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Nontoxic Extraction Experimentation Log w/ Photos (tek WIP) Options
 
amor_fati
#1 Posted : 9/19/2009 4:04:35 PM

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This thread's shifted gears quite a bit since it was opened. It started as a simple nontoxic extraction of chaliponga that ended in failure, but has mutated into a seemingly functional nontoxic tek for MHRB (possibly chaliponga, as well). The meat of this thread started here and developed into an experimental tek. The basic rundown of this is that a jar containing MHRB, lime, water and limonene can be fitted to a blender to accomplish pulverization, reaction and mixing all in one go and more effectively than any of those steps performed separately. The material can then be transfered to THP in order to thoroughly wash with limonene and collect it for salting w/ FASW.

Original OP:
Quote:
SWIM's been working on this, and has decided to begin logging his results. So far for chaliponga:
-Lime doesn't seem to work well, and doesn't even produce heat.
-Sodium carbonate yielded a very minute amount of powdery tannish fumarate, but the reaction had perhaps not reached completion.
-The limonene passed through the sodium carbonate basified paste precipitated a blackish goo, perhaps something that a defat would have gotten rid of; never-the-less, a good sign that the sodium carbonate had managed to break down the plant material.
-SWIM hasn't performed acidification as of yet.

SWIM's ideas for the next 50g (depending on the results of the first):
-Soak the pulverized material in vinegar and incubate in a crock-pot and dry in a food dehydrator.
-Defat with limonene.
-Basify with sodium carbonate.
 

Live plants. Sustainable, ethically sourced, native American owned.
 
amor_fati
#2 Posted : 11/3/2009 6:03:59 AM

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SWIM seemed to get a decent amount of fumarate from this, but it was flaky and unlike any fumarate SWIM's gotten before. Even after purification, it was still different. The freebase yield was gooey and difficult to weigh but was plenty active, though it was more difficult to smoke than the crystals SWIM's accustomed to smoking. SWIM ended up fairly swamped in his scheduling for the duration of his experiment and didn't take notes and ended combining the acid bathed-then-bassified material with the previously basified material. So he did manage to get something out of his process, but it was not quite what would be expected. His results remain inconclusive but with some indication of potential success.

He may try this on powderized mimosa soon. I'll broaden the title when does.
 
amor_fati
#3 Posted : 11/12/2009 5:58:40 AM

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SWIM's resolved to do some side-by-side experimentation with MHRB. Half of his MHRB is going to be extracted using Jorkest's method with lye, while 2/6 of his stock will A/B'd w/ vinegar and sodium carbonate and the remaining 1/6 will STB'd w/ lime. The only solvent used will be limonene. The results of each process will be compared to determine the viability of the methods in question.

The product from each will be purified with water using bufoman's method for further comparison. A sample of each will then be freebased with sodium carbonate, pulled with bestine and evapped to compare the final freebase product.

Finally the material used in the two nontoxic tests will be combined and basified with lye to determine what the nontoxic reagents were not able to retrieve.
 
endlessness
#4 Posted : 11/12/2009 10:27:33 AM

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hey fati, thanks for sharing the info!

Two questions... how are you going to yield the A/B dmt? Are you planning on evapping the limo, or pulling again with vinegar, evapping and pasting with sodium carbonate and then retrieving with IPA, or ?

Also, what is bufoman's water purification method, any link there?

Smile
 
biopsylo
#5 Posted : 11/13/2009 2:47:30 AM

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Quote:
Bufoman's Method of Removing Excess Fumaric Acid:

To separate the desirables from the fumaric acid one simply adds 12mL H2O per gram of material. (the DMT fumarate is soluble in the water while the fumaric acid is not).

The aqueous (now yellow) solution is carefully decanted into a clean beaker or drying surface.

The water is reduced by 1/2 with a hair drier and then allow to sit open to the air and slowly evaporate.

Within a day (at most) large transparent crystals will begin to precipitate out one can collect these. (If one does not care about ascetics the solution can just be rapidly evaporate with a hair drier or on the oven and the crystals utilized right away. However SWIM recommends the crystallization.)

