I'd hope they'd be issued with a brain before being allowed into a kitchen, but I guess you never can tell.

ok, thank you.

then SWIM will soak it for longer in the lye.. because acid cooking is not swims favorite hobby!

Question for veterans of this tek, particularly wrt to the minimum polymer discussion (which i see as another iteration of Max Ion), here: https://www.dmt-nexus.me...aspx?g=posts&t=97103

When collecting the pulls, Max Ion says to let first pull cool to room temp, then move to fridge and store there until all pulls have been collected. Since 6 pulls could take several hours, wouldn’t it be useful to keep the pulls at room temp or warmer until all pulls have been collected?

As I understand crystallization, the extraction solution is collected with above ambient heat to get closer to ‘super-saturation’ then cooled below ambient to reduce solubility, which aids crystallization. Is there any foreseeable problem delaying the slow cooling (to minimize polymerization, to avoid goo) and subsequent ‘super cooling’ (to force crystallization), until after all pulls have been collected?

Guess i’ll find out.

Here’s the first plan:
- Follow tek through basing
- Follow ronsonol dosing
- Store pulls, while collecting, in sous vide controlled 50c water bath
- No solvent evaporation
- Cool combined pulls to ambient
- Cool further till stable temp in fridge
- Finish in freezer per tek.


Later 2/28: Started earlier w 50g mhrb powder and a 1 qt mason jar. After 3 freeze/thaw cycles, and a 19hr acid soak, I salinated and based per the tek. Heated ronsonol using jar-in-sieve setup in boiling water; cooled acid-powder to ambient; did six 50mL pulls, with four 20-sec bicycle peddle shakes over 45 mins per pull (heated solvent seemed a waste of time, given the volume differences, next time just gonna leave jar in 50C bath; 4 pulls in 45 minutes doesn’t fully clear after each shake, so I switched to three 6-7 minute rests then a long final rest for max solvent recovery per pull, still only recovered 230 of 300mL added). After each pull, pulled solvent was combined in a jar warming at 50C. No evaporation step. After all pulls, the crystal clear, but ever so slightly yellow-tinged solution was emptied into 9”x9” pyrex baking dish & covered w plastic wrap and then tin foil, allowed to reach ambient temp (~1hr), then put in 38F fridge (~1.5hrs). Moved to freezer and will leave in for 12-18 hrs. Update sometime tomorrow.

3/1: I let it crystallize for 24hrs; pics at 12, 18, 24 hrs are crappy, but clear enough to see not much change over those periods. Very white and sparkly results, a couple small patches of yellow oil (see “Dried” pic) which I attribute to contamination (imo: the slight yellow tinge mentioned above reaggregated, from a couple of miniscule drops of the black-red-yellow tar that had dissolved/dispersed in the pulled solvent). Notice this contamination in the “Scraped” pic.

Yield only 1%. My excuses: 1st DMT run ever/learning curve; not sure what typical yield is from the powder I have; fresh/unloaded solvent; perhaps the changes to tek reduced yield.

My focus with this run was to maximize white crystal quality, which I did for the most part. Future runs will work on completely eliminating contamination, using a better-suited container and better solvent removal. I’ll also focus on improving yields, and testing some ideas I have to improve the maceration, acidification, salination, and pulling processes.

This is a great tek, CYB; which along with ideas generated in Loveall et al’s Minimum Polymer thread/tek can improve crystallization quality and consistency. I hope we can also find ways to reduce elapsed time considerably.

Thanks All!

3/4: Next iteration (#2) of adjustments to Max Ion is crystallizing now (50g of MHRB powder from same batch). This run is focused on reducing the roughly 5-6hr pull process in Max Ion to 1 hour, based on Loveall’s “Pull” steps, here: https://wiki.dmt-nexus.m...one_with_IPA_and_Naphtha (4 x 10 min pulls w 65mL/pull heated ronsonol).

I didn’t change the order of the NaOH addition from Max Ion (same timing as NaCl addition; 19 hr, 50C bath), but i am using a 1L Erlenmeyer flask this time (which eliminated visible tar contamination during pulls, and allowed for 93% solvent recovery), so, due to the extra container volume, I added 5g more NaOH to hit pH 12 when additional water was added to get pre-solvent surface to bottom of flask neck.

