Author Topic: Largescale DMT alcohol cake extraction method?  (Read 552 times)

micro

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Re: Largescale DMT alcohol cake extraction method?
« Reply #20 on: August 13, 2011, 03:59:13 PM »
I wonder where the failure is. Recovered under 300mg of crude tar from 360g of finely powdered MHRB.
MHRB was based with NaOH and extracted with toluene.
Resulting extract was freeze percipated and the toluene decanted.
Toluene residue was air dried and then dissolved in acetone.
The resulting asetone solution was then mixed with cannabis leaf.
Bioassay of said mixture was rewarding. Definitely active product.

But the yield was questionably low.
Multiple extractions to the same material will be pursued.

This whole process of going thru 1.5kg of bark has prowided low yeilds.
The Cake method was used for the first 200g with utter failure, it does not work with finely powdered bark.
But een going thru the first kg of raw material, only about 1.5g of pure white solid was produced.
« Last Edit: August 13, 2011, 04:01:09 PM by micro »

romiir

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Re: Largescale DMT alcohol cake extraction method?
« Reply #21 on: August 15, 2011, 01:25:11 AM »
The best way to do this of the currently established methods is to use a pressure buchner funnel system with the super-finely powdered plant material. Think how a Mr. Coffee Espresso machine is built, but larger. There are many creative ways to do this (plastic bottle with drilled lid filter and a bar clamp to apply the pressure isn't unheard of, and it is effective), pressure filtration of the alcohol though the material under high temperature and pressure followed by evaporation will yield the plant resin extract which is much easier to do an standard A/B tek upon. (the plant extract will be acidic, so, defat if needed then do STB) A single alcohol pull with 3 volumes more alcohol then the plant material will yield nearly all of the resin content even if the temperature isn't that great. Some patience is needed for this, especially on the large scale, but it can be done. (think 12 hour pressure filtration for powdery material) Also it goes without saying, no sparks or open flame around the large volume of alcohol. In a sealed system there is no smell, and the alcohol is recyclable. (STB from the alcohol fraction, skip evaporation and do non-polar extraction, neutralize alcohol ph (or slightly acidic), distill (or filter), repeat, though you can evap to see what the resin extract looks like.)

Other thoughts:

Temperature won't hurt anything here as long as its acidic in aqueous solution. The plant alkaloids are always found in their salt forms, but if your really paranoid, add a bit of your favorite acid to the extraction liquid.

Gravity can also be used, but you need a lot of gravity... (tall column, lots of fluid pressure) and patience... Gravity doesn't work very well on the super powdery material (very slow), and if you don't powder it, you aren't getting the yields you should be.

Also stay away from methanol, if you don't understand how to use sugar + yeast + still to create 95% EtOH, stay away from these extractions for your own good. Isopropyl alcohol is also a good substitute, and doesn't have any detrimental effects on alkaloids, reactants, nor is it particularly toxic in humans (but it's expensive, and if you oxidize it somehow (not really relevant here) you end up with acetone rather then nasty crap, methanol loves to form nasty toxic crap, crap in, crap out...)


Oh and I almost forgot, Pickling Lime (CaOH) is food safe, doesn't burn you unless your really stupid, and is a great OTC base for such things found at any store that sells canning equipment in lieu of the nasty lye. CaOH will take you up to a ph of 12.3 or 12.4, and IIRC DMT is 99% freebased at pH 10.68, and 99.9% freebased at 11.68. Anything 12 and up is overkill for DMT, so it is plenty caustic, but won't even (easily) burn your bare hands, whereas NaOH will dissolve them.

Boy do I love science! These purely theoretical forum discussions are fun! However I don't answer PMs, do not PM me asking for advice.

romiir

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Re: Largescale DMT alcohol cake extraction method?
« Reply #22 on: August 15, 2011, 01:40:13 AM »
This whole process of going thru 1.5kg of bark has prowided low yeilds.
The Cake method was used for the first 200g with utter failure, it does not work with finely powdered bark.
But een going thru the first kg of raw material, only about 1.5g of pure white solid was produced.

