Minimum Polymer

[Loveall]

After learning from the last data turn, gonna try this approach:

- De-polymerization of natural DMT (?): 100g root bark, microwaved with 300ml of a "strong" 15% citric acid solution till 100ml evaporate (about 100 minutes at 200W).
- Allow to cool, add ~100ml naphtha
- Slowly mix in ~500ml of 10% NaOH (try to avoid polymerization by giving DMT FB the opportunity to move out of the water as it forms and not reach a high aqueous concentration)
- Pulls/freeze precipitate

Are you going to include a filtration step in there? I'm interested in experimenting with this technique myself, but I learned the hard way that putting basified MHRB solids into my separatory funnel is really, really unpleasant.

Incidentally, it was during that same experiment that I found that after repeated citric acid cooks (3-4 washes at pH 2 and 80°C for a total of 6-8 hours), I could only recover a negligible amount of DMT from the remaining solids via STB. It's possible that it may have (re)polymerized per your hypothesis though.

Do you think adding salt late in the process and doing another pull could yield additional product, per Cyb's Max Ion? Maybe once the DMT is dilute enough in the aqueous phase, ionic strength overtakes polymerization as the limiting factor for additional yields.

Hi

No filtration, it all happens in a quart jar. Naphtha separates to the top and is pipetted. out.

Cyb's max ion is 5-6% NaCl I believe, which is not too hash, also since the DMT is diluted to <0.3% it could be fine avoiding polymerization. So yes, it could well be that ionic strength helps, and we have many successful max ion results from folks. It has worked well for me.

It's interesting because there is an interplay. When minimally polymerized (e.g. long acid treatment), the partition coefficient seems very good for white DMT. As it polymerizes (or of natural de-polymerization was not complete during the acid step), heat and ionic strength may become important (but too much ionic strength could become counterproductive if it begins to catalyze polymerization). Dry teks don't use salt and excessive polymerization could be why. I once tried a dry Tek with salt and got the reddest funkiest DMT I've ever seen. All this is hypothetical interpretation of observations since I can't actually measure DMT polymerization.

 

[Ruffles]

I might have missed the thread on the yellow goo being a polymer so I`ll just ask.

Where or what is the evidence that suggests the yellow goo to be a DMT polymer?

My (unevidenced) opinion is that the goo is just a pre-nucleation or a gel-like aggregation of DMT before it actually becomes a crystal. Goo always crashes first as the nps cools, then comes the white stuff.

There is yellow fumaric DMT goo as well. Assuming the goo is polymerization, what would that yellow fumaric goo be?

 

[downwardsfromzero]

There is spectrographic evidence of oligomerisation, but I'm damned if I know where to find it right now. Maybe in the morning, or by someone else with a direct clue.

Polymeric goo would, in principle, still be able to react with fumaric acid.

 

[Ruffles]

There is spectrographic evidence of oligomerisation, but I'm damned if I know where to find it right now. Maybe in the morning, or by someone else with a direct clue.

Polymeric goo would, in principle, still be able to react with fumaric acid.

What I mean by fumaric DMT goo is after adding FASA to loaded NPS, the first stuff that falls to the bottom is droplets-like of yellowish whatever, after more FASA it eventually turns to solids.

Let me put it in a question: does fumaric DMT polymerize?

 

[downwardsfromzero]

I think DMT fumarate would be unlikely to polymerise, but if DMT oligomers are in solution they may well precipitate first as a goo. Acetone is a far better solvent for DMT than naphtha is, so it would be likely that the DMT oligomers are far more soluble in acetone than in naphtha as well. It would be necessary to perform some careful tests on the gooey fumarate to ascertain how/if it differs from the crystalline material. I know the stuff you're talking about - it slowly crystallises of the course of a few days or more if the humidity is low enough. The fact that it is coloured suggests some kind of electronic interaction commensurate with polymerisation.

Did your fumaric goo eventually crystallise? If so, did its colour remain the same? If it lightens, this would suggest depolymerisation was occurring.

 

[Loveall]

Here is the evidence for polymerization/oligomerization (since we don't know how long the chains are we use both words).

DMT polymerization - Plant Analysis and Substance Testing - Welcome to the DMT-Nexus

Main evidence is Benzyme's mass spec with multiples of 188 for goo (red in his case). Based on this, Jess was able to get xtals from goo, and I roughly repeated his work to confirm with a long organic acid step of high concentration (15%) that was magnetically stirred for a while. Time and concentration helped, as a quick mild acid step kept the polymer mostly intact.

 

[Ruffles]

Did your fumaric goo eventually crystallise? If so, did its colour remain the same? If it lightens, this would suggest depolymerisation was occurring.

Yes, it all eventually crystallizes. Fumaric crystal color depends on NPS used, xylene first pull usually brings that yellow stuff regardless, second pull is whiter. Chlorof usually brings white stuff in whatever pull it is, but there is that yellowish pre-crystal goo before precipitates get big on top of this NPS (in this case the FASA cloud and crystals float). Would say it lightens somewhat, but that would be misleading, feels more like the yellow stuff stays in the core of the crystal and the white covers around it, making it turn `whiter`.