Additionally, citric acid was substituted for vinegar. As pH of the powder-water solution was already 4.3, the 0.5g citrate, dissolved in approx 20mL water, dropped pH of the solution to 3.7 (obviously very little buffering in the powder-water solution).


About to do pulls on a third iteration of Max Ion, will describe changes in 3rd iteration after results from 2nd iteration are posted.


3/6 am: Decanted solvent from my 2nd iteration of Max Ion last night, after 24hrs of freezer time. Total yield 0.8%, roughly 20% less than the previous full-on Max Ion recipe. It’s looking like my batch of powder won’t be able to produce the 2-3g yields that some report with Max Ion. I again used fresh solvent, so the reported yield is likely understated.

Quality was improved (due to narrow neck container, careful syringe decanting), no visible yellow aggregations in the crystalized product; but still a barely visible oily film on the dish surface, that, when scraped, accumulates small amounts of a yellow goo. The dry, brilliant white crystals (see attched pic) can mostly be removed without scraping the surface; so it is possible to carefully separate the visibly pure crystals from the “contaminated” crystal-oil component, then re-crystallization of the yellow-tainted product.

At first glance, the yield is disappointing vs the full-on Max Ion recipe. But, considering that the 6 decants in Max Ion each have 4 separate shake-clear cycles in 5-6 hrs of working time (24 total shake-clear cycles; where the separation of the product occurs), and Loveall’s 4 decants each have only one shake-clear cycle in 1 hr of working time, it appears that Loveall's method is much more efficient, likely capable of equalling Max Ion yields with major savings of working and elapsed time, by adding additional pulls. Btw, recall that Loveall’s pulls use 30% more solvent than Max Ion, so they can potentially hold a bigger product load; and though it may just be related to change in container shape between my runs, Loveall’s method clears in 3-4 minutes, so shake-clearing cycles could be easily doubled without extending the 1 hour working time.

Separately, I have a 3rd iteration crystallizing atm. This one again uses 50g powder from the same batch, and fresh solvent. It follows the same process as the previous, 2nd, iteration; but substitutes 50g KCl for the NaCl, and reduces the salination-acidification step to a 1-hr duration. See attached pic for water vs loaded solvent comparison.


3/6 pm: Decanted solvent from my 3rd iteration of Max Ion, after 24hrs of freezer time. Total yield 0.7%, roughly 12% less than the previous, 2nd, iteration. I again used fresh solvent, so the reported yield is likely understated.

Quality was consistent with previous iteration, no visible yellow aggregations in the crystalized product; but still a barely visible oily film on the dish surface, that, when scraped, accumulates small amounts of a yellow goo. The dry, brilliant white crystals can mostly be removed without scraping the surface (notice the scraped and unscraped areas surrounding the white crystals in the “Scraped” pic below).

The yield reduction versus the previous run indicates that a longer acidification-salination period and/or perhaps higher KCL level would be needed to reach/exceed iteration 2’s yield.


The next Iteration (#4) will use the Max Ion freeze-thaw through basing steps, substituting citric acid for vinegar, and KCl for NaOH; and using Loveall’s 4 x 10 minute, 65mL pulls, substituting 2 shake-clear cycles per pull vs Loveall’s single cycle per pull. The goal is to meet/exceed Max Ion yield while significanyly reducing pull times (which is most of the ‘working’ time commitment in this tek).

When this goal is achieved, I’ll replicate the process, and cut freezer time in half, to see yield effect of 12 vs 24 hour crystallization periods. Afterwards, I’ll start work on reducing the nearly 2 day maceration time. I’d like to get the entire process, purple powder to white crystals, down to less than one day of elapsed time.


3/7: Iteration #4 has started; 50g MHRB powder from same batch, in 300mL water, is beginning 2nd of 3 freeze-thaw cycles in a 24 hour period.


3/8: Iteration #4 defrosted and transferred to a 1000mL narrow-neck erlenmeyer flask, topped up with water to ~900mL, then acidified with citric acid and salinated w KCl, in 50c bath. Pre-adjustment pH started around 4.5, After dissolving 1g citrate in 20mL water & stirring in, pH decreased to 3.5. 90g KCl (molar equiv of 70g NaCl) dissolved in 50mL of the mhrb solution and then added back to flask, raising pH above 5 pH. Took another 50mL pull from the mhrb solution and dissolved 2g additional citrate and added, taking pH back to 3.5. Will let it bathe at 50C for 19 hrs, then base with NaOH.


