~~

for some people, what you made would be ok, if not maybe simme ir down in volume.
 
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slopes

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Progress repost on the Salt n' Vinegar method.

1) I heated 12.5g crushed rolling tobacco with 100ml white vinegar and a splash of distilled water

2) Simmered mixture and reduced to a mushy state

3) Pressed out all liquid from mushed mixture

4) Repeated steps 1 - 3 with the same tobacco

5) Heated the 60ml of brown juice obtained

6) Added 1 x teaspoon table salt and dissolved

7) Let liquid cool, placed in glass jar with lid and put in freezer

8) When a third to half of the mixture had formed mushy ice crystals at the base of the jar I quickly drained off the remaining liquid

9) I heated the mushy ice crystal part (now itself thawed to a liquid) with 40ml distilled water

10) Repeated steps 6 - 7.

I'm now at stage 8 again and a bit stuck. There is some residue in the bottom of my glass container (when the ice has melted) - but I don't know if it is silt, undissolved salt or what. Freezing/thawing/cooling/heating takes time.

Perhaps nothing separates out when frozen?

The ice crystals are notably clearer than the remaining liquids - which remain brown throughout. Perhaps it is the drained liquid that concentrates?
 
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tceight

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Perhaps tceight's comments should be interpreted as follows: we are not recommending that you try adding specific substances to your eliquid. If, however, you choose to do so, then please share the details of your experience. :)
while there was certainly a tongue planted firmly in cheek when I wrote this, my views on such things have been posted when we last discussed this approach.
In all seriousness, a 'designer vape' does sound like a perfect interim step the path of entelechy, the final place being needing/wanting nothing at all.
Let me be more precise, "if you have the means and wherewithal to do it." means a few hundred million, a lab, and a decade.
"Save yourself some time, and do a search on here to see what has already been attempted. Then be sure to let us know how things work out with that approach"
Selegaline, neuroprotective,nootropic are all good keywords to start searching for past discussions.
maybe not nootropic, I don't believe if i've read much on here about that. Probably another forum.

I don't believe it's that esoteric a word.
 
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tceight

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no lack of interest here, just time.
If I have something of value to add, I will make the time. Otherwise I am just wasting it, where it would be better spent actually doing extractions/experiments.

I've a process that works well for me pretty much as I posted. At this point I am just looking at optimizing it and to do so requires true experimentation. For that, I need better gear.... microgram scale, pipettes, etc. rather than eyeballing and guessing how well things work.
I can't expect DVAP to do all the hard math. :)

path forward is
1. How much IS in the tobacco to begin with and available to the mineral oil.

2. the minimum amount of bicarb solution to ensure maximal transfer without dilution.

3. extraction to oil, what method has best balance between ease and efficiency. (1. single oil soak. 2. multiple oil soak. 3. oil soak and press, 4. interface method, 5.something else.)

4. partition coefficient of mineral oil and acidic water, at achievable pH ranges in the kitchen.
5. partition coefficient of mineral oil and basic water,------ Done, DVAP gave us the minimum of 4.

6. with the above information, create an optimized writeup of 'DIY' to create a standardized solution at a given strength.

7. what strength is acceptable. We bandy about the 'maximum' we can get, looking at 20mg/ml. In reality, guestimating the strength of my past conconctions, I was vaping 5-7 mg/ml, and that is lots for the 'missing component'. Later extractions I am guessing them to be about 15mg/ml and I cut it 50% with 30mg/ml nicotine only juice. That is 'one' person.

DVAP's pure WTA trials where running much higher concentrations. Also his is a lot cleaner. Possible some other minor component that is not removed in the kitchen method adds synergy, or maybe I am just more sensitive to the effects.

With enough users of a standardized extract then we can determine if a stronger or weaker end product is needed.
1. if weaker, then further optimization is possible with more dilutant in the process.
2. if stronger, then loss of efficiency is required for performance.
3. if all over the map, then 3 versions can be created.
A). max efficiency 'lite' version.
B). standard
C). high octane.
 
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DVap

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Plus, I'm getting tired of hard math! Pretty much in discomfort lately, and if the surgeon saws on my neck, I'll be in no mood to do math at all for awhile, be it figuring 2^n for n = 0 to 8 or anything harder.

With oil -vs- basic water, we know the oil works and should work -vs- the solid matrix as well. So that's a point to hang hat upon. The idea of investigating optimizing the extraction for solid to oil is a good way to go. Often such steps are done in duplicate or even triplicate. Assuming a minimally effective coefficient of 4, using 3 serial extractions would give us (theoretically, but probably not really in practice.. but close enough):

Extraction #1 80/20 (and from the remaining 20)...
Extraction #2 16/4 (and from the remaining 4)...
Extraction #3 4/1

Or 99%.

I'd stop after 1 for simplicity, or after 2 for recovery. 3 just makes more work for diminishing return.

I'd be more confident of the partitioning in liquid/liquid systems. Liquid/solid can be unpredictable!
 
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