Discussing Alternative Spice Extraction Techniques

[Infundibulum]

Hi all,

SWIM has made some interesting observations lately regarding the solubility of dmt fumarate in acetone (basically it is totally insoluble) and this initiated some nice discussions with 69ron on the Pure DMT Fumarate from freebase DMT topic, which led to the consensus that other extraction teks can be developed using less toxic materials and abolishing (or minimising) the use of non-polar solvents.

The different theoretical teks proposed so far are:

1 - Mix powder mimosa with 1 part calcium hydroxide.
2 - Add enough water to make it wet and mix. It should be like wet clay. (This freebases the DMT)
3 - Spread it out and let it dry completely.
4 - Dissolve it in acetone and filter out the solids. (Freebase DMT and other junk dissolves into the acetone)
5 - Saturate the acetone with fumaric acid.
6 - DMT fumarate precipitates out of the acetone. (Some other junk might also precipitate out the first time)
7 - Mix DMT fumarate with 1 part calcium hydroxide.
8 - Add enough water to make it wet and mix. (Freebase the DMT again)
9 - Spread it out and let it dry completely.
10- Dissolve it in acetone and filter out the solids. (At this point only alkaloids like DMT should dissolve)
11- Evaporate the acetone to get nearly pure freebase DMT.

and

1) acid extraction of MHRB. Your acid is FUMARIC ACID, so you convert all dmt to fumarate salt
2) boil down the extracts to a very very low volume.
3) add excess of acetone and cause precipitation of fumaric acid and DMT fumarate
4) collect precipitate and freebase it

Or:

1) extract MHRB with acetone and filter off all pieces. (soxhlet should work miracles here)
2) (optional)evap to a managable volume.
3) add excess fumaric acid.
4) see the beautiful precipitate falling.
5) freebase it

The idea of this topic is therefore to gather individuals' observations, ideas and propositions so that other experimenters can read them, comment on them or avoid doing them if negative feedback from other people is given.


SWIM's latest observations regard:

A) The formation of fumarate salt of the other MHRB alkaloids aka jungle spice;
SWIM did a STB on MHRB, pulled with naptha + collected the dmt, then did 3 xylene pulls which were evaporated down to a thick oil with strong indole smell. SWIM couldn't wait for the ages it usually takes for this oil to get solid; SWIM mixed this oil with fumaric-acid saturated acetone (FASA) and converted all of the alkaloids to the fumarate salt which quickly precipitated, leaving behind an acetone containing lipid impurities. When the latter acetone was evaporated, a yellowish lipid layer was left with no indolic smell. SWIM thinks to try snorting the jungle spice fumarate as well as freebasing it.

B) FASA was added in both naptha and xylene pulls from Diplopterys cabrerana after A/B extraction causing the salted alkaloids to precipitate. FASA was added until no more precipitation formed. Precipitates were collected and naptha and xylene containing FASA were washed in excess water to remove the residual fumaric acid and most of the acetone and were re-used for further pulls. Now SWIM uses the same ~100ml of non-polar solvent again and again until no further fumarate salts precipitate after FASA addition.

Now SWIM plans to freebase the fumarate salts in the following way:
1) dissolve them in the minimum amount of water possible
2) dropwise add water saturated with sodium carbonate so that freebases precipitate
3) collect the freebase precipitates


Any ideas / suggestions are only helpful!

 

[amor_fati]

SWIM's third pull yielded 44mg, for a total of 212mg of tentatively estimated 230mg. SWIM considers this adequately successful.

Both batches of jungle-spice mentioned above seem to be decently active, though the batch collected from the aqueous solution is a bit more oily than that collected from acetone evap. SWIM is considering dissolving the oily batch into acetone in order to achieve a dryer yield.