The remaining solution is then reduced again with a hair drier and allowed to sit as before. Once it has fully evaporated the crystals can be collected.


i enjoyed this little tek. it was offered to me in the fumaric acid approach- fasw thread.
 
amor_fati
#6 Posted : 11/13/2009 3:07:47 AM

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This all essentially going to be like Jorkest's tek in that the product will be retrieved from limonene with FASW, but SWIM will be ammending nontoxic THP apporaches for half the stock to be extracted in order to determine what sort of a difference lye makes and whether it's worthwhile to do away with it altogether.

SWIM understands that with straightforward A/B (with lengthy, high-heat acid boils), nontoxic bases should work just fine, but SWIM isn't a fan of the odors from acid boils. For his A/B, he'll use a minimal amount of acid refluxed in a hot water bath, evaporate the acid, and basify with sodium carbonate. So for both nontoxic experiments, he use a minimal amount of water and have moist basified material in THP, which he will pass limonene through. Each amount of limonene from each sample will be kept separate and mixed with measured amounts of FASW.

After SWIM evaps the FASW, he will purify by placing the product (taking note of weight of product vs weight of fumaric acid used) in test-tubes, adding the minimal amount of water to pull fumarate without pulling fumaric acid. The water will be reduced by heat and air and then allowed to evaporate slowly in order to retrieve a nearly pure fumarate product.

Anyway that's the gist of it.
 
amor_fati
#7 Posted : 11/17/2009 5:49:04 AM

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No results on the nontoxic front quite yet--as SWIM's trying not to rush it--but he would like to mention that his lye extraction has yielded 6.5g from a 450mL sltn of aprx 3g of fumaric acid, so 3.5g of DMT from half a kilo so far. SWIM's relieved so far, since the bark hadn't been quite purple. Judging from the haste of this process, there's probably a good deal more in there. So SWIM knows that he should get at least a gram from each of the nontoxic experiments if they work out alright. Though the amounts aren't perfectly even between each sample, they're close enough for a judgment in the matter.

There are a couple things to mention on the nontoxic experiments: SWIM's opted for using lime on all three rather than sodium carbonate (he'll likely reserve this exclusively for freebase conversion from fumarate instead), since the bark isn't perfectly pulverized, otherwise SWIM has stuck with acid cook for the two and STB for the other one. The lime STB is yielding a polar substance along with the limonene, just as SWIM's seen in cactus extraction, so SWIM will likely separate this layer, mix it with some lime and put it back in THP. He's hoping it will stop cropping up, otherwise it may very well be oxidized DMT (he's guessing it's not, but if it is, this would be a decent way to isolate it).
 
amor_fati
#8 Posted : 11/23/2009 5:10:13 AM

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SWIM's making another change to the nontoxic experimentation, which merits another title change, I'm afraid. He took the jars he had done the acid/heat treatment on and mixed lime and water into the contents. Then he got a wild hair and decided to try blending the mixture in one of the jars, using the same method he used to pulverize the bark. First he decided to see if the blade assembly's material was resistant to limonene, which it seemed to be after pouring some in it for a while. So then he added some limonene to the jar and bleneded the whole thing. The result had the doughy consistency of hydrated and basified cactus material. SWIM's transfered the material to THP, and after he's washed it sufficiently with limonene, he'll have the results.

This particular experiment will take priority over the other two nontoxic experiments. If it works out well--as SWIM believes it will--he will use the same method on the other two, without limonene in the blender, and will have three variations to compare: Modified A/B blended w/ limonene, modified A/B blended w/o limonene, and modified STB blended w/o limonene. SWIM's hoping the third will be just as easy and successful as any of the others, as he'd rather not have to use vinegar. If any of these turn out well, SWIM's in the process of developing the easiest and most wholesome DMT extraction, yet.

So here's the rundown, so far:

What's needed:

1-Break up whole inner MHRB sufficiently to pulverize.
2-Add 100g to a regular-mouth quart jart. (SWIM's using an excess of 150g, but this is a bit much)
3-Attach blade assembly to the mouth of the jar and pulverize w/ blender. (this step may prove unnecessary, but SWIM will not be able to confirm it this time around)
4-Add 50-100g hydrated lime to the jar w/ sufficient amount of water to thoroughly moisten contents
5-Add an amount of limonene just short of filling the jar. (this step may be unnecessary but may prove beneficial)
6-Attach blade assembly and blend contents thoroughly until of a doughy consistency.
7-Prepare THP by cutting the bottom off a 32oz HDPE spray bottle, stuffing cotton balls in the neck loosely, and covering the nape of the neck with a few layers of cotton rag, and set the bottle in a clean regular mouth quart jar.
8-Pour the contents of the blending jar into THP and stir while allowing limonene to pass through into the collection jar.
9-Continue to pass limonene through THP until satisfied, adding more if necessary. (preferrably by pouring the limonene into the original blending jar and using it to collect any remenants into THP)
10-Collect product by FASW.

