No evaporation or freezing (In-progress)

[Ethnochemist]

So swim has been reading up on a whole bunch of teks, and swim feels that this is the best place to talk about it. Many questions.

69Ron posted a tek like so:

Here’s another option which gets out ALL the alkaloids.

This is the Dry A/B Acetone Tech, meaning there's no liquid/liquid extraction here. It's still an A/B extraction, but without a water phase and without emulsion trouble. And it’s so easy anyone can do it.

Dissolve the ground seeds in 4 parts acetone. Filter and discard the acetone (no actives get dissolve in it). Repeat this maybe 3 times.

Add 1/3 part sodium carbonate (not sodium bicarbonate) and enough water to make the seeds wet, but not watery, and mix for a few minutes. This freebases the alkaloids.

Add 2 grams anhydrous magnesium sulfate for every 1 ml of water used above. This chemically dries the material.

Extract with 4 parts acetone. Filter. Evaporate the acetone to get the alkaloids. Repeat maybe 3 times.

The thing swim does not like about this method is the evaporation stage, this is a lot of acetone. Everything else seems convenient and doable (since it avoids emulsions and such steps).

So swim wanted to find ways to avoid the acetone evaporation step. SWIM would like to just directly add FASA to the final acetone; however, it was mentioned somewhere on this forum that this may not be the most efficient method of precipitation. The actual FASA method suggests citric acid, and then the slow conversion to fumarate (so slow ). SWIM isn't sure if adding citric acid/acetone solution to the alkaloid-acetone and then FASA will precipitate all the alkaloids out any better than just FASA.

Another question: how pure can one get the DMT-fumarate when washing with acetone? And even if it's clean, the extract will still be sticky because of the oxides and j. spice when converting back to freebase, no? If so, maybe the zinc method could be incorporated somewhere in this tek.

Thanks,
E.C.

 

[amor_fati]

The thing swim does not like about this method is the evaporation stage, this is a lot of acetone. Everything else seems convenient and doable (since it avoids emulsions and such steps).

So swim wanted to find ways to avoid the acetone evaporation step. SWIM would like to just directly add FASA to the final acetone; however, it was mentioned somewhere on this forum that this may not be the most efficient method of precipitation. The actual FASA method suggests citric acid, and then the slow conversion to fumarate (so slow ). SWIM isn't sure if adding citric acid/acetone solution to the alkaloid-acetone and then FASA will precipitate all the alkaloids out any better than just FASA.

Firstly, total evaporation will simply yield all the alkaloids in freebase form, plus the N-Oxides. Evaporation of acetone is incredibly viable, though SWIM can see that evapping smaller amounts is preferrable. SWIM would think that evaporating the acetone to a smaller amount, rather than completely would be the best bet; it will be easier to go straight to the FASA method this way.

Secondly, SWIY's confusing one of the acetone-based extraction teks with the FASA method, as the FASA method is independent of--though integral to--those teks. FASA can be employed with A/B and STB teks.

Another question: how pure can one get the DMT-fumarate when washing with acetone? And even if it's clean, the extract will still be sticky because of the oxides and j. spice when converting back to freebase, no? If so, maybe the zinc method could be incorporated somewhere in this tek.

N-Oxides will not be present in the salt-product, but will remain dissolved in the acetone. Jungle-spice fumarate seems to precipitate more solidly than even pure DMT fumarate. Conversion of N-oxides is an option that will probably require full evaporation, rather than going straight to FASA. SWIM believes that this will require the incorporation of a secondary A/B procedure, but could be mistaken. After A/B extraction, FASA could be employed as long as xylene, toulene, or DCM is used as the NPS.

SWIM wonders whether zinc could be employed with citric acid added to the extraction acetone. The zinc could then be filtered and FASA could be utilized. SWIM's FOAF considered utilizing ascorbic instead of zinc, but it doesn't seem to be very soluble in acetone.

MHRB's yields tend to be satisfactory without N-oxide conversion, anyway.

 

[Ethnochemist]

Thanks for the reply.

Yeah, swim meant it in context of larger-scale extraction (at least a half kilo). Evaporating that much acetone causes a good amount of fumes.

But nonetheless, so swiy is saying that swim should concentrate the acetone first by evaporating, before adding FASA? Hmmm, swim figured that this might be necessary.

SWIM had another idea though, he remembers this from an old Salvia extraction tek.

Once swiy has the acetone=alkaloid solution, swiy could then add xylene. After a little mixing, swiy would then add water to make the layers separate. SWIM does understand that this totally defeats the purpose of having a non-liquid/liquid extraction method, but maybe due to the MHRB-acetone washes at the beginning, the chance of an emulsion would be very low.