SWIM is also considering the possibilities of minimizing one's DMT analogue extraction kit to this:

Half-gallon Jug of Anhydrous Acetone
Half-gallon Jug of CASA (Citric Acid Saturated Acetone)
Bottle of FASA (Fumaric Acid Saturated Acetone)
Naphtha (for separating spice from jungle-spice)
DCM (for pipe cleaning)
Sodium Carbonate
Lime
Distilled Water
Non-Iodized Table Salt (as desiccant)
Epsom Salt (for drying acetone)
1Gal Jar w/lid (for MHRB extraction)
Salting Container w/ Lid
Freebasing Container
Freeze-Precip. Container w/ Lid
Evaporating Dish
Pipettes
Spatula/Stirrer

 

[513orangejuice]

sea salt would be fine too, right?

 

[amor_fati]

Maybe, but why bother? Sea salt contains substances other than sodium chloride, and SWIM would rather not have to account for those elements. Salt is a very neutral component of this process, so any additional factors may make it a little less neutral.


So Infundibulum, SWIY got a 1% yield with SWIY's tek from drugs-forum? SWIM was thinking it would possibly boost the yield to replace step 7 with the method SWIM's been using, considering how difficult and messy step seven seems to be. This would be a superior and incredibly straight forward tek if it proves a consistently high yield. One could also cease the process after the fumarate conversion, and convert to freebase as needed. And of course, it wouldn't be difficult to separate the pure spice from the jungle-spice with a simple naphtha wash. The time factor seems like a minor nuisance, as much of that time is spent waiting rather than spent on work.

Could this be the future of spice extraction? SWIM thinks that within two years, this or a related tek may be the primary way these extractions are performed. And by the way, SWIM's grown quite fond of acetone.

 

[Infundibulum]

Yep, step 7 is definitely a pain in the bum! freebasing using the calcium carbonate (or calcium hydroxide) paste is a much much better approach! SWIM can't wait to get back to experiments, he;s too busy at the moment to do this kind of stuff...SWIM also wants to try using glacial acetic acid (=100% acetic acid) instead of citric acid in the first step of extraction. But how many can get their hands on glacial acetic acid??

 

[513orangejuice]

DAMNIT SWIM went out and bought some free flowing salt, without iodide. Kroger brand. Then SWIM gets home to sit down and read the ingredients, and finds Sodium silicoaluminate(Anti caking agent). After first purchasing rock salt, for making ice cream, that ended up looking like gravel with rocks in it. lol SWIM wonders what would be the right brand of pure salt and where to find it?...

 

[amor_fati]

SWIM's contains calcium silicate, which is also an anti-caking agent. It acts as a desiccant, so it shouldn't be a problem.

 

[513orangejuice]

Ok, kewl. SWIM has a vendeta against those anti caking agents, tho. Every thing SWIM buys has one it in. From citric acid to salt,...

 

[elmictlan]

Hello all my first post

Everything here is imaginery SWIM has a very active imagination: SWIM is very interested in this technique SWIM tried it but failed <CASA + FASA>. SWIM allowed acetone to evap leaving what SWIM thought was C-A+SPICEFUMERATE, SWIM was upset with this but could only blame himself, the resulting mixture was collected and dried and looked and tasted very much like CA SWIM is a brewer and is familiar with the taste <only a tiny quantity was tested SWIM has heard CA od is not a pleasant experience> SWIM then washed this with acetone to try and dissolve the CA and in SWIM'S knowledge leaving the spice fumerate which is insoluable in acetone, SWIM's mixture tasted very different still acidic but not citrus like. SWIM was unhappy with purity though and did not decide to attempt a freebase although SWIM later decided that this would have been a good idea. SWIM believes you may be able to help him answer a few question so that further experiments can be carried out with hopefully more positive results <SWIM is a scientist and understands negative results are still good results and can be learned from and has>.SWIM will list the questions any insight will be greatly appreciated and further posts of results will come:
1. The suitable ratio of MHRB:CASA as not to waste acetone?
2. The suitable ratio of CASA:FASA as not to waste acetone?
3. Swim assumes acetone is to be sealed so no evap occurs is this correct?
4. Would someone explain a good filter method SWIM used a vinbrite wine filter which worked well but SWIM realised it is made of plastic would some also be able to supply a list of suitable plastics for use with acetone?

