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idea for obtaining freebase..

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endlessness

endlessness

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So I was thinking about this last night.. Lets say one has some mimosa alkaloid-rich limonene pulls.. and one's goal is freebase dmt/jimjam spice, also in a non-toxic way (or not very toxic at least :p ) ..

What people been doing is going through the step of salting out limo either with some acqueous acid solution (vinegar or fasw), and evapping that (which takes energy and time), or with FASI, which has the little disadvantage of later having a mixed limo+IPA, and this IPA will need to be evapped first to reuse the limo. and then to get freebase people make paste with sodium carbonate and pull with IPA or acetone.

So what I thought is.. what if one salts out using some slightly acidic solution, and theeeeeen... (drumrolls)... base the hell out of this solution with sodium carbonate, supersaturating the whole thing, no worries if theres undissolved sodium carbonate.. Then one would mix this with dry IPA, which, because of the sodium carbonate, would rise to the top, picking up all of the freebase alks and leaving the bottom layer of water and sodium carbonate.. then just separate and evap.

how does that sound? viable, problematic, intelligent, stupid, interesting, unnecessary, great, weird or..... ? :D

any possible issues there you guys see?

SWIM wont be able to test this for a while but maybe in a couple of months when he hopefully gets some time again
 
Sounds a hell of a lot better than using naphtha and would probably be a good way for new extractors to jump right into it, but SWIM doesn't like IPA and can't quit his love affair with fumaric acid. Plus, IPA really isn't incredibly nontoxic.
 
yeah fumaric acid is very nice to play around with... I was thinking not necesarily to substitute it, but lets say one wants part of his stash as freebase and the other part as fumarate.. with some of this he could then do the normal salting a-la FASI FASW and crew.. Then this person could make this proposed IPA separation on the other part of the limo, and get his freebase-full IPA ready to infuse some changa or whatever, without having to dry the fumarate, then base and paste, then pull...

as for the IPA not being incredibly non-toxic, yeah thats true, and why I made the consideration in the beginning.. But it is generally quite safe and evaporates very fast leaving no residue (and SWIM has USP grade IPA).. But in any case, doesnt this sodium carbonate separation work with ethanol also? I sort of remember that it could but im not sure... what about acetone?

and something else important to know: the solubility of the sodium salts formed when basing the lightly acidic solution (so sodium acetate or sodium fumarate or whatever depending on which acid is used), in IPA (or acetone/ethanol in case it works)... If they are soluble then it would be a contaminant in final product.. otherwise would be clean
 
I agree, Fum salts are lovely. The only problem is they don't vaporise.

Endlessness: I have some limonene which I allready precipped from with a bit of fumaric acid saturted IPA. Then I washed the limo with water to remove other fumaric acid.

If you describe your technique again breifly and in a straightforward way, I will preform it and take pics so you can see the results. I don't have any sodium carbonate, so if you
can ajust for NaOH that'd be great. But if not, I can make some from bicarbonate.
 
Gee us a hand with this one lobsterman, How much NaOH to a gram of dimethyltryptamine fumarate? The molar ratio is 1:1 but obviously you will want excess. It is stable at ph13 as we all extract freebase like that, but in a concentrated solution couldn't too much NaOH react with the DMT itself?
 
endlessness said:
yeah fumaric acid is very nice to play around with... I was thinking not necesarily to substitute it, but lets say one wants part of his stash as freebase and the other part as fumarate.. with some of this he could then do the normal salting a-la FASI FASW and crew.. Then this person could make this proposed IPA separation on the other part of the limo, and get his freebase-full IPA ready to infuse some changa or whatever, without having to dry the fumarate, then base and paste, then pull...
Click to expand...

Oh certainly, it's probably a great alternative in that it yields a full-spectrum smokable product more immediately, though SWIM's not so certain that IPA evaps much cleaner than, say, heptane (which won't achieve full-spectrum anyway) or acetone when evaporating to crystallize or otherwise precipitate. However, acetone wouldn't work in the same way as IPA for a process like this to answer the next paragraph's question, as he believes that it wouldn't separate as well, if at all, hence the typical use of drytek procedures.

To briefly explain SWIM's assessment of IPA: SWIM's method of manual crystallization seems to work well to remove heptane, acetone, and/or water to yield a very solid and dry product, but when IPA was attempted, it never seemed to dry completely and remained quite malleable. IPA doesn't seem to evaporate as fast as acetone or heptane, and SWIM's technique requires that a solvent be able to almost immediately evaporate upon surface area exposure, which acetone and heptane seem a bit more capable of. Water works well because freebase spice isn't incredibly soluble in water, so SWIM's procedure simply forces it out (the same could likely be said of heptane), but freebase is quite soluble in IPA, so the product remains quite saturated with the solvent.

