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FASA alteration of final purification Options
 
bufoman
#1 Posted : 4/27/2009 9:35:17 PM

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One thing a buddy had reported is that the FASA method results in a product highly contaminated with fumaric acid. This was confirmed by TLC and other tests. Fumaric acid is only very weakly soluble in water whereas the DMT fumerate is soluble enough. Thus rather than doing several acetone washes at the end one can just extract the white crystals with a small amount of water to remove the desired compound and leave behind the unionized fumaric acid. Carefully decant the liquid off and then just evaporate the water to get the product. Maybe do one more water wash just to be safe.

Of course this takes longer to evaporate the water however the product will have minimal fumaric acid whereas even with severeal acetone washes a large fraction of the product can be fumaric acid crystals. Also one does not have to use very much water as DMT fumerate is water soluble I do not know the exact amount however. i have heard that 69ron (although i did not read this myself) said it is not very soluble however I disagree I do not know the exact amount but pure DMT fumarate does dissolve in water. DMT fumarate is commonly used for IV injections in the scientific literature. SWIMs experience would confirm this high soluability. I was unable to find any info on DMT fumarate solubility if anyone knows it that would be great. It could be used to figure out the exact amount of water needed. But do not calculate the solubility on your own from your FASA because it will be impure and contaminated with undissolved fumaric acid!!! Anyone who would do this would think it was very weakly water soluble.

One could also add a base and extract the freebase with an organic solvent.
 

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bufoman
#2 Posted : 4/28/2009 10:38:58 PM

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One thing SWIMs foaf noticed was that the initial crystals that crash out have less unreacted fumaric acid (unionized) but as they collect overtime the ratio of DMT fumarate to unionized fumarate becomes less. This method works much better than the acetone washes as a lot of acetone will have to be used to adequately remove all of the fumarate where as a relatively small amount of water is need to dissolve the desired product.


 
memo
#3 Posted : 4/28/2009 11:21:26 PM

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Although SWIMs dmt Fumarate may be highly contaminated with Fumaric acid it is a non-issue for him. The Fumaric acid that SWIM uses to make FASA is from dietary supplement capsules, 500mg pure Fumaric Acid per capsule. He only adds enough FASA to acetone until he stops getting precipitates. Since he only uses the Fumarate for pharmahuasca and storage purposes it seems like a non issue to him. 50mg of product is a strong pharmahuasca dose when combined with 200mg harmalas. For storage purposes any extra Fumaric acid will be left behind when converting back to freebase. Unless you need it very pure for I.V. or something like that is shouldn't be too much of an issue. Although he guesses that depending on the proceedure that you use the amount of Fumaric acid contamination could vary.
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bufoman
#4 Posted : 4/29/2009 1:55:42 AM

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It is nice to know how much of the actual compound SWIY has extracted and how much SWIY is going to ingest. Depending on a variety of factors that arise during the extraction such as pressure, temperature, concentrations, ... the amount of fumarate present in the final product could vary significantly. It can be some what high especially if one collects the crystals that settle out after the first few hours. however there is still good product that settles out even after a day or two. If one wishes to purify this they can with a small amount of water.

For converting to the freebase of course it doesn't matter but for snorting, IM injection, IV injection or even taking orally SWIM would assume many would prefer to have a clean product at least so they can know the dosage they are taking.

BTW Strassman used DMT fumarate IV in his clinical studies on DMT.
 
memo
#5 Posted : 4/29/2009 2:07:21 AM

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I see what you are saying, and it is good to know how to clean it up if that is desired.
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bufoman
#6 Posted : 4/30/2009 8:22:41 PM

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SWIMS friend has reported that if one allows most of the water to evaporate off from the water extraction and then let the solution get cold (in refrigerator or outside). Large transparent beautiful crystals were form. Some form clusters and look like little chunks of rock candy.
 
bufoman
#7 Posted : 5/1/2009 3:01:04 PM

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Here is the final tech although as with any it is always open to modification. This really works well to clean up your product and the resulting crystals are beautiful. NE SWIMS with friends that have FASA product sitting around should tell them to give it a shot. They will not be disappointed. If your product is fully water soluble it means that the acetone took out all the fumaric acid but this is unlikely unless you used a lot and let it sit. Here is the Tech

Once one has collected the white-offwhite crystals that have collected on the bottom and inside of the jar. They are placed in a clean beaker. (These crystals contain both DMT fumerate and a large portion of unreacted 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 that collect can be collected.

