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Plodding on -- FASA without limonene Options
 
anonhippie
#1 Posted : 9/12/2013 10:10:19 AM

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Joined: 16-Jun-2013
Last visit: 24-Dec-2022
I'm looking for a little advice on how to perform my next extraction. My problem is that I can't get my hands on light naphtha, even from lighter fluid. So instead I've performed several alternative teks, with varying success.

Veggie Tek
So, a month or so ago, I was using the veggie tek in an attempt to extract dmt from phalaris. Besides the fact that I never got DMT (I think the plant was not phalaris in the end) the process was not exactly friendly because of the enormous amount of evaporation that was required.

References:
Dreamer042's Hippie Tek
The frustratingly un-locatable poor man's tek that I wish I could read

STB with manual precipitation
Then I managed to obtain MHRB. I decided to follow the later half of the veggie tek. At that point it wasn't a veggie tek at all because using NaOH required using another non-polar besides veggie oil due to the saponification risk, but anyway the steps were:
1) STB using NaOH on the MHRB -- let it sit for several days
2) Seperate solids from liquids to ease pulling (liquids go in sep. funnel, solids in jar)
3) 4-5 pulls with HEAVY naphtha. I haven't been able to find a light naphtha. This product is sold as camp fuel, is clear, and evaporates slowly but cleanly. Maybe its not even naphtha??? I couldn't find an MSDS.... Italy.....
4) Wash naphtha with water basified with sodium carbonate.
5) Pull from the naphtha using water acidified with citric acid.
6) Evaporate the water down to a small amount.
7) Dry and basify the water with sodium carbonate
8 ) pull with alcohol. decant it. evaporate it.

Because I used a small amount of initial material, the yield was also small and I ended up smoking a lot of it in tobacco/passion flower splifs. Yum!-- however the trips never lasted that long or went that deep.

Refs:
Explanation of Heavy vs Light Naphtha
Not everyone's worried about saponification -- LucidLemonade's tek

STB with water precip.
I then extracted the leftovers from an aya brew that I never drank as well as a final cleanup of the extraction above. My new route was mostly the same except for the later steps, because I hate evapping (I always feel that I lose product and patience):

6) Basify the water with NaOH, put it in the fridge for a day.
7)The precipitate was filtered and then pulled using 95% alcohol.

This was used to make changa. My changa turned out to be very heavy on the harmalas, and barely any DMT effect. Given the initial materials, and eyeing the precipitate I would of thought that I would have had a good ratio. I've finally bought a mg scale online, so hopefully in the future I won't be submitted to the vagaries of extraction yields.

When I created water basified with NaOH, my tap water precipitated out a lot of gunk. Its obviously very hard water, so if I were to do the above tek again I should obviously use distilled water. Maybe a lot of that precipitate wasn't DMT. I thought about this before hand, and tried to remedy by the final alcohol pull. I tried to dry the alcohol with sodium carbonate so it wouldn't pick up any water-solubles that came from the tap water / NaOH. On trying to dissolve the precipitate, it did so very slowly.... could this have been an indication that the DMT was highly contaminated with hard water precipitates?

References:
Various posts on precipitating DMT out of water:
https://www.dmt-nexus.me...spx?g=posts&t=25811
https://www.dmt-nexus.me...spx?g=posts&t=15118
https://www.dmt-nexus.me...spx?g=posts&t=19438

My Future -- Acetone extract with FASA precip?
In italy fumaric acid is illegal. I think this paper has something to do with it. But I've hypothetically found the one supplier on ebay who doesn't know these laws and perhaps it will even hypothetically arrive.

Now I want to do this tek:
Quote:
A Safer DMT Extraction - No Lye, No Naphtha

For one thing, it inspired a DMT extraction that doesn't require any lye or hydrocarbon solvents (like naphtha, toluene, etc.). This tek uses only citric acid, fumaric acid, acetone, sodium carbonate, and water. This makes it much safer for the layman than playing with strong lye solutions and being exposed to the vapors of hydrocarbon solvents.