Main evidence is Benzyme's mass spec with multiples of 188 for goo (red in his case).

Thank you for the reference Loveall. The mass spec has the technical problem of not having exact controls, how would you get the 2, 3, 4 ,5 unit oligomers to run individually? Maybe 2 units is workable if you chemically block one side of DMT.

Another thing I`m trying to wrap my head around on this concept... maybe a tangent in this discussion thread, sorry... but, would polymers be psychoactive? If so, well, we know the yellow and red stuff is active, but how would be the mechanism of action? Would it bind its exo or endo positions at 5HT receptors?

 

[downwardsfromzero]

Another thing I`m trying to wrap my head around on this concept... maybe a tangent in this discussion thread, sorry... but, would polymers be psychoactive? If so, well, we know the yellow and red stuff is active, but how would be the mechanism of action? Would it bind its exo or endo positions at 5HT receptors?

Good question. This would involve some fairly intricate research to be determined anything like conclusively. Since the oligomers are strongly suspected to be acid labile towards an active monomer; it might involve things such as preparing oligomer-bound cloned 5ht-2a receptors, which is no mean feat especially if one wants to control the oligomer size. Might be a job for the successors of David Nichols.

 

[Loveall]

Thank you for the reference Loveall. The mass spec has the technical problem of not having exact controls, how would you get the 2, 3, 4 ,5 unit oligomers to run individually? Maybe 2 units is workable if you chemically block one side of DMT.

Another thing I`m trying to wrap my head around on this concept... maybe a tangent in this discussion thread, sorry... but, would polymers be psychoactive? If so, well, we know the yellow and red stuff is active, but how would be the mechanism of action? Would it bind its exo or endo positions at 5HT receptors?

Not sure I understand the mass spec question. I imagine a 3D "DMT ball" with the indole rings weakly interacting and coming together. The amine tails (which can ionize) would stick out. The mass spec could rip parts of these balls apart to explain the different DMT multiples. Kind of like partially blowing off seeds of a dandelion. Pure speculation on my part.

During mini A/B, oily DMT forms a cloudy solution when dissolved in acid. Stirring over time in high acidic conditions, it can become clear (after which basing gently and pulling generates xtals). This could be consistent with larger groupings of DMT being broken up.

As far as activity;

- Vaping: I think heat would break up the oligomer before vaporizing. On the more precise electronic devices (compared to brute force flame) I have subjectively felt that goo needs higher temps than xtals. Some have claimed that goo is less potent on an e-mesh vs xtals, I have personally found that goo can be just as potent after increasing the temperature setting.

- Orally: I would speculate oligomers would be broken down by the metabolic process. Not sure if intestinal absorption is lower for oligomers that survive the stomach HCl (if any). Perhaps the tradition of long aya boils has the benefit of breaking up oligomers (?).

An aggressive pressure cooker treatment of acacia has been reported to minimize goo. Perhaps this plant family has a higher natural DMT/NMT oligomerization degree than DMT in MHRB and benefits from a more aggressive acid treatment before going to base.

Disclaimer is that all this is speculation trying to explain ongoing experimental results.

 

[Dirty T]

I have a backsalt bottle I basified yesterday sitting in a warm water bath (90* C. I use a Pyur 500ml for backsalt and a Pyur 2L for basifying). It was collecting crystals along the top layer (I use reused Naptha for everything and my Naptha literally won't pull anymore so I either have to backsalt it and clean it up or use some fresh Naptha which I technically should have done to begin with.) I let it sit overnight and it looks like a snow globe. The thing is just filled with floating freebase DMT Crystals.

I only brought this up because Loveall said after basing and pulling generates crystals but just basifying will cause the now insoluble DMT to crash out and float around. It really does look like a snow globe, a magical snow globe at that.

A side note, the backsalting was done after pulling 'spent' MHRB with 800ml Xylene two times. The Xylene was then backsalted using 350ml 5% acetic acid (Distilled White Vinegar) heated to 80* C on a hot plate then after all pulls were backsalted and solvent removed the jar was left overnight at 140* C on a hot plate to remove any residual Xylene. It was then basified using 50g NaoH and 1500ml distilled water. I pulled twice with "saturated Naptha" about 200ml but yield was practically none. You can see the DMT floating around laughing at me. I'll pull with clean Naptha today.

 

[Loveall]

I know those mini A/B snow globes that appear after basing. They move into the naphtha for me. Sometimes it takes a bunch of shaking and heat. More NaOH or salt could help too, not sure.

 

[Loveall]

Have results for this posted earlier:

Here is a potential practical test with actual numbers. I haven't done this yet, but plan to try something similar to this:

-Extract: Mix 100g of bark with 500ml of 15% citric acid solution. Microwave at 300W for 30 minutes. Replace any lost water, stir, and repeat microwave run two times for a total of three runs.
-Dilute: Add water to reach ~1L of volume in the extraction vessel. Ideally, the vessel narrows near the top to make pipetting easier in the next step.
-Pull: Add ~150ml of naphtha and shake solution. Add lime and continue shaking. Solution expected to go from light red, to milky, to dark red (after ~ 50g of lime). Settle, allow layers to separate (hopefully they do), and remove solvent layer with a pipette or turkey baster. Repeat naphtha pull 4 more times (warmer pulls at 50C may be better but if polymerization is very low room temp may be fine, IDK).