IPA is cheap, pure, and usually ready at hand, but SWIM now only uses it to clean smoking devices as an alternative to acetone, since he already has it for disinfecting purposes. The only solvents that ever touch SWIM's spice anymore are limonene and water, and the only reagents are vinegar (to a very small degree, as pretreatment), lime, fumaric acid, and sodium carbonate. Admittedly, if SWIM didn't have a food dehydrator, evaporating water for FASW would be a pain, but he can do it to obtain fairly massive quantities of fumarate in one shot and do with the fumarate what he will. He no longer has to spend any time evaporating anything to achieve freebase, so no more solvent fumes whatsoever.

All of SWIM's discrepancies aside, your method is probably ideal for changa, and SWIM would like to see how it turns out.

and something else important to know: the solubility of the sodium salts formed when basing the lightly acidic solution (so sodium acetate or sodium fumarate or whatever depending on which acid is used), in IPA (or acetone/ethanol in case it works)... If they are soluble then it would be a contaminant in final product.. otherwise would be clean
Click to expand...

SWIM doesn't believe sodium fumarate to be very soluble, if at all, in anhydrous IPA. He can't say about sodium acetate, though he believes syzygypsy's limonene tek used a similar process and had no complaints in that regard. In any case, it's probably much more soluble in water and would likely only be present in trace amounts, at most.
 
I hope one of you clever fellows invents a process for getting full spectrum (Jimjam?) freebase directly from the saturated d-limo. I've been trying to come up with one, but I am still such an amateur....

Pokey
 
Phlux- said:
pokey - perhaps evap and wash with water ? (not the most stylish way to do things tho)
Click to expand...

you can evaporate limonene? no way what an expensive waste! (and stinky)
 
I think I've read that D-limo doesn't evap well. That's why the DMT gets salted out with fumaric acid. There must be another way to get the freebase out of there though...

Pokey
 
well yeah this was the exact point of the proposed method in this thread, and it just might work, cant know until its tried.

otherwise one can just salt it out (with fumaric acid solution or vinegar for example), evap the water and freebase the dmt salt by making paste with sodium carbonate, drying and then pulling with IPA. But you know this already I guess...

to get freebase directly from limo, well, its tricky because freebase dmt/fullrange is very soluble in limonene.. there might be some other trick, who knows, but otherwise its easy enough to migrate it out of limonene by salting and then finding the best way to retrieve it without the salt evaporation. I proposed this method here.. there is another method which amor fati had told me it worked, but SWIM tried and he couldnt get it right: to simply base the dmt-containing solution (which has been salted from the limonene), and let it stand in the fridge for few days and then the dmt should precipitate and one can retrieve by simple filtration. But when SWIM tried, after days and days there, nothing really precipitated (and there was definitely dmt there).. So I dont know whats up with that.. Fati are you there to explain?
 
endlessness said:
there is another method which amor fati had told me it worked, but SWIM tried and he couldnt get it right: to simply base the dmt-containing solution (which has been salted from the limonene), and let it stand in the fridge for few days and then the dmt should precipitate and one can retrieve by simple filtration. But when SWIM tried, after days and days there, nothing really precipitated (and there was definitely dmt there).. So I dont know whats up with that.. Fati are you there to explain?
Click to expand...

? No idea.

The method SWIM uses requires that the salt be dried (water evaped) first, then it only takes an hour to obtain hard, dry, smokable freebase: Amor fati's Approach to Freebase Spice Conversion - DMT-Nexus Wiki

SWIM also hates filtering anything at all and only ever uses THP to filter out undesirables to retrieve desirables in solution. 69ron has proposed a method of removing excess fumaric acid from spice-containing FASW by putting it in the freezer, but SWIM's never tried it. When rextallizing fumarate, leaving a partially evaped solution in the fridge for a time help it to form larger crystals. That's all SWIM can think of that you may be thinking of.

Although, the first time SWIM basified fumarates, he did it STB in a solution of sodium carbonate using naphtha to pull. The mixture had been in cold conditions for a time, and a red oil was floating atop the aqueous layer, below the naphtha layer. SWIM retrieved this and bioassayed and determined it was likely jungle spice, though he had later been told that FASA retrieved spice was mostly pure DMT (the presence of JS could have been due to the use of non-lab-grade toluene or xylene). That was some time ago, and he never repeated and simply performed drytek conversions from there on out until he developed a nontoxic technique.

Perhaps your thinking of someone else, though.
 
hmmm I really thought it was you but i guess my memory is not the most reliable, sorry about that.. :)

but yeah unless something new comes up, so far it seems drying the salt is necessary, either evapping acqueous solution or doing the FASI to precipitate it...

I will try this other IPA sodium carbonate separation, though, see if it works.. will take a few weeks before I can do anything I think but I will make some tests when I do have time
 
I will be at a good point in my current extraction to try your idea endlessness. Could you be more specific about the slightly acidic solution. I'm happy to experiment, but I'm a real chemistry novice still. and don't want to screw it up!:oops:

The dry IPA will pull all the alkaloids? I've only used IPA with fumaric acid to salt out my BLAB. Would acetone work? I have acetone and have worked with it quite a bit.

Please advise.

Pokey the Excited:d
 
Acetone probably won't separate the way IPA does, and IPA will likely have some amount of water, salts and bas even when it does separate--these wouldn't be too difficult to clean out with water after evaping though (not to mention it would likely clean out potential trace IPA contamination as well).
 
