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official extraction help thread

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Mini A/B - the acid phase does a good job of breaking up the polymer. Ime, re-x of polymeric goo tends to be wasteful and confusing, as different sizes of polymer dissolve at different temperatures.
thanks, just got a bit of goo off my first pull of an ATB with 50g Acuminata bark, ill see how much i get off it and if i think its worth it ill try a mini a/b - have wanted to try a proper hit of the goo/spice so keen to give it a whirl. Do you think freeze precip would be better to form crystals than evaporating for any reason? I evapped this pull.
 
Do you think freeze precip would be better to form crystals than evaporating for any reason?
While they can both produce good results, freeze precipitation would tend to produce purer crystals, although slow evaporation is the favoured way of producing large crystals.

The main thing with evaporation is that the last remaining portion of solvent will contain a higher concentration of impurities, and a mixed solvent like naphtha will have its more volatile components evaporating in greater proportion at first. This means that the material which crystallises later on is more likely to contain impurities and trapped hydrocarbons. There may also be a bit more polymerisation later on, as a function of exposure to oxygen for a longer period.

Freeze precipitation carries the further advantage of preserving the solvent for subsequent reuse; conversely, evaporated solvent is effectively lost, unless one were going to unusual lengths to capture and condense it - something which isn't realistically feasible for the average hobbyist as the required rate of evaporation is too slow.
 
why not take the opportunity to try FASA? it doesnt have to specifically be fumaric acid however, i forget which other ones, pretty sure its in one of the FASA/FASI threads, but theres other, more common, acids you can use that will form a DMT salt that immediately crashes out of a NP solvent upon addition of acetone or isopropanol that has been saturated with as much of the given acid as it can hold. I think ascorbic acid (vitamin C) is one of them, regardless of if it is, ascorbate can be smoked directly. citric acid too though im pretty sure its really hygroscopic so it might not be practical without molecular sieves and a dessicator. odds are your local brew shop will have something. it was either speculated or confirmed, tartaric acid may work too, which is available at any supermarket. It is worth digging into, FASA will work with many acids, saturating many solvents.

after filtering and drying, you then dissolve in a very small amount of clean water and add some carbonate solution, and basify the carboxylic DMT salt back to the freebase we know and love.
the great thing is it fits right into an existing tek, you just use something like toluene, xylene, limonene perhaps, or another NPS that dissolves DMT too well to crystalize from, but will happily extract at room temp, in place of naptha. And instead of freeze precip or evap, you dry it (magnesium sulfate) then filter and add fumaric acid saturated acetone, which also must be dry similarly.
you can use exotic or low volatility solvents here too and just wash them out after you collect your DMT fumarate crystals. the acetone will wash out with water, as will IPA. the solvent can be re-used so much.
Later you dissolve the fumarate in a small volume of water and drip in some sodium or potassium carbonate.

That milky DMT freebase milk in the video eventually forms large clean crystals, which someone has documented and put up in the wiki.
another important aspect is that once you have your DMT fumarate, it is insanely stable in that form, kept dry and refrigerated it will last decades iirc. so if you are doing a bigger batch than youl consume for a good long while, you only have to freebase what you intend to use.

since FASA works with limonene, you can do your entire process start to finish using food-safe chemicals, or house-safe solvents, this was a remark someone made that stuck with me.
 

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I’ve been having issues with re x. I heat up the heptane in a crystalizing dish. Wait till I start to see bubbles and toss the Fb from an STB extraction. I use to get a layer of crystals on top of slag. Last few years, some of the crystals clearly get caught in the slag. I hope you guys can help me out. I use to use Doc Edingtons and never had an issue with that, but it’s been out of business for a while. I’ve tried Bestine, 99-100% heptane from Amazon and I have success here and there but can never replicate. Any help is appreciated. I’m sure I’m doing something wrong. Tried altering temp, nothing seems to help. Thank you
 

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I heat up the heptane in a crystalizing dish. Wait till I start to see bubbles and toss the Fb from an STB extraction
Small detail, but it might be better to add the hot heptane to the crystals, for more precise control of the solvent ratio. There is a slight issue with the low melting point of at least one of the DMT polymorphs - and all of them melt at a lower temperature than boiling heptane, of course. In that case, a more careful addition of the right amount of FB powder to somewhat cooler heptane could bring better results. Oiling out is more likely to occur if the solvent is oversaturated. This is something that tryptamines are particularly prone to do, especially if the DMT already starts crashing out of the heptane at a temperature above its melting point.