Unfortunately some DMT oil came trough along with the powder. Yield was fine, 2.2% after 3 pulls. Not sure why min polymer was not obtained. I started a mini A/B and the acid solution was cloudy. Inspired by the PC results reported here, I PC'ed the acid solution and it became clear after 1 hour . This could be an indication of de-polymerization and perhaps a PC is best for min polymer (?).

So next I'm trying this:

- In a quart jar, mix 100g of bark, 100ml of vinegar and top off with water near the top.
- PC for 4 hours
- Add naphtha
- Shake in NaOH 5g at a time until emulsion breaks
- Pull (3x), evap, freeze

 

[Ruffles]

Not sure I understand the mass spec question.

Lemme rephrase that: where would you get or how would you make precise DMT oligomers to run as controls in the mass spec?

I assume that the ultimate reference for a ionization spectrum comes from controls, in this case, a 2 DMT molecules oligomer, a 3 DMT oligomer, a 4 DMT oligomer, a circularized DMT oligomer and so on, all run individually in the same equipment, parameter and reagents. Sure you can simulate and predict, but there is the gold standard. Gotta email thermo-fisher and ask for that

 

[Loveall]

Not sure I understand the mass spec question.

Lemme rephrase that: where would you get or how would you make precise DMT oligomers to run as controls in the mass spec?

I assume that the ultimate reference for a ionization spectrum comes from controls, in this case, a 2 DMT molecules oligomer, a 3 DMT oligomer, a 4 DMT oligomer, a circularized DMT oligomer and so on, all run individually in the same equipment, parameter and reagents. Sure you can simulate and predict, but there is the gold standard. Gotta email thermo-fisher and ask for that

I think Benzyme has his mass spec calibrated with some other standard. Don't think we need those specific reference molecules unless we are measuring a yield.

 

[Loveall]

Unfortunately some DMT oil came trough along with the powder. Yield was fine, 2.2% after 3 pulls. Not sure why min polymer was not obtained. I started a mini A/B and the acid solution was cloudy. Inspired by the PC results reported here, I PC'ed the acid solution and it became clear after 1 hour . This could be an indication of de-polymerization and perhaps a PC is best for min polymer (?).

The PC treatment was effective and essentially all the oily DMT came back as white xtals. After scraping up was slightly off white. Looks really good to me.

I'm going to focus on PC treatment of the bark in pursuit of a min polymer process.

Thanks to Northerner for his report on PC and acacia.

 

[Jees]

Hi Loveall,
I did things a bit parallel with you, following you lead. I used the last deep yellow sticky crystal-goo pulls to play with. Nuking with acid (muriatic, phosphoric acid, citric acid) did not do the trick on it's own.
Then I had the backwash at pH3 to 4 with phosphoric acid (so not this much of acidic strength) and PC'ed for 1 hour, I cannot say the yellow color lessened. Pulled with naphtha and still got an oily layer but at lower temps though, not so fast anymore.
So my PC action failed to lighten the backwash color (golden yellow) whereas yours did, what acid did you use please? I placed a glass beaker inside the PC on an elevated level, then a waterlayer at the bottom to boil, the backwash was 100ml. So my backwash saw only glass in the PC, no metal.
I think to keep working in too small volumes, too concentrated.

Edit: backwashcolor pic added

 

[Loveall]

It was citric acid, but not a lot. The liquid saw metal (aluminum) and was pretty dilute. Northerner had the acidic bark in contact with the metal.

 

[Jees]

Ok, thanks, I'll see what freezes, and if still too yellow I'll copy cat

 

[Jees]

Ok, thanks, I'll see what freezes, and if still too yellow I'll copy cat

Definitely better (see pic), there is at least white now and the yellow is dry enough to just about not-stick. In practice one could leave it this way, but it looks to have come only half way of the idealized target which comprises of de-coloring a deep yellow backwash. Thinking of repeating same procedure with only one variable changed: adding a piece of aluminium in the pressure cooked recipient.

 

[IridiumAndLace]

Here's a question for you... Do you suppose our hypothetical DMT polymer is more soluble in naphtha versus heptane?

I ask because I always pull with heptane, and while I get beautiful white crystals every time, I struggle with yields. My latest run stands at 1.2% after five pulls, which is about as good as I've ever gotten. If you're pulling with naphtha and getting that much in crystals plus some polymerized goo as well, maybe that's part of my issue?

If that's the case, perhaps an optimized extraction protocol begins with a low-polymer extraction with naphtha, followed by a mini-A/B with a PC depolymerization during the acid stage, then a re-x with heptane.

Or for that matter, could I skip the naphtha pull and mini-A/B by simply pressure cooking the MHRB in acid during the initial workkup? I have a pressure canner large enough to fit two large beakers, maybe I'll try that this evening.....