Pokey said:
I will be at a good point in my current extraction to try your idea endlessness. Could you be more specific about the slightly acidic solution. I'm happy to experiment, but I'm a real chemistry novice still. and don't want to screw it up!:oops:

The dry IPA will pull all the alkaloids? I've only used IPA with fumaric acid to salt out my BLAB. Would acetone work? I have acetone and have worked with it quite a bit.

Please advise.

Pokey the Excited:d
Click to expand...


the slightly acidic solution is basically to turn the dmt in the limonene into a salt that is not soluble in the limonene anymore. When I say slightly, its because you dont need it to be very acid, in fact, being very acid would be a waste because later you will add a base again, and the more acid you have used, the more base you will have to use afterwards... So, which acid do you have? I mean, if it was vinegar, I would just add a little splash to water.. So lets say its a 100ml limonene pull, I would make a 30ml water-vinegar solution where maybe half is vinegar or smt, and do 3x acidified water pulls per limonene pull (and then reuse the limonene). If it was using fumaric acid, would be more or less the same, except it would be making a solution with 30ml water and throw a little bit of fumaric acid inside and mix (and filter/decant away from any undissolved fumaric acid that stays on the bottom), and then use this fumaric acidified water to pull on the limonene

is the rest of the proceedure clear?
 
Sorry, was away for the weekend.

I have vinegar or fumaric acid. I'll try the vinegar. The rest of the process is clear, and I'll start working on it tomorrow!

Thanks for all your help.

Pokey
 
Endlessness...funny you should post this I have posted a question regarding similar thoughts..I left it up because I'm way back at the beginning of the salting...and wondering if
you have say an aqueous solution of alkaloids, and then you begin to pull the limonene...can one hypothetically , stop there? and evap that to achieve collecting salts present? I'm wondering if you do this are you getting perfectly good ready to use base salts?

:? :arrow: :?:
 
So here is my report so far:

BLAB with 500 grams of MHRB gave me 500ml of saturated D-limonene

Mixed 300 ml of water with 300ml of vinegar (ph 2.4, will use way less vinegar next time!)

Did two "pulls" of 300 ml each- I use quotes because it didn't seem like these were pulls in the normal sense, much more like washes with acidic soultion "washing" the DMT out of the D-limonene. Adding half the volume and shaking like hell 4 or 5 times, then seperating just didn't feel like pulling....

While I waited for the solutions to seperate (9-10 times), I did some experimenting with sodium carbonate and acidic solution. I checked the ph of my saturated solution; it was 3.4. So the alkaloids raised the ph from 2.4 to 3.4. Never would have predicted that! I made a batch of vinegar/water solution with a ph of 3.4. This is when I realized I used way too much vinegar in my solution:oops: . I took my 50/50 solution and added 300 ml of water and the ph was still 2.4... Oops! After diluting the solution with water by pouring out half and adding water again 5 or 6 times I finally got the ph to 3. Wow. A little vinegar goes a long way!

Once I finally had 300 ml of ph 3.4 solution I added 3 g of sodium carbonate (trying to decide if it was worth it to reduce the 600 ml of solution I was working with before adding sodium carbonate) and got a ph of 9.6. Added 2 more grams and the ph came up to 9.8. Again, not what I would have predicted. An additional 3 grams brought the ph to 10.

I figured that was enough experimenting with ph. If 8 grams brought 300 ml of 3.4 ph solution to 10, then logically 25 grams added to my 600 ml would be sufficient to raise the ph and freebase the DMT.

Well.... Anyone ever mix vinegar and baking soda -AKA sodium bi-carbonate? It's an exciting chemical reaction that produces fizzing, frothing, and in a closed container is explosive. The reaction when mixing ph 3.4 solution with sodium carbonate is very similar:shock: :shock: . Luckily I didn't mix too vigorously, and had another jar to catch the stuff that did overflow. I recommend adding the sodium carbonate very slowly! Why this didn't occur to me before I made an erupting volcano in my mason jar we may never know...

So after everthing settled and i mixed well, I had a ph of 8.1. No idea why it wasn't higher (also don't know why I didn't get a reaction when experimenting with the sodium carbonate earlier). I added 20 more grams of sodium carbonate and the ph is now 8.8. The solution looks very much like milk.

So the first question: Is 8.8 high enough? I had to buy 5 lbs of sodium carbonate when I was gathering supplies, so I am not against adding more!

Second question: What's up with the ph going up when the solution is saturated with DMT, but then taking so much more sodium carbonate to hit only 8.8?

Third question: Why didn't I anticipate the volcano effect when mixing a vinegar solution with sodium carbonate? C'mon, that was my favorite experiment, well really the only experiment I found any merit in when I did chemistry in school....

So that's where things are now. I would appreciate advice about raising the ph further, and also a link to the "dry IPA" tek would be cool. I made anhydrous magnesium sulfate already.


Pokey the Mad Scientist8)
 
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