SWIY would then do as many Xylene pulls as necessary and then employ FASA. (SWIY would know when to stop since alkaloids would stop precipitating from the Xylene.


---

Thanks for the info on the zinc and N-Oxides. But swim is wondering, in a general context, after enough acetone washes of the fumarate salts, and then conversion to freebase, how is the product? Sticky? Farely pure looking crystals? or more the typical yellow?

Thanks,
E.C.

 

[Infundibulum]

Hi Ethnochemist,

But nonetheless, so swiy is saying that swim should concentrate the acetone first by evaporating, before adding FASA? Hmmm, swim figured that this might be necessary.

There is absolutely no need to concentrate the acetone. FASA will salt the alkaloids and insoluble as they are they will fall out no matter the acetone volume.

SWIM had another idea though, he remembers this from an old Salvia extraction tek.

Once swiy has the acetone=alkaloid solution, swiy could then add xylene. After a little mixing, swiy would then add water to make the layers separate. SWIM does understand that this totally defeats the purpose of having a non-liquid/liquid extraction method, but maybe due to the MHRB-acetone washes at the beginning, the chance of an emulsion would be very low.

SWIY would then do as many Xylene pulls as necessary and then employ FASA. (SWIY would know when to stop since alkaloids would stop precipitating from the Xylene.

Salvinorins are not alkaloids. It is more of a diterpenoid. It has not a single nitrogen atom, so it cannot be ionised or form salts or anything like that.

What you propose with the xylene and acetone and water seems to have little logical coherence. Just add FASA in the acetone that has the freebased alkaloids, it's way faster and 100% reliable. Only the alkaloids will be salted out and they will precipitate. Why bother with all useless procedure you mentioned?? It would only make sense if you were afraid that addition of FASA in the acetone pulls would not precipitate the alkaloids (I guess SWIYs' fear is that too much acetone will hinder precipitation). Which is not the case, so do not make it unnecessarily complicated:wink:

Then SWIY can reuse the alkaloid-depleted acetone for the subsequent pulls.

 

[Jorkest]

the fumaric salts are extremely pure..there are no oils or fats in them..very pure...but there is most likely a mix of alkaloids..but its snow white...kinda looks like salt

 

[amor_fati]

Good to know, Infundiblum. SWIM never considered that the same acetone could be reused. SWIM supposes that in larger volumes, the potential for residual fumaric acid would be quite diminished. SWIM was thinking of the anadertha extraction tek which recommends reducing the amount of acetone before salting out the alkaloids. SWIM might've ended up wasting considerable amounts of acetone, had he not been informed.

 

[Ethnochemist]

Thank you for the excellent responses guys. Very appreciated.

Yes, swim knows that Sal-A is not an alkaloid. The point of the Xylene trick was under the assumption that the Fumarate salts would not precipitate in acetone alone...as was a doubt in some post on this forum.

Glad to know that the fumarates will precipitate no problem.

E.C.

 

[Ethnochemist]

Update:

swim is at the point where he filtered off the acetone from the sodium carbonate + mgso4 + bark. The acetone is greenish actually and there are a LOT of particles in the acetone. They do not seem to be settling.

SWIM does not want to add FASA and have to wash it with the green particles because it's not settling that well right now.

He's thinking about doing the xylene + water trick mentioned above....since that will instantly separate the particles from the xylene, which swim can't imagine being a very clear color either.

Just looking for some advice. Thanks,
E.C.


EDIT: Update: the stuff is actually settling....it's just taking a long while. SWIM will check up on it tomorrow...and siphon off the nice clearer layer. He'll then add the FASA and see where he is at that point, hopefully some pretty crystals will show up....that would make swim feel much better about the procedure so far.

 

[Ethnochemist]

So swim waited a day, the acetone was still a little cloudy, but a huge majority of it settled. So far, swim siphoned off about 40ml, then added 15ml of FASA. At first, only one of those dmt-fumarate "strands" formed...but after about an hour, dust started collecting at the bottom of the test tube. It's the same color as that lone strand of dmt-fumarate, but swim isn't sure if it's the same stuff (could it be fumaric acid?).

SWIM still has about 600ml of acetone solution left, so he's hoping for a somewhat decent yield.

He actually split his solution into three containers (two 100ml flasks and one 500ml). The 500ml solution settled a lot more junk, but the solution is much more cloudy and darker....maybe the yield from that one will be better.


SWIM's question though. The particles in the acetone technically shouldn't be there (sodium carbonate...mgso4..plant matter). This is why he's thinking about the xylene+water trick. If swim remembers correctly, after adding the water, the particles will stay in the lower layer, while cleaner xylene will sit on top. Maybe that only worked in swim's previous extractions, it's possible that the xylene will end up just as cloudy.