One now has highly pure DMT fumarate. The crystals are very nice to look at. One can attempt to wash the fumaric acid crystals again with an additional 10mL of H2O to see if any crystals are obtained however due to its solubility most of the DMT fumarate will collect during the first attempt.
 
extrememetal43
#8 Posted : 5/5/2009 4:01:35 PM
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is it any good at removing impurities aside from fumaric acid. a buddy had 1.5 g's of yellow freebase and upon conbersion to fumerate ended up with 1.1 g equivalent so he lost 27% alred in impurities but the fasa crystals are not white at all. will this remove additional impurities?
 
amor_fati
#9 Posted : 5/5/2009 4:45:45 PM

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extrememetal43 wrote:
is it any good at removing impurities aside from fumaric acid. a buddy had 1.5 g's of yellow freebase and upon conbersion to fumerate ended up with 1.1 g equivalent so he lost 27% alred in impurities but the fasa crystals are not white at all. will this remove additional impurities?


Yikes, SWIM would worry about water contamination. Did SWIY make sure that he reacted all of the product that was dissolved dissolved? It can be tricky sometimes. It should turn out about 1/3 heavier. SWIM's product from MHRB, once converted from fumarate to freebase, is yellow because of the jungle spice.
 
bufoman
#10 Posted : 5/5/2009 8:10:58 PM

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There is no evidence that through FASA there are any impurities. In fact some MS and chromatography analysis of the FASA fumarate products show only DMT.

How did SWIY's buddy convert it to fumarate? If one makes DMT fumarate correctly from freebase there is no need to do this water wash as there should not be any excess fumaric acid. However they can use this tech to re-crystalize the fumarate salt to get nice crystals. Just follow the tech to get nice transparent crystal clusters.

The whole Jungle spice myth is highly questionable. At first SWIM was very fascinated by the whole thing. However everyone who has performed MS on the extract has found it to be mainly DMT with a few minor impurities. If one continues to extract from the orange/red "jungle spice" with hot hexanes they can continue to pull nice white DMT crystals. This can be repeated many times until there is almost nothing left over aside form some oily residue which still shows mainly DMT via MS. This residue may be a small amount of high MW products. If some one thinks that they have a lot of JS it is most def mainly DMT that they have not yet crystalized. keep extracting. That said diff sources of bark may have diff components but several diff people have looked and found mainly DMT. Many people have assayed these extractions. Just continue to extract the JS with hot hexanes and place the hexanes in the freezer you can convert almost all of the "JS" into white crystals of pure DMT. The true orange oily "JS" that results is active and different from DMT however its MS results show that it contains mostly DMT or a High MW component that gives DMT upon fragmentation.

There is no doubt that the JS experience is different than pure DMT however that JS most people have is still mainly made up of DMT with a few minor additional alkaloids. So this small amount of other alkaloids very likely potentiates the DMT in the mixture. But these are minor minor alkaloids.

 
amor_fati
#11 Posted : 5/5/2009 8:43:52 PM

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The jungle-spice can still discolor spice and disrupt the crystal structure to yield a yellow wax, rather than clear or yellow crystals. SWIM's separated jungle-spice from pure-spice so that he has nearly pure spice and nearly pure jungle-spice, and there's quite a huge difference between the two. The JS is nearly inactive on it's own but definitely effects the activity of DMT. And there's definitely enough JS in mimosa to impact a straight mimosa extract (toulene or xylene extracted and preciped with FASA). The activity and physical structure of the freebase yielded from this is far different than that yielded from naphtha.
 
extrememetal43
#12 Posted : 5/6/2009 1:56:37 AM
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my buddies work was converted from freebase done with naptha, very yellow to start...no water in acetone. it has a definite yellow to it before and after the conversion iy was an off white. it was like 1.5 fumerate which is 1.1 freebase. it was thouroughly salted. it had beautiful crystals but not white but the crystal structure was the best ive ever seen.
 
