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.
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.
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?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
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.
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…
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.
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.
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So you’re telling me to stop keeping spent plant powders in jars “just in case”?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?
Eat Compost, there is a character in the last series of 'The Boys' who eats dirt, maybe something to aspire to haha
Btw, that one's already out the stable door over here:
Does this mean: the extraction is complete in 2 hours but it won't harm anything to stretch this phase out for a few days?
At what stage, exactly, would I introduce some vinegar, and how much?
Yes, the initial alcoholic extraction can stand more or less indefinitely, but it's worth understanding it in context of the next step:
There's also scope for a cold rest after filtering off the bark. This will allow more tannins to precipitate before adding the lime, and hence will reduce the amount of lime required. HOWEVER, there's a higher probability of DMT/alkaloidal residue remaining in the insolubles before lime has been added, which is part of the reason for my suggestion of doing the initial extraction warm and minimising wait times, then taking it slow and steady with the lime precipitation instead.
Only add acid after the lime precipitation has been completed, and the clear liquid has been separated from any solids. Ideally this should be left for any turbidity to settle out and decanted once more before neutralisation. Imo, while vinegar will work, it doesn't taste so great, so you might be better off using one of the other food acids like citric, malic or tartaric. Ascorbic is OK for short-term use, but has a tendency to decompose. Vinegar is mostly water too, so it'll be diluting your solution relatively more than some other acids.
Ok, i didn't see any mention of heating on the tek instructions, so I went room temp. It's been sitting in vodka for about 14 hours. According to the tek instructions my next step is to filter out the plant matter and begin slowly adding the lime. Do you suggest another step prior to that?
cool, how much citric acid do you recommend?
heard and appreciated
If you let the filtered brew stand in to the fridge for a while, you see further tannins precipitate. This may be better for lime economy, but it remains to be established whether any significant amount of actives gets trapped in the sediment.
I'd recommend titrating a small sample of the tincture and using a result of that test to calculate a sensible amount for the remaining volume. If that sounds too daunting, try adding, say, 10 mg increments of acid to a 10 mL aliquot until you get to a desired pH level as determined either by spotting on pH test paper or simply by tasting a tiny drop. A pH of 7 or less should be fine, but you'll not want to go as low as pH 4 without a sound reason.
Shouldn't be an issue, but I mention it because the idea originated from a research paper where acorns were heated in vodka to extract the tannins. It's linked to in several posts over the past couple of years while the method was first being developed and tested.