At this point, after precipitating the crystals, how could one separate the plant-matter/mgso4/Na2CO3 from the dmt fumarate? or could that trick come in handy.

E.C.

EDIT: Another update. So swim combined about 500ml of the solution into a 1L jar (it was pretty cloudy, can't really see through it. SWIM then added about 150ml of FASA, which produced a lot of crystals....not as many as swim was expecting, but they coat the bottom of the glass jar. SWIM is going to wait for them to settle now, give about 2-3 acetone washes, and check out the yield (this is only one run though...it might be less than 500mg (from 250g of MHRB), swim has yet to re-extract from the original bark though. A few more pulls will probably get the rest out.

 

[Ethnochemist]

Update. All crystals have been concentrated into a 50ml test tube and are now being washed.

Crappy cell-phone camera.

There's a large concentration of them at the bottom of the tube and they have a pretty strong amber tint, even after one wash. SWIM's starting to think that they won't be getting any whiter. Maybe this is the result from precipitating from acetone rather than Xylene.They also did not form any strand-like crystals, just dust.

Since this yield is a little lower than expected, swim is probably going to convert it all into freebase (swim is going to do an A/B + FASA tek starting tonight...he'll be able to compare the crystals tomorrow night).

SWIM feels that without better equipment (and time), this extraction has a lot of potential for yield loss. SWIY has to do a lot of pulls of everything to get all the alkaloids out, as opposed to an A/B, where swiy just pulls twice on the bark, and a few times with the NP solvent. No emulsions though, that's always good.

E.C.

 

[Ethnochemist]

Well, the acetone was a little brown, but figured it was enough washes anyway. Swim decanted as much acetone as possible, then put the tube in a boiling water bath to dry it all (took less than a minutes...awesome).

So he then used hot water to dissolve the brown sediment he just dried. The water turned black almost...and apparently all that brown stuff just settled to the bottom, he's going to wait till it completely settles, then he'll decant the fumarate-water, ditch the sediment, and basify the water to see if at least something freebases.

SWIM thinks it should because when he added the FASA a long time ago, he actually saw a bunch of crystals form and settle (not sure what they were, but he's praying that at least some of it was fumarate). SWIM will find out tomorrow if anything will freebase or not.

E.C.

Just for the record, the yield (if any at all) is tiny compared to the huge amount of crystals in swim's test tube from the A/B-FASA extraction.

 

[amor_fati]

Hmm, that's quite a strange yield. Could SWIY give a basic rundown of the steps taken and the amounts used? There are a lot of intricacies within this technique that may significantly reduce the yield, so be as precise as possible when listing the details of your procedure.

Also, was powdered MHRB used?

 

[Ethnochemist]

Materials: Powdered purple/pink MHRB powder (known to have a decent alkaloid content since swim extracted from it before). 100% acetone from lab store and Ace Hardware Acetone.

FASA prepared using 100% acetone and Fumaric Acid. SWIM tried to do 618mg per 100ml, but that actually didn't even dissolve, crystals still sitting on the bottom. Nonetheless, it's saturated.

1. SWIM put 250g of the powder in a gallon wide-mouth jar. Added the Ace hardware acetone. Waited for it to settle a little. Filtered through a T-shirt. A lot stayed in the jar, but anything on the filter, swim just put back in the jar. This was repeated another 2 times.
2. Jar placed in boiling water bath so the acetone would dry.
3. Added about 100g of Sodium carbonate. Mixed. Then added water, wet but not watery...kind of like cookie dough. Mixed for a several minutes. It turned a light green actually, not the whole thing, but spots of it. Made a mistake here, didn't record how much water went in.
4. Made up for it by adding ridiculous amounts of MgSO4, probably around 600grams (swim thought he had about 300ml of water).
5. Added 100% acetone (about 4 parts by volume). Filtered through a T-shirt.....this took a very long time. Brown acetone.
6. Added FASA to the acetone. Went off like a snow-globe. Waited for them to settle. Decanted the acetone, and transferred into a 50ml test tube.
7. Washed twice with acetone.
8. Decanted acetone, dried the precipitate on the bottom in a boiling water bath (made a cup of tea without the tea haha). Brown, dirt-looking precipitate.
9. Dissolved it in the same tube with hot water.
10. Today...swim's looking at it, there is a lot of stuff that settled to the bottom, brown dusty junk. The water sitting on top of it is also brown-ish.

At this point swim will save the water, get rid of the sediment (would have dissolved if it were good stuff). Then swim will just basify the water. And see if any crystals form. SWIM expects at least something.

