TEK "TnT tek" - Vodka DMT extraction for oral use TEK (super easy!)

[Transform]

Has anyone sat down and worked out the expected fraction of DMT that would be expected to end up in the precipitate? I have insufficient knowledge to work it out but it really seems like the partitioning would be poor (not no idea how poor) and I would like to understand.

Partitioning? What do you mean by that? When it's an insoluble solid phase versus a liquid phase, we don't really talk about partitioning. DMT is exceptionally soluble in aqueous ethanol; rinsing the precipitated calcium tannin a couple of times with a little more vodka recovers effectively all the soluble alkaloids. The rinsing makes up for whatever mechanical holdup of dissolved DMT there may have been.

 

[stuartroelke]

Has anyone sat down and worked out the expected fraction of DMT that would be expected to end up in the precipitate? I have insufficient knowledge to work it out but it really seems like the partitioning would be poor (not no idea how poor) and I would like to understand.

I've also been curious about this. Since freebase is soluble in pure ethanol, I've often wondered what the potential loss could be when it comes to saturation and freeze precipitation / recrystallization.

 

[stuartroelke]

The lime precipitation occurs well enough at room temperature. Calcium hydroxide is somewhat unusual in having an inverse solubility curve in water, meaning that it's actually more soluble at lower temperatures. I'm not sure how that shapes up when it comes to aquoethanolic solutions, nor have I any observations on what happens to the lime-treated solution on heating. It's a nuance that appears to be unimportant at present.

The reason I mention freezing is as an alternative method for concentrating the solution by freezing the water out as ice, thus conserving the ethanol content. This is in contrast to evaporation, where the ethanol preferentially gets removed. So, only freeze it if you want to try that out as a method for concentrating the tincture. It's likely to have good keeping properties when kept in a closed bottle and protected from light, and the liquid form can help with measuring the doses once you've established its concentration one way or another.

And I'm super-stoked to find that this tannin removal method has proven to be so useful to you

Wouldn't freezing either acetone or alcohol—solvents that also extract fats and oils—without a defat step lead to some congealing with the frozen water layer? Wouldn't that cause loss since freebase is lipophilic? Would lowering the pH first—to get protonated salts—work better? Or, does the CaOH somehow remove enough lipids?

I only ask because this is an issue with extracting pure salvinorin A (highly lipophilic), and that is why defatting is done before freeze precipitation / recrystalization.

 

[Transform]

Wouldn't freezing either acetone or alcohol—solvents that also extract fats and oils—without a defat step lead to some congealing with the frozen water layer? Wouldn't that cause loss since freebase is lipophilic? Would lowering the pH first—to get protonated salts—work better? Or, does the CaOH somehow remove enough lipids?

I only ask because this is an issue with extracting pure salvinorin A (highly lipophilic), and that is why defatting is done before freeze precipitation / recrystalization.

That depends entirely on the specific substance and solvent. In the case of DMT in aqueous ethanol, preliminary experiments indicate that it retains significant solubility at freezer temperatures, with a phase separation - which nonetheless remains liquid (albeit somewhat viscous, i.e. goo) at c. -24°C - occurs only with aquoethanolic mixtures below c. 25% ABV. There's ample room for further, more precise experimentation to pin down the figures. A set of temperature/concentration/solubility graphs would be the main research goal there.

With the TnT tincture - the solids from one example of which were analysed and found to consist of only 20% DMT - it's possible to separate water ice as crystals without any other solids forming, although it's equally worth noting that the analysed sample was not freeze-dewatered, and vice-versa.

So, in the case of DMT in aqueous ethanol at the temperature of a domestic freezer, freeze precipitation seems difficult at best, and when in the form of a crude tincture containing as yet undefined "impurities" this appears to be practically impossible.

 

[stuartroelke]

That depends entirely on the specific substance and solvent. In the case of DMT in aqueous ethanol, preliminary experiments indicate that it retains significant solubility at freezer temperatures, with a phase separation - which nonetheless remains liquid (albeit somewhat viscous, i.e. goo) at c. -24°C - occurs only with aquoethanolic mixtures below c. 25% ABV. There's ample room for further, more precise experimentation to pin down the figures. A set of temperature/concentration/solubility graphs would be the main research goal there.

With the TnT tincture - the solids from one example of which were analysed and found to consist of only 20% DMT - it's possible to separate water ice as crystals without any other solids forming, although it's equally worth noting that the analysed sample was not freeze-dewatered, and vice-versa.

So, in the case of DMT in aqueous ethanol at the temperature of a domestic freezer, freeze precipitation seems difficult at best, and when in the form of a crude tincture containing as yet undefined "impurities" this appears to be practically impossible.

I wasn't thinking decent freeze precipitation would be possible with ethanol; I was hypothesizing about potential loss when highly lipophilic compounds partition into lipids, which then separate upon cooling and might get tossed out with the ice. Does that make sense?


Not sure if this is actually a concern here. I just know that's why fats / oils / waxes are often removed before putting saturated ethanol in the freezer (salvinorin A was the example I'm most familiar with). I'm probably overthinking this since MHRB ethanol extracts "goo-ing" could have more to do with polysaccharides than lipids and waxes.

 

[Transform]

I wasn't thinking decent freeze precipitation would be possible with ethanol; I was hypothesizing about potential loss when highly lipophilic compounds partition into lipids, which then separate upon cooling and might get tossed out with the ice. Does that make sense?

Well, there's the Golden Rule…

in the field of extraction there is a Golden Rule: don't chuck ANYTHING away until you're sure you've got the goods!

so, basically, you're not going to toss away the ice without being sure it's only water and nothing else in any significant quantity. Very much a valid point, though.

Not sure if this is actually a concern here. I just know that's why fats / oils / waxes are often removed before putting saturated ethanol in the freezer (salvinorin A was the example I'm most familiar with). I'm probably overthinking this since MHRB ethanol extracts "goo-ing" could have more to do with polysaccharides than lipids and waxes.

The main issue with separating ice crystals from the TnT MHRB tinctures appears to be mechanical losses due to the tincture sticking to and between the ice crystals. This becomes another reason to hold onto the ice.

There's also the possibility that I may have a slight issue with hoarding, at least, apparently, when compared to the average US citizen (and just where is this "away" that things get chucked? )