Thank you very much SWIM looks forward to reading any replys.
ELMICTLAN

 

[swam rollbre]

SWIM's FOAF posted this on Drugs forum, but it was intended for the Nexus, which, at this time was down without any hopes for resurrection:

Hi all,

SWIM's FOAF would like to share his experimental observations on novel ways of spice acquisition. In a way it is a follow-up from the ceased dmt-nexus forum where similar discussions were held. SWIM's FOAF has been able to extract dmt from MHRB using just water, acetone, citric acid, fumaric acid and sodium carbonate.

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.


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

Control: If no fumaric-acid saturated acetone is added in the citric-acid saturated acetone extract (step 4) NO precipitates are seen after 3-4 days. This suggests that the precipitates are the fumarate salt of "some kind" of alkaloid.

Considerations:

3) this method definitely takes ages; it relies on the acetone insolubility of the alkaloids' fumarate salts. The rate limiting step is the conversion of alkaloid-citrate to alkaloid-fumarate. This problem could be overcome IF one was using an acid weaker than fumaric acid. This acid must be available in relatively anhydrous form (like the case of citrc and fumaric acids) and must be dissolvable in acetone. A good candidate could be glacial acetic acid (=100% acetic acid) since it has a pKa of 4.75 and is therefore weaker than fumaric acid. But not everybody can get glacial acetic acid easily (as opposed to teh other chemicals used in this method).....

Any suggestions / corrections and improvements are more than welcome!

can anyone explain why the supposed dmt-tannate would convert to dmt-citrate, and especially why the citrate would slowly covert to dmt-fumarate? i grok the "sink" effect and all, i just don't see why the goodies wouldn't just ignore the fumaric acid altogether and remain citrate indefinitely....
has there been any follow up n this? anybody adopt this as their default extraction process?

[also, when was the nexus down with no hope of recovery?]

thanks! live in love

 

[GreenDMT]

Hi all,

SWIM's FOAF would like to share his experimental observations on novel ways of spice acquisition. In a way it is a follow-up from the ceased dmt-nexus forum where similar discussions were held. SWIM's FOAF has been able to extract dmt from MHRB using just water, acetone, citric acid, fumaric acid and sodium carbonate. The purpose of sharing such experimental results is immensely useful because they can build platforms onto which others may be able to add ideas and (hopefully!) resulting in faster, more efficient, more clean, and more eco-friendly teks.

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.

Control: If no fumaric-acid saturated acetone is added in the citric-acid saturated acetone extract (step 4) NO precipitates are seen after 3-4 days. This suggests that the precipitates are the fumarate salt of "some kind" of alkaloid.

Considerations:

1) In a pilot experiment of SWIM's FOAF just acetone was ued for the initial MHRB extraction. Addition of fumaric acid saturated acetone did not produce any precipitates immediately and on the other hand this silly guy did not wait for few days to see if anything precipitates.

2) Step 7 can be tricky. Sane humans would most likely go for an already tested A/B extraction using small quantities of a NP solvent.

3) this method definitely takes ages; it relies on the acetone insolubility of the alkaloids' fumarate salts. The rate limiting step is the conversion of alkaloid-citrate to alkaloid-fumarate. This problem could be overcome IF one was using an acid weaker than fumaric acid. This acid must be available in relatively anhydrous form (like the case of citrc and fumaric acids) and must be dissolvable in acetone. A good candidate could be glacial acetic acid (=100% acetic acid) since it has a pKa of 4.75 and is therefore weaker than fumaric acid. But not everybody can get glacial acetic acid easily (as opposed to teh other chemicals used in this method).....

