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Idea for white freebase crystals from limonene without need for fumaric acid

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endlessness

endlessness

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So Infundibulum once gave the idea of precipitating dmt out of water. It worked when dmt fumarate is dissolved in water and sodium carb (or other non-weak base) is added, then the solution is put in the fridge for 3-5 days (just a few hours is not enough) and dmt precipitates.

I tested this and indeed it worked perfectly. So I added the explanation to BLAB tek and made the wiki fumarates->freebase conversion tek (conversion type 1).

Now I had 2 ideas

If one has fumaric acid:

1- If one wants the freebase straight away without going through all the trouble of precipitating fumarates with FASI for limo or FASA for xylene (or salting with FASW and evaping water), just salt with FASW, and before evaporating already add sodium carbonate and into the fridge for 3-5 days for precipitating the freebase (saving time and energy)

but the main idea I had was for those that dont have fumaric acid. I once tried salting with vinegar and precipitating freebase out of water and it didnt work, Infundibulum says it has to do with acetic acid's chemical properties. Dagger said he tried it and it worked, though, so it seems a hit-and-miss kind of thing, more tests are needed. BUT... I thought, what about other easy to find acids? So the idea I had:

2- Salt limonene with dilute lemon juice solution, add sodium carbonate and put in the fridge for 3-5 days to see if dmt precipitates. Anybody can find lemon all around the world, and if it works to get pure white freebase crystals like that, it would be wonderful, no trouble of evaporating or waiting for fumarate precipitations, no need for hard-to-find (for some people) fumaric acid, etc..

Anybody willing to try this out? The worse that can happen is it doesnt precipitate and then one needs to re-extract the solution...
 
DMT freebase precipitates very nicely (and quickly) from DMT acetate when NaOH is used as the base. I’ve done this several times when cleaning very dirty spice (looked like brown sugar).

Here’s what I did: Dissolve dirty spice in vinegar, dilute with water, add NaOH solution. The solution immediately becomes opaque and the freebase starts to settle out very quickly.
 
hmmm interesting, I tried using sodium carbonate, maybe thats why. With sodium carbonate it didnt work for me.. Maybe it has to be lye, which is fine to some extent though personally I would preffer if the last chemicals to be in touch with spice would be more 'inert' than lye, considering after precipitation one would already smoke it.

Anyways thanks for the heads up!
 
Yes, it does work very nicely with lye.

In addition, I think you can extract the dmt freebase in a matter of minutes this way, provided the concentration of dmt freebase is high enough. What you do is sprinkle lye beads into the water and just let it fall to the bottom. As it falls it will instantly precipitate dmt freebase. In a short time it will all be in a concentrated thin layer on the bottom of the glass. Then heat the glass enough to turn the dmt freebase to a liquid. Here is where the concentration of dmt freebase comes in. It needs to be high enough to be able to turn into a liquid. When this has happened, just start stirring it around. This should make the precipitating dmt into a liquid as well.

When this is done, just cool it down in the fridge to make the dmt liquid harder. Then pour off the water. The freebase dmt can then be air dried. It should crystalize in a few days to a week. I have had no problems with loss of actives this way, even though the freebase has been laying in room temperature with air contact for 1-2 months.
 
SWIM forgot about this thread, but is in the process of a 2nd small batch extraction where he is already at the FASW step. That is being frozen now to separate from the limo. I told him to try your solution 1 for like 50% (or all) of the FASW once that is separated. Maybe if he does 50/50 normal way vs evaping fumarates he can get some sort of comparison.

Hopefully he can remember next time to try the lemon juice thing out.
 
Hi endlessness, quick question about water precipittion: fasw once the emulsion settled has been mixed with sodium carbonate water (maybe not enough saturated??...) and put in the fridge which was pretty strong. Other liquids were in the fridge too but only the jars with the goodies froze :-( interesting! like the sod carb make the water more sensitive to cold...
The jars has been thawed but now there is two layers, one really thick with flowing crystals at the bottom (probably sodium carbonate?) and one quarter at the top is liquid!