Infundibulum wrote:
The purely imaginary method described below does work, but it works really really slow. SWIM's FOAF was able to extract ~100mg freebase alkaloids from 10g of MHRB. This method does not discriminate between the alkaloids that are extracted (j.spice, d., d-Noxide etc etc), this is however a subject of discussion.

The tek:

1) dissolve 5g of citric acid per 100ml acetone

2) take the shredded/powdered bark and cover it with enough citric acid acetone. Incubate in a warm place, gently agitating every so often. After 2-3 hours, filter off the citric-acid saturated acetone extract and set aside (this solution should have acquired the dark reddish colour of MHRB). Repeat 2 more times.

3) saturate acetone with fumaric acid. Acetone can hold ~20mg/ml fumaric acid if let for a day or so to completely dissolve.

4) Add the fumaric acid-saturated acetone in the citric acid-saturated acetone MHRB extract. One cannot put too much.

5) Set it aside and wait for 2-3 days. One should see a yellowish precipitate on the bottom.

NOTE: In step 2 one is making an acetone extraction and at the same time converting the alkaloids their citrate salt. After addition of the fumaric acid-saturated acetone in step 4, there is an interconversion of alkaloid-citrate to alkaloid-fumarate salt, like:

dmt-citrate + fumaric acid <-> dmt-fumarate + citric acid

citric acid has a pKa of 3.13, while fumaric acid's pka is 3.43. Fumaric acid is a weaker acid and thus in the above reaction one should have most of the dmt as a citrate salt and just a tiny amount as a fumarate salt. dmt-fumarate however is totally insoluble in acetone (while dmt-citrate is perfectly soluble), and it precipitates as soon as it forms. The insolubility of dmt-fumarate acts therefore as a "sink" and given time all of the dmt-citrate will eventually convert to dmt-fumarate and precipitate out.

6) wash the precipitated fumarate salts with acetone, then take them out and let them dry.

7) dissolve the alkaloid-fumarate salts in 5ml of tap water, then and then add saturated sodium carbonate to make the solution basic. The alkaloids will be freebased and the solution will become milky. In 3 days they will precipitate out forming nice needle-like crystal in the basic solution. At this stage, one can filter the solution (nasty procedure since the crystals tend to be sticky and waxy) and retrieve any left alkaloids by dissolving them in acetone.

8 ) Let the crystals dry, wash them with acetone (it removes any traces of sodium corbonate which is totally insoluble in acetone), evaporate the acetone and enjoy the product.

For the FOAF of SWIM 30mg were for a good STRONG experience.


However, I see everyone is using xylene or toluene or limonene to pre-extract the DMT. I want to be serious, but on the other hand I don't want to spend around $30-40 having d-limo shipped to me. Does this tek work well if I give it in enough time? Could it be a sort of big leisurely FASA without d-limo? Or should I be truer to my hippie ways and go back to the hippie tek Big grin ???

Refs:
Original post for FASA tek
Additional ideas on FASA

Thank you so much for reading this long post! I'm getting a little discouraged and tired of low yields, so I really want my next extraction to be a good one. While I'm preparing for such a venture, ayahuasca and other interests will have to keep me busy for the rest of my vacation.
 

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endlessness
#2 Posted : 9/12/2013 1:19:28 PM

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If you have alcohol, sodium carb , fumaric acid and acetone, I suggest you do this instead:

https://www.dmt-nexus.me...spx?g=posts&t=30501

and then at the end you can do FASA on it to have a purer product.

I´ve tried once to straight away base the mimosa and pull with acetone and do FASA, but the alkaloids did not precipitate, maybe too many impurities in solvent prevented the crystallization from happen. You could probably still do it, but if alkaloids dont crystallize, evap acetone to leave your impure dmt fumarate, then mix with sodium carb and bit of water to make paste, dry again, pull with acetone again, and do FASA again. Maybe by repeating, you can get it cleaner and cleaner, until it precipitates nicely.
 
 
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