Any suggestions / corrections and improvements are more than welcome!

[/quote]

I was trying to do something similar, but my problem is somehow do not use acetone,to be eco friendly

 

[Loveall]

SWIM's FOAF posted this on Drugs forum, but it was intended for the Nexus, which, at this time was down without any hopes for resurrection:

Hi all,

SWIM's FOAF would like to share his experimental observations on novel ways of spice acquisition. In a way it is a follow-up from the ceased dmt-nexus forum where similar discussions were held. SWIM's FOAF has been able to extract dmt from MHRB using just water, acetone, citric acid, fumaric acid and sodium carbonate. The purpose of sharing such experimental results is immensely useful because they can build platforms onto which others may be able to add ideas and (hopefully!) resulting in faster, more efficient, more clean, and more eco-friendly teks.

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.

Control: If no fumaric-acid saturated acetone is added in the citric-acid saturated acetone extract (step 4) NO precipitates are seen after 3-4 days. This suggests that the precipitates are the fumarate salt of "some kind" of alkaloid.

Considerations:

1) In a pilot experiment of SWIM's FOAF just acetone was ued for the initial MHRB extraction. Addition of fumaric acid saturated acetone did not produce any precipitates immediately and on the other hand this silly guy did not wait for few days to see if anything precipitates.

2) Step 7 can be tricky. Sane humans would most likely go for an already tested A/B extraction using small quantities of a NP solvent.

3) this method definitely takes ages; it relies on the acetone insolubility of the alkaloids' fumarate salts. The rate limiting step is the conversion of alkaloid-citrate to alkaloid-fumarate. This problem could be overcome IF one was using an acid weaker than fumaric acid. This acid must be available in relatively anhydrous form (like the case of citrc and fumaric acids) and must be dissolvable in acetone. A good candidate could be glacial acetic acid (=100% acetic acid) since it has a pKa of 4.75 and is therefore weaker than fumaric acid. But not everybody can get glacial acetic acid easily (as opposed to teh other chemicals used in this method).....

Any suggestions / corrections and improvements are more than welcome!

Sorry for ressurecting and old thread. What ever hapened to this approach? I see it mentioned in this thread too, but that goes into A/B extraction.

I don't get why the citric acid is needed. Is the natural dmt salt is soluble in acetone? If not, why would addimg citric make it soluble? I guess citric may enhance solubility of the natural salt, but that seems unlikely. Seems like one needs to wait a few days and that may be why the first pilot experiment without citric did not work?

Also, some have seen dmt fumarate be soluble in PG.

If the natural dmt salt is soluble in acetone why not do this:

- Extract powdered bark with acetone (is the natural dmt salt soluble?) (e.g 100g into 800ml after 5 pulls)
- Add fumaric acid granules in acetone (more than enough to salt 3% DMT yields and staying bellow the 15mg/ml saturation (e.g 3g of fumaric in 800ml of extract)
- Wait a few days and hope DMT fumarate crashes
- Decant/rinse with fresh acetone/dry
- Dissolve product into two parts PG (should be soluble) and load into vape pen.

It cannot possibly be this simple, right? Guess it is worth a test to see what happens?

 

[Loveall]

- Extract powdered bark with acetone (is the natural dmt salt soluble?) (e.g 100g into 800ml after 5 pulls)
- Add fumaric acid granules in acetone (more than enough to salt 3% DMT yields and staying bellow the 15mg/ml saturation (e.g 3g of fumaric in 800ml of extract)
- Wait a few days and hope DMT fumarate crashes

I tried this yesterday with 10g of MHRB. I warmed the acetone in a hot water bath aslo. 18h after salting and seeing no precipitation of consequence. I will try to figure out where the DMT is, but maybe acetone alone does not pull the natural salt from MHRB.

 

[doubledog]

Freebasing is probably needed for this to work. Solubility of natural salt in (pure) acetone is most likely quite low.