3/9: After 19 hrs, basified with 45g NaOH (pH ~12.5), and let flask continue to bathe for 2 more hours @ 50C. Heated up to 50C 4 x 65mL portions of fresh ronsonol, for 4 pulls. Each pull consisted of 4 bicycle shake-clear cycles, lasting about 15 minutes, total pull time 65minutes. Pulls were collected in a jar and allowed to cool to ambient (~71-72F), then placed in a fridge to chill for an hour, then poured into a pyrex baking pan and covered with plastic wrap and placed in a freezer to crystallize.


3/11: Cold Filtered, dried, and scraped after 24-hrs in freezer, 1.1% yield (0.135g in coffee filter, 0.410g in pan). Looks like Iteration #4 (Loveall’s improvements) at least matches the original Max Ion, AND SAVES 4-5 HOURS OF HANDS-ON TIME.

Will start working on reducing pre-basing time.

Thanks Cyb & Loveall.

I think this will work well. Adding a seed DMT xtal right before freezing could be useful too per Mindlusion.

Thanks for your support, Loveall.

I expect to get my 1st seed from this. lol

I have a tip for your contamination problem there. There is nothing wrong with the strategy you are employing here, combining all of the naphtha pulls before proceeding with crystallization is the right approach. The small minuscule drops you were talking about which were stuck floating in your solvent? This is normal, not a consequence of any poor technique on your part. Extractions are prone to emulsions, and non-polar solvents aren't perfect, and can still hold onto traces of water, and these micro emulsions that you are seeing can take hours if not days to settle out by themselves.

Fortunately, there is a simple solution for this. Because the contamination comes from the aqueous layer, it can be simply washed out. This is standard practice after any A/B workup. After you have collected all your non-polar extracts, you add 100mLs of 5% Na2CO3 in water (any mild base would do) and give it a good mix. All of that yellow contamination and micro emulsion will get washed into the water layer, and you can simply separate the layers again as before, except now you have a clean naphtha extract. The beauty of the washing step is that you don't have to wait any time at all for the layers to separate, and you can ensure 100% recovery of the solvent. You can do 4-5 pulls quick and dirty, and then rely on the washing step to remove the contamination. To further improve this and ensure a crystal clear naptha extract, you need to remove the traces of water, since water will still be present. There are a number of ways to go about this. The best way is to use a desiccant, like anhydrous MgSO4, which you can make from heating epsom salts in the oven. This desiccant does a great job at cleaning up contamination, so much so that sometimes you can get away with just using the desiccant without the water wash, since the contamination will stick and coagulate with the MgSO4, then you can filter through a coffee filter to have a perfectly clear extract. Most people are too lazy or pressed for time to filter, including myself sometimes, so my favorite method here, especially when dealing with amines (such as DMT) is to use granular K2CO3 which has been dried in the oven. Its a great desiccant, but unlike MgSO4 it isn't a fine powder, so it doesn't make the naptha cloudy and need to be filtered out, it can be quickly decanted into a clean glass jar. No muss no fuss.

Now if you don't have any desiccants, there is another shortcut that is effective in a pinch as well.. after your water wash, you wash again this time with a saturated salt solution (NaCl). The saturated salt water acts as a desiccant, and as a washing rinse. It will do a great job at sucking up any of those miniscule micro emulsion drops, it also has a higher density and surface tension than water, so its easy to separate from the naphtha as well. This is useful if you are doing the separations without a glass separatory funnel (a ziplock freezer bag works in a pinch too, but be aware that you will be leeching plasticizers). You can even skip the first water wash if you want, since the saturated salt water will also dilute any of the yellow contamination, but if you are going to do one you might as well do the other, not saving much time here. You just need to be careful not to leave any droplets in your solvent, or you will end up with salt in your product.. Thats why it is always best to combine this step with a final drying and filtration with a desiccant, but you work with what you have.

I sincerely appreciate your response, particularly the change in tone.

I am very certain that this generous and helpful explanation will be useful to me and others in the future.

I admire simplicity, which I jokingly refer to as laziness. So, with all due respect, for now, I’ll stick with not sucking up visible drops of tar, and see how that goes, vs adding rework to achieve non-visible purity. It is a personal goal of mine to show others that high purity and reasonable yield can be achieved, with minimal effort, by non-chemists.