SWIM can point out a few possible things wrong. For one, the filtering was done outside, and it was pretty humid. Wouldn't be surprised if at least some water got in...yet still, not enough to lose such massive yields. SWIM also only did one pull on his MgSO4-plant-Na2CO3, he probably should have done several, but 100% acetone is expensive, swim just wanted to gauge how effective this method was. Also, swim could have used a better filter, but he does not have a vacuum or a good buchner funnel. SWIM is sure this would have been much more effective.

E.C.

 

[amor_fati]

Materials: Powdered purple/pink MHRB powder (known to have a decent alkaloid content since swim extracted from it before). 100% acetone from lab store and Ace Hardware Acetone.

FASA prepared using 100% acetone and Fumaric Acid. SWIM tried to do 618mg per 100ml, but that actually didn't even dissolve, crystals still sitting on the bottom. Nonetheless, it's saturated.

SWIM is assuming that the all of the acetone used in extraction and FASA was dried with MgSO4? SWIM can't vouch for the purity of ace's acetone and doesn't know where to confirm it, unfortunately.

3. Added about 100g of Sodium carbonate. Mixed. Then added water, wet but not watery...kind of like cookie dough. Mixed for a several minutes. It turned a light green actually, not the whole thing, but spots of it. Made a mistake here, didn't record how much water went in.
4. Made up for it by adding ridiculous amounts of MgSO4, probably around 600grams (swim thought he had about 300ml of water).

The amount of water used shouldn't matter so much as the consistency. If the material can be stirred without revealing any dry parts it should be thoroughly moistened. SWIM believes that there should not be an excess of water if the material can be squeezed without water running out of it, but this is really only necessary for reducing the amount of MgSO4 required to dry it. SWIM assumes MgSO4 was rendered anhydrous prior to use?

Was the material allowed to soak for about an hour or more before drying?

5. Added 100% acetone (about 4 parts by volume). Filtered through a T-shirt.....this took a very long time. Brown acetone.

How well was the material stirred into the acetone?

SWIM would worry about product getting caught in the t-shirt, so SWIM would probably do three washes of the bark and filter through the same spot on the filter before moving on to FASA.

6. Added FASA to the acetone. Went off like a snow-globe. Waited for them to settle. Decanted the acetone, and transferred into a 50ml test tube.

After the crystals settled, did SWIY attempt adding more FASA to the solution to see if anymore precipitation would occur?

7. Washed twice with acetone.
8. Decanted acetone, dried the precipitate on the bottom in a boiling water bath (made a cup of tea without the tea haha). Brown, dirt-looking precipitate.
9. Dissolved it in the same tube with hot water.
10. Today...swim's looking at it, there is a lot of stuff that settled to the bottom, brown dusty junk. The water sitting on top of it is also brown-ish.

At this point swim will save the water, get rid of the sediment (would have dissolved if it were good stuff). Then swim will just basify the water. And see if any crystals form. SWIM expects at least something.

SWIY should try dissolving the sediment in fresh water just to ensure that it's not fumarate.

SWIM can point out a few possible things wrong. For one, the filtering was done outside, and it was pretty humid. Wouldn't be surprised if at least some water got in...yet still, not enough to lose such massive yields. SWIM also only did one pull on his MgSO4-plant-Na2CO3, he probably should have done several, but 100% acetone is expensive, swim just wanted to gauge how effective this method was. Also, swim could have used a better filter, but he does not have a vacuum or a good buchner funnel. SWIM is sure this would have been much more effective.

SWIM's never used lab-grade acetone and only used kleanstrip brand, as it reportedly contains 95-100% acetone with the the potential 5% impurity being water. SWIM dries his acetone with anhydrous MgSO4 prior to use. SWIM wouldn't be surprised if water contamination was present, considering the conditions.

 

[Ethnochemist]

Yeah swim added excess FASA and no he did not dry out the Ace acetone with MgSO4 (and yeh it was epsom salt baked in an oven at 500F for 3 hours).

It was most likely the basifying step. SWIM should have waited longer, he only waited for a few min. He also might have wanted to add more water. SWIM really didn't like the T-Shirt business anyway. Too much of a mess. A/B extraction is definitely better practically (as long as swiy has something like a hot bath to help with emulsions).

But if swim had a big buchner funnel, a vacuum, and some decent filter paper, he would be all over this procedure. Not only that, with a large funnel, for the parts where swiy has to extract or wash with acetone several times, swiy can just add it to the funnel while the plant is still on the filter paper. It would have made things so much easier this way. But swim doesn't have much space or money for equipment .

SWIM still has about half kilo of MHRB....he has plenty of material to work with, he might do this procedure on a smaller scale in the future.

E.C.