Could you or anyone tell what's going on and if it is possible to salvage the spice from there??

Many thanks
 
it would help if you would tell us how much dmt is it, approximately how much water was used to dissolve it (hot or not), how much sodium carb was used to saturate water (and how exactly you did that saturation, how long you let it settle, what temp was the water, was it filtered to remove excess sodium carb, etc). If you can also post pictures, all of these are things that help us getting an understanding of whats going on.

Dont throw anything away it can always be saved :)

by the way, just as a first look (still will wait for your clarifications to really try to give some feedback), I think you mistook fridge for freezer. Its not meant to be frozen, rather to be put in the fridge. Maybe you added it to the freezer and all sodium carbonate crashed out together with your dmt so even after its thawed the sodium carb is staying precipitated and not really redissolving, so what you have is a bunch of sodium carbonate and dmt. If thats the case you'll have to separate them (decant/filter) and then repeatedly wash the solids with water to remove sodium carbonate and leave you with dmt freebase.
 
Thanks endless for your really quick answer, so it was the second salting of an exteraction of 100g of MHRB so no idea of the amount of dmt (perhaps about 500mg...), the sodium carbonate was added to about 100ml of water till saturation but the sodium carbo ran out... but the water seemed to be saturated:oops: , no idea of temperature:? , and no pictures right now... it seems like the procedure was not followed as it should be, that explains why that happend...

And no there is no mistakes between fridge and freezer but the fridge seems going very strong. It seems like what you explain is exactly what's going on, the sodium carbonate crystals at the bottom mixed with the spice because of the freezing process.
So conclusion there gonna be some washing with water as you adviced, thank you so much ma for your time next time the procedure will be better followed...

One more thing, freebase does not disolve at all in water?

Cheers:d
 
SWIM has done the FASW->Sodium Carbonate conversion a few times now and each time he has gotten those same huge sodium carbonate crystals in the container along with the Freebase. Once it was a conversion from already evaperated Fumarate to Freebase and once it was directly from the FASW as outlined in this thread. He thinks that perhaps his fridge might be too cold as well which is causing this or perhaps over saturated and or not properly decanted sodium carbonate water. The first time he didn't let the Sodium carbonate water settle for very long so it was hard to say. 2nd time he did let it settle, but the water that was used was warmed slightly so it would allow more saturation. Next time SWIM is going to use room temp dH2O and make sure that the Sodium Carbonate water settles for a bit and perhaps is poured through a coffee filter when decanted. He thinks (with no great chemistry knowledge) it could be either too cold a fridge or over saturated Sodium Carbonate which then forms the crystals.


It seems to be a not so uncommon problem from what I found after doing a search here once SWIM had the issue. I don't think Endlessness has ever had this problem but a few others have such as:

DMT fumarate conversion comparison (pics) - FASA/FASI/FASW - Welcome to the DMT-Nexus (I posted a similar experience from SWIMS first extraction a few posts down).


But even so you can just do as endlessness says and wash all the crystals with water. You should probably see some really clear big crystals as well as some flaky/shiny freebase. SWIM just poured the crystals onto a coffee filter and then after that all drained through continued to pour water over them to soak up the Sodium carbonate crystals into the H20 and then through the filter. The Freebase is not very (? at all) soluable in room temp water so it will stick around in the filter.
 
Thanks Malaclypse, your advices are much appreciated and that's reassuring to see others came across the same phenomenon... let's get to work now... ;-)
 
if one precips with sodium carb - on fumarates - as one does it within 10 mins yellow goo is all over
of one decants the - milk - then lets that drop out the dmt is white
repeating the proceedure can get more - white dmt out of the yellow -but the yellow is good as is.
nice tek - only now do i realize it is the best freebasing tek.
 
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