As you may have noticed, some of your contribution on Loveall’s Minimum Polymer thread has been incorporated into my work here, to avoid discoloration due to polymorphs. Thank you for that, as well.

I appreciate your change in tone as well. I never meant to insult you, I do appreciate your posts as well, I only felt like it was necessary to say something and defend my friends when there was something off. And I know I could do more to help out others in the general sense.
I also joke about laziness being a driver for efficiency and improvement, even the development of entirely new procedures. In reality its not just laziness, but financial and time constraints! Both are effective drivers for improvement. One of the beauties of organic chemistry is that the more simple and efficient a process is, the less energy it requires to carry out. That is the evolution of life in a nutshell. That is not just thermodynamically speaking, but including personally for the chemist! Imagine a process or extraction that only yields 10%, then you still have to waste time and energy separating that 10% from the 90% crap, making it 10x worse in the amount of time and work overall. Where a process that yields above 90%, the product is so clean that you barely have to spend any extra work in purification, making it 10x better overall. This kind of thinking leads to improvement, I can't tell you how much it kills me inside when I see another chemist using an outdated and inefficient procedure, destroying perfectly good precursor, because they couldn't be bothered to think about how it could be improved instead.

I truly appreciate your comments. I give you a lot of credit for the thoughts expressed in your first paragraph. Loyalty is a mostly good attribute.

In this case, I did not attack your friends, just insisted that they admit reality, and contribute some new, practical improvements to old, inefficient teks found here. but I won’t rehash.

I admit that I did attack you, after you failed to acknowledge the truth of my restatement of your initial attack on my statements being “wrong”, and your further subsequent ad hominem attacks, which you later edited. In the hope that we both understand each other more clearly, and will proceed with goodwill…peace.

I like the word ‘elegant’, to describe the concepts you discuss in most of the 2nd paragraph.

And as far a taking the good and improving it, especially if there is a big opportunity for improvement, that’s what I think is possible here, with Max Ion. It’s a solid & simple tek, the biggest opportunity is to reduce the time to completion. At the moment, I am exploring the possibilities in the extraction process, but where the biggest opportunity is in reducing the time of the maceration process (start of tek up to basing). We need some creative ideas for this, and the literature shows a number of possibilities, some may be adaptable to a kitchen environment.

Iteration # 4 results above.

Thank you everyone who brought us to this point and Cyb for compiling such a comprehensive document.

It sure takes a lot longer than previous methods attempted but the results are wonderful.

50g mhrb
Followed tek to the letter apart from a slightly lower salt content as ran out of pure salt and was too impatient to go out to the shops. 56g used.

Duration from first freeze cycle to scraping ~ 96 hours

3 pulls with 50ml new naptha per pull yielding 0.445 beautiful hyper fluff.

Will update when the soup is depleted as time allows.

So far in a novice's experience seems to be the best result in terms of efficiency against mhrb wastage.

Thanks again



Edit update:

After 6 pulls of 50ml new naptha total yield .536 giving a little over 1%

It is likely that there is more to squeeze out and the naptha needs a final evap.

Doesnt sound like much compared to some results here but on average this mhrb has be granting around 0.6% with any other methods attempted so there has been much rejoicing.

As a curiosity, an idea of filtered water was to pour tap water through some coffee filters. Is that good enough?

Hi !!, why dont use DCM or EtoAc for the pulls and heptane or hexane for crystalization?
DCM have the mayor affinity at room temp. Because the layer of DCM stay at the bottom? prevent a reaction? emulsion?


regards

You can use many solventsx they are just not part of this process.

Also, I don't think they warmed the hexane in that paper either, while the naphtha hydrocarbon is warmed in this process. That makes a difference.

By the way, limonene (not on that list) has a good partion coefficient and is convenient (pleasant smell) based on my experience. If you want to boost your partition coefficient use that. Also, benzoic acid easily takes DMT out of the solution.

I use unfiltered tap water with great results.

yeaaa, but not deal with warm flamable solvent is a great thing i think..
and the use of dcm have the good that need much less solvent to.
the limonene need to warm to?

Limonene pulls very well at room temp.

I have a large volumen of acidic water(ph 2.7 ascorbic