The advantages of this method would be a completely nontoxic extraction from whole MHRB without sacrificing yields, very contained and with a minimum of material, very little mess and simple multi-purpose use of household equipment.

If this works out as well or nearly as well as the lye extraction, SWIM'll author a proper tek based on his results.



Some news from the lye extraction:

After purification SWIM weighed about 5.2g, which would mean that his estimated amount of contained freebase would be less than the actual amount by almost half a gram. However, considering that the amount of fumaric acid added to the the water used for FASW was in slight excess of the proper amount needed for saturation, SWIM likely overestimated the amount of fumaric acid in the evap yield. So the yield from the first pull would be aprx. 0.8%.

SWIM saved 3g of the larger fumarate rocks and freebased the rest with sodium carbonate and a minimum of water. He attempted to forgo the use of acetone altogether, but soon realized after the first couple evaps (which he did in a shot glass at 29C in a food dehydrator within hours) that he needs to pull with larger amounts at higher temperatures evap over longer periods of time to do effectively. Unfortunately, he was pressed for time and went with the acetone to get the rest, but he managed a few rock-hard white crystals amounting to 60mg (the rest in the shot-glass didn't crystallize properly, so he just retrieved it with acetone). With the acetone, SWIM neglected dessicant, so some amount of impurities likely made it through, though no of them would be a problem; SWIM will likely purify with bestine anyway.

The first three photos are the first FASW evap from the lye extraction, the next three are the water purified fumarates, the next is 60mg of bestine evap crystallized freebase, and the next two are acetone evap freebase:
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Jorkest
#9 Posted : 11/23/2009 5:16:05 PM

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nice work dude!
it's a sound
 
amor_fati
#10 Posted : 11/23/2009 5:33:04 PM

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Back at you. Thanks for the tek!
 
Jorkest
#11 Posted : 11/23/2009 6:20:31 PM

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hehe! i just love experimentation...working with known techniques..finding kinks and making them work better...more efficiently...

endlessness and i have been talking about writing up a tek for a purely natural extraction tek...it would be the form of an A/B...using vinegar, d-limo, sodium carbonate, and water

we would use this tek..instead of using acetone to get the freebase spice

https://wiki.dmt-nexus.m...Fumarate_to_DMT_Freebase
it's a sound
 
amor_fati
#12 Posted : 11/23/2009 10:36:53 PM

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SWIM'll probably leave freebase conversion open-ended but include notes on possible methods and the toxicity and hazards of each. He would likely only touch on the use of sodium carbonate, and then refer to the use of acetone/dessicant, warm heptane, and Infudiblum's nontoxic method, as you referenced. SWIM's anxious to write a tek already, but he really wants to give it three trials to confirm its effectiveness and tweaks the particulars. He'll probably include a pictorial, as well. SWIM'll continue to edit it to include more specific amounts of materials after he has his results prepared and compared to your method.

SWIM hasn't had the greatest luck with sodium carbonate, but lime seems promising. Also, the difference between the consistency of the material when blended compared to without is quite vast, as well, and gives SWIM much more confidence in its potential. The blender seems to handle the material just fine, SWIM will find out just how much the limonene contributes to this (hopefully without burning out the motor); either way, using the limonene probably helps to improve the results of the first yield, due to such thorough mixing. SWIM's also hoping that the vinegar/heat didn't play too huge of a role in how easily it blended, as he would like to do away with that, altogether, in order to keep it simple and reduce time, work and odor.
 
Jorkest
#13 Posted : 11/23/2009 10:50:34 PM

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cool dude...cant wait to see how it all works out!
it's a sound
 
Phlux-
#14 Posted : 11/24/2009 7:28:26 AM

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did u modify the jar lid to hold the blending peice ? as per that old mycellial water tek ?
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...unlike the "blind leading the blind". we are more akin to a group of blind-from-birth people who have all simultaneously been given the gift of sight but have no words or mental processing capabilites to work with this new "gift".