bufoman
#13 Posted : 5/6/2009 2:04:43 AM

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Take the JS and extract it with hot hexane or naptha then place this in the freezer to decrease solubility and induce crystallization. this needs to be done 5 -10 times to remove all of the N,N. The resulting oil JS will still be largely residual DMT or a high MW component which gives DMT on ionization (unlikely). The left over true JS will be a relatively small amount (not super low but only a hundred mg or so per pound bark) and when it is evaluated via MS it will be largely DMT with a few high m/w components. Some sources may have higher amounts of N-oxide and thus may appear to be larger amount of JS but this is just N-oxide not the other compounds. Admittedly it is hard to do this research because the accuracy of the MHRB is unknown. However SWIMs have noticed that what most people call JS is mostly DMT. Most people only do 1 or 2 pulls on it. Do 5-10 hexane washes and see how little of the true JS is left. Also TLC shows three components to the JS. the major being DMT or a component with the same RF unlikely in light of the MS data.

SWIM knows that their is truth to the JS but what most people call JS is mostly just DMT with a small amount of other compounds. These may or may not alter the activity of DMT. SWIM as do many others think they def do however they are very minor components.
 
bufoman
#14 Posted : 5/6/2009 2:07:32 AM

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If fumarate is crystalized properly the crystals are beautiful. The FASA crystals are impure and are typically not that ascetically pleasing. Extracting and re-crystalizing with water will fix this.

if one crystalizes the FB slowly they can get some nice big beautiful clusters. I have seen some beautiful pics on this website of peoples crystallizations. Crystallization is truly an ART.
 
Infundibulum
#15 Posted : 5/6/2009 3:40:23 PM

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bufoman wrote:
SWIM knows that their is truth to the JS but what most people call JS is mostly just DMT with a small amount of other compounds. These may or may not alter the activity of DMT. SWIM as do many others think they def do however they are very minor components.

This is what SWIM's friend believes ("believe" as opposed to having firm evidence); his JS preparation was washed 100s of times to get rid of the vast majority of dmt. A preparation of 10mg of the latter JS was very very inactive. But a 30mg pure dmt dose 10min after the failed JS launch was experienced as an surprisingly strong dose. This type of experiment (smoking JS and then dmt) was consistent for SWIM.

SWIM believes that the JS contains some modifiers that can modify the experience when smoked in very small amounts.

It's also very nice to see that other people are reaching to similar conclusions, thus giving a better understanding of the JS enigma.

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amor_fati
#16 Posted : 5/25/2009 7:16:49 AM

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Hey bufoman, this method worked great for SWIM! His product is a bit sticky, though, but quite solid. SWIM was wondering if SWIY knows a good way to reduce the stickiness?
 
amor_fati
#17 Posted : 5/26/2009 4:25:06 PM

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Ahh, SWIM just stretched it out and let it sit, and it's no longer sticky. The volume of the product has significantly decreased, though the weight is much the same. It's definitely the consistency of hard rock candy. Thanks, Bufoman!
 
bufoman
#18 Posted : 5/27/2009 5:26:46 AM

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No prob man it does work great. SWIM noticed that the initial large rock candy crystals should be separated before all the water evaporates like a true crystallization. The last bit of water likely contains some impurities N-oxides ??? and thus is initially oily but does solidify but not as easily, it also may not be as pure. If one has a lot of this they should re-crystalize this residue in water as well but there will always be some waxy residue in the last of the water. SWIM's friend just keeps this separate from the nice crystals
 
Phlux-
#19 Posted : 5/27/2009 3:49:49 PM

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fumaric acid is soluble in water see my post - http://www.dmt-nexus.me/...aspx?g=posts&t=2883
and the fasw in jorkests new tek
guess not as much as its soluble in acetone
swim intends to try this tek very soon and will post pic of these nice xtals.

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amor_fati
#20 Posted : 5/27/2009 5:05:57 PM

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I think the point is that the fumarate is much more soluble than the fumaric acid, so a little bit of water will dissolve the fumarate, but not the fumaric acid (I'm not positive on this: but I believe the fumaric acid would be even less soluble in a solution of the fumarate, much like harmaloid HCls in salt and vinegar solution). SWIM had fumaric left over in his test-tube and retrieved the expected amount of fumarate. SWIM believes that the fumaric contamination probably doesn't effect the weight so much as the taste and consistency of the crystals.
 
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