Well... I'd suggest not harvesting the plants too early nor during the wet season. Or finding someone who actually ships you root bark rather then normal bark during the dry season. If you powder it yourself it is a lot easier to see what you have.

Many vendors (especially Mexican) are harvesting too young of plants, and mixing a fair amount of normal bark powder in with your order for your convenience, it has plenty of excellent purple/red tannin dyes for all your textile needs! =]

From wikipedia:
"Dried Mexican Mimosa tenuiflora root bark has been recently shown to have a DMT (Dimethyltryptamine) content of about 1%.[3] The stem bark has about 0.03% DMT."

This is all just hearsay of course.

joejack

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Re: Largescale DMT alcohol cake extraction method?
« Reply #23 on: August 18, 2011, 07:24:09 PM »
There is a method in trippipedia, a finnish drug version of wikipedia.It's an detailed extraction technique for mimosa hostilis, the quide states a 570mg yeld from 100g of the plant.Would you guys like me to translate it? the guide is quite kitchen friendly and the most dangerous chemical used is hydroxide.

I was thinking about harvesting some (Phalaris arundinacea),red canary grass.Im very close to doing so, please, give me the push to do it :P

only concern i have is that im not much of a herbalist and here in finland we have plants that look like it, so what happens if i try to isolate it from plant that isn't red canary grass, like its decorational version?

the wikipedia has a statement that directly translated would be 'the leaves of the plant contain DMT and 5-MEO-DMT this limits the plants use as livestock but has made some people trying to make drugs of it'. Is it doable with the same guide than with mimosa hostilis?(maybe i should translate it first to have answer to this)

reDEEMed

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Re: Largescale DMT alcohol cake extraction method?
« Reply #24 on: August 18, 2011, 07:54:36 PM »
Sure, I'd love to read it in engrish. I have quite a bit of mhrb and 5% yield would be something I'd have to see to believe.
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Vesp

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Re: Largescale DMT alcohol cake extraction method?
« Reply #25 on: August 20, 2011, 02:09:11 AM »
Has anyone ever actually extracted DMT from Phalaris arundinacea? Obviously there is a lot of talk and texts about how to do it, but I've never heard anyone actually having success with it, besides getting an active goop, or something from a wheat grass juicer.



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joejack

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Re: Largescale DMT alcohol cake extraction method?
« Reply #26 on: August 20, 2011, 12:58:16 PM »
Disclaimer: dont try this untill someone has read this thru and sayed it will work.Also i dont know what white wine vinegar is, im assuming its just acetic acid(i dont like wine in the first place).Also the purified benzin is probably the same stuff as in Zippo lighters.


DMT from Mimosa Hostilis rootbark

 1. Mix 125ml of 5% white wine vinegar to 1 liter of distilled water, boiled water will also do well

        2.grind 100g of Mimosa Hostilis rootbark to fine powder using a good coffee grinder of a blender

       3.Add the rootbark and half of water acetic acid to steamboiler( it's possible to do this with two pots, bigger pot with water and set to stove, smaller pot inside the bigger) mix well and heat with mild power for about two hours, untill it starts to boil.After this put most of the liquid to plastic container.

        4. Add the rest of the water-acetic acid solution to the boiler and reboil.After the heating pour the liquid to same plastic boiler than in part 3.Squeeze the plant to extract all the liquid out from it.Dispose of the rootbark

        5.Put this plastic container to freezer for two hours

        6.After two hours the plant parts should be a mess on the bottom of plastic container.Pour the mess thru old t-shirt thru 750ml bottle and discard the mess.

        7.Preaheat the water in steamboiler and put the bottle to this hot water bath.

        8.Pour 100ml of warm water to a small bottle and add 1 tablespoon of NaOH.Spin the bottle to mix.