If polymerisation has become an issue - perhaps due to the starting material, for example - you'll likely see better results if you run the initial product through a mini A/B and crystallise carefully from that.
 
Small detail, but it might be better to add the hot heptane to the crystals, for more precise control of the solvent ratio. There is a slight issue with the low melting point of at least one of the DMT polymorphs - and all of them melt at a lower temperature than boiling heptane, of course. In that case, a more careful addition of the right amount of FB powder to somewhat cooler heptane could bring better results. Oiling out is more likely to occur if the solvent is oversaturated. This is something that tryptamines are particularly prone to do, especially if the DMT already starts crashing out of the heptane at a temperature above its melting point.

If polymerisation has become an issue - perhaps due to the starting material, for example - you'll likely see better results if you run the initial product through a mini A/B and crystallise carefully from that.
Thanks for the insight. In the hot water bath I don’t think the heptane was up to boiling but I’ve checked it before at that point and it was 140-160. Shulgin remarked there were many different ranges of crystallization temps and my old method use to produce great white fluffy crystals. I just never use to have an issue with this. I have tried lower solvent temps and have the same issues, could be bad heptane maybe. What mini ab tek would you recommend? Also as far as basic chemistry regarding these extractions, is there somewhere I can find out about basic terminology? My chemistry knowledge is lacking for sure.
 
@Transform Thank you for telling me to freeze precip !! Finnaly got crystals 😁 - Used 'Acacia acuminata minimalist ATB (50g) bark' (dont think the tek is on here found it on reddit), a small yeild but it was expected as i tried evapping half my solvent and tried to precip the other half just to see the difference - got more pulls to go so will defs freeze precip from now on. Super stoked much appreciate the help. Got more pulls to go as well so super keen to see how much I get in total
 

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Ok, I have a magnetic stirrer and by this circumstance I got Teflon stirring things....

Question: I only found information that Teflon is not affected or attacked by lye water even if high lye for stb, is this correct?

Anyone got better knowledge or superior Infos?

Samen question for a stainless steel filter, would it work for a lye soup?

Noticed the language thing. Will try to not post with a beer to much again.
 
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Ok, I have a magnetic stirrer and by this circumstance I got Teflon stirring things....

Question: I only found information that Teflon is not affected or attacked by lye water even if high lye for stb, is this correct?

Anyone got better knowledge or superior Infos?

Samen question for a stainless steel filter, would it work for a lye soup?

Noticed the language thing. Will try to not post with a beer to much again.
Teflon is effectively inert to lye solutions at our usual working temperature, as is stainless steel. Only significantly stronger bases like butyl lithium start causing discoloration of the teflon, while stainless steel starts getting noticeably attacked by highly concentrated lye at a significant rate somewhere above 180°C. Resistance of the steel will depend on the particular alloy, as well as whether there is any contact with alloys of a more inert composition, but it will be practically unaffected by short term contact with aqueous alkaline solutions at room temperature.
 
Ah ok, ty.

The stainless steel is for a short pouring, my lab filters get stuck with micro residue almost instantly. Therefore I think it should work with the stainless steel, if the stitching holds its place?
At least worth the try next time I guess.



Discoloration? You mean if it gets transparent?
Or you mean the Teflon gets brownish?
I forgot the stirring rods in soup for a few days then I was to lazy and so on. Now one of it got slightly brown edges.... ;(

As far as I can see there was not much DMT left, no crystals formed after 12h yesterday. Will check another time later....
 
Discoloration? You mean if it gets transparent?
Or you mean the Teflon gets brownish?
I forgot the stirring rods in soup for a few days then I was to lazy and so on. Now one of it got slightly brown edges..
Brownish. Unfortunately that's hard to distinguish from mimosa dye, except the latter should be removable with a short treatment using hypochlorite bleach.

Either way, it's entirely superficial and of little consequence - even if it turned out to be base-induced hydrolysis, the traces of fluoride released into the base soup will just stay there when the NPS pulls are made, and the stir bars remain usable if you're not intending to do any especially sensitive chemical reactions where you'd be better off starting with new equipment.
 
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