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Acid Stage of Extraction -- Clarification requested, + follow-up question

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Samvidbuho

Rising Star
Reading the "DMT EXtraction Guide" & the "FAQ - DMT F. A. Q. & Troubleshooting Guide",

Twice encountering mention of multiple "acid cooks", this for the first time. The procedure remains somewhat obscure to me - the basic image I have is:

1. Combine solvent(H2O)-acid, now for a triple acid cook,
2. Add 1/3 total volume of acid mixture to bark, stir, apply heat over time,

[3. Leaving heat on, add the other 1/3 (stir, heat,) then final 1/3 of solvent-acid]?

The 3rd step is where details lack.

Further question: Is it necessary for one to filter (at least partially) each previous solvent-acid mixture before adding the next volume?



For the sake of knowledge, I imagine someone, say, using flask + stir bar over magnetic stir plate, introduce acid into flask all at once, turn stirring on, turn heat on. The necessitation of multiple acid cooks would seem to be eliminated if the stirring were kept constant, this is so? And, any advantages offered by varying the temperature in a multi-stage acidification step (say by even turning the heat down before adding the next volume of acid) ((and, for the sake of simplicity, ignoring in this imaginary example, any fumes created by addition of acid mixture over heat!)) could be easily transferred to the stir plate setup, again without the need to separate this stage in to multiple components. Yet I don't know, any insight would be much appreciated.


Lastly, I could find no information on Nitric Acid. Again, for knowledge's sake, use of i.e. 68% HNO3 diluted with ultra-pure water to pH 4-5 would appear not damage any of the compounds of interest, and would be safely neutralized with base as ex. KNO3, yet I wouldn't want to make any assumptions.


Much gratitude in advance for any insight, even towards one of the question would be most welcome
 
I add acid only for the first "cook" (just heating the solution is sufficient yield-wise, cooking can turn plant material into gunk that does not filter well maybe also depending on the acid used).

The second and third "cooks" are done with plain water.

I used to prepare pH 4.0 water beforehand for all the cooks but it got concetrated when reducing the filtrate and now I simply add just about 1-2 mL acetic acid per liter per 100 g MHRB (not sure about the numbers but it was enough to bring the solution down to pH 3-4). I believe a pinch of vinegar or lemon juice should be enough since the MHRB solution itself is not basic (I found it slightly acidic actually).

The idea behind this is to convert natural DMT salt (presumably DMT tannate) to acetate, citrate or other salt that may be (?) better broken down by strong base. I've read tannates are hard to freebase even with strong bases like KOH or NaOH.

I tried hydrochloric, phosphoric, citric and acetic acids with same results. I use acetic since it's monoprotic (easy titration to desired pH and also no nasty fumes) but any common acid would do in theory.

Some people dispute whether the acid cook is really necessary, especially if you don't plan to defat.
 
Ah, ah, ah - I think I get it now. The concentrating while reducing the filtrate, the addition of water for the 2nd and 3rd simmer makes sense in this context. In the past, someone never did the reduction step, still to good results, but I think it would be good to do that. Do you let the reduction happen during these two steps, then, evaporating the water?
Thank you for explaining this, as well as with the acids :)


Instead of using H2O for the 2nd and 3rd simmerings, have you ever tried refluxing with maybe 20% EtOH-H2O, or another solvent, to try and coax this transition more fluidly?

Thank you again for the help
 
Making multiple acid cooks is like using the same tea bag for three successive pots of tea.

The point of the acid cook is to make the alkaloids into a form more water-soluble than the tannate.

To increase the energy efficiency of your 2nd and 3rd acid cooks, you can place the liquid from the previous cook into the top of a double boiler to evaporate atop the successive cook.
 
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