         9.Add the water-NaOH mixture slowly to the 750ml bottle in the water bath.Shake the bottle untill the liquid is entirely colored black.Open the bottle after every shake.Leave in the bottle a small space for 20ml of purified benzin.At this point would be nice to check the PH of the liquid, that should be 13,4.

        10.set a small bottle that has purified benzin to another purified steam bath, only 60ml of benzin needed.let the cap slightly open.

        11.When the benzin has warmed, add 20 ml to 750ml bottle in steam bath, and shake for a few minutes.Open the cap after every shake.Set the bottle to steam bath        and wait for the benzin to separate as a clear liquid on top of water.

        12. Use a pipette to separate the benzin to tight container. BE VERY CAREFUL THAT THE DARKER LIQUID DOESNT COME WITH.   


        13. Repeat steps 10  - 12 for two times.

        14.Put the tight container to the freezer.White flakes will appear in few hours, but wait afternight untill all flakes have separated from benzin.

        15. Scrape the bottom of the jar and sides to remove flakes, do this in a cold space

        16.Pour the benzin thru a coffee filter to another pot.Let the flakes dry in filter.Benzin can be reused

        17.DMT is usable at this point, but its recomemded to do a ammonia was to remove impurities.This makes DMT nicer to use
        Freeze a small portion of liquid containing 50% NH4OH and distilled water, after its frozen put few ml thru the dry crystalls in coffee filter so that they are dry   

        18. Let the crystalss dry for  at least 4 hours or overnight


Result : 100g of material produced 570mg of DMT

wouldnt 5% yeld be 5g?

reDEEMed

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Re: Largescale DMT alcohol cake extraction method?
« Reply #27 on: August 23, 2011, 07:14:20 AM »
That yield sounds low. I usually get atleast 1% and I don't really get all hardcore with it.
"Ego is a structure that is erected by a neurotic individual who is a member of a neurotic culture against the facts of the matter. And culture, which we put on like an overcoat, is the collectivized consensus about what sort of neurotic behaviors are acceptable."
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letters

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Re: Largescale DMT alcohol cake extraction method?
« Reply #28 on: August 23, 2011, 05:00:46 PM »
my experience with the cake method is that it is far less convenient then a traditional STB, even in large scale, unless you have a pressure filtration setup or your mimosa is not in powder form.
By far, the best way for extraction (not only for mimosa, but other plants as well which contain alkaloids) is to use soxhlet. a modified large scale liquid liquid extractor can be used for very big scale extractions. we usually do it by moistening the plant matter with ammonia and "soxhletting" that for a day with a suitable solvent.

Wizard X

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Re: Largescale DMT alcohol cake extraction method?
« Reply #29 on: August 24, 2011, 12:54:11 AM »
Interesting reading...
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delafonze19

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Re: Largescale DMT alcohol cake extraction method?
« Reply #30 on: August 24, 2011, 09:50:53 AM »
Attempting a 5kg stb is an recurring nightmare. Each freeze precip carries a ton of black/brown goo. Five gallon bucket is not big enough to properly dilute. try heating the thing, the aquarium immersion heater lasted about 2 days. In a plesant dream an a/b with defat at minimum but even better the cake. I have never heard of good results from ammonia wash
« Last Edit: August 24, 2011, 03:28:18 PM by delafonze19 »

letters

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Re: Largescale DMT alcohol cake extraction method?
« Reply #31 on: August 31, 2011, 12:47:36 PM »
Attempting a 5kg stb is an recurring nightmare. Each freeze precip carries a ton of black/brown goo. Five gallon bucket is not big enough to properly dilute. try heating the thing, the aquarium immersion heater lasted about 2 days. In a plesant dream an a/b with defat at minimum but even better the cake. I have never heard of good results from ammonia wash

usually 1Gal jug is good for .5Kg, so 5Kg should be done preferably in a 10Gal drum. using a turkey baster of some kind makes pulling the alkanes solvents easy. Heating this whole thing can be easily done in your bath tub with hot water from the tap. shaking might require 2 people, or you could use a wide mouth drum and stir it with a wooden or glass rod like a witch would over her pot.