IT IS ONLY TO THE EXTENT THAT WE ARE WILLING TO EXPOSE OURSELVES OVER AND OVER AGAIN TO ANNIHILATION THAT WE DISCOVER THAT PART OF OURSELVES THAT IS INDESTRUCTIBLE.


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amor_fati
#15 Posted : 11/24/2009 2:25:33 PM

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Nope, it fit perfectly as it was; no leakage or anything. Like so: http://dmt-nexus.me/forum/default.aspx?g=posts&m=90007#post90007
 
amor_fati
#16 Posted : 11/26/2009 7:16:08 AM

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SWIM just roped his failed chaliponga extraction into this: He put it to the blender and got it into THP--very gooey.

Sadness today, though. SWIM knocked over his separatory funnel and broke the top off of it (fortunately empty). This won't set him back in his progress, as he's got a gravy separator on the way. At least he'll be able to test his new methods using strictly household equipment.... This'll teach SWIM not to work on extractions while on psilocybe (http://dmt-nexus.me/forum/defau...ts&m=93727#post93727).
 
amor_fati
#17 Posted : 11/27/2009 1:26:27 AM

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SWIM's lye extraction may be getting close to exhaustion, so SWIM will test the pH, add more lye, and shake the hell out of it for a week. However, the first picture shows what SWIM got out of his second pull: The pile on the left is about 1.5g and the ball on the right is about 750mg, and since the amount of fumaric acid used couldn't be much more than 1g, that's a pretty good haul. So that supposed ~1.7g (from 2.250g fumarate) on top of the prior ~3.9g freebase (in 5.2g fumarate) is about 5.5g from 500g MHRB (over 1%!) The ball was incredibly dense, so he decided to put that with his purified fumarate (second photo), which he will further purify when he's finished with the lye. The pile was scraped up using acetone to facilitate, as it was very difficult; it was then dried and freebased. SWIM's collected that freebase w/ warm heptane.

Results are in for the nontoxic extraction! SWIM's first pull yielded 2g before purification, which should be about 1g of fumarate, though likely more. SWIM will purify this and will refrain from freebasing any of it until all nontoxic experimentation is complete. It should be noted that SWIM used a very small amount of limonene and unknown amounts of lime, so for his next pull, he'll blend in more lime and maybe use slightly more limonene. In regards to the amount, it represents that this method can pull the bare minimum of expected yield from MHRB (meaning it can likely pull more). Only ~150g of MHRB is in use, so aprx .5% was retrieved in the first pull. If it can pull at least the same amount on subsequent pulls, it'll be on par with the lye. Of course, SWIM won't know these numbers for sure until after purification. The last two photos show the unpurified fumarate yield.

The rest of the photos go into some detail of how SWIM's performing the extraction. One of the photos shows excess water that came through with the limonene: This happens with cactus extraction, as well, and can easily be separated out.
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amor_fati
#18 Posted : 11/27/2009 4:02:14 AM

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SWIM's now convinced that limonene is necessary in the blending stage after attempting to blend his other modified A/B jar without it. It seems to serve as a sort of lubricant enabling a more thorough blend. The material will eat the limonene; however, SWIM considers this a good thing, as it indicates even distribution of the solvent through the material. Adding more solvent and stirring should release most of the solvent, which would presumably be rich in alkaloidal content.

SWIM's thinking that his blending and lime content may not have been quite sufficient for the first A/B jar's first wash, but the second blend seemed much more thorough. Fortunately, his method makes this easy to fix. SWIM wishes he had some fresh bark to try doing all of the blending in one go with broken up bark, lime, water, and limonene, all at the same time. Next time, SWIM will also get himself a scale, capable of weighing the materials and try to devise a tek including adequate measurements.
 
Touche Guevara
#19 Posted : 11/27/2009 5:18:27 AM
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Amazing research.
 
amor_fati
#20 Posted : 11/27/2009 6:18:48 AM

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Yeah, Super Spice-o-Matic! Hours and hours glued to the Nexus certainly pays off.

Here's the final outcome: 1.4g purified fumarate (SWIM crystallized it kinda fast and funny, but it should be plenty pure), so that's a little over a gram in freebase--as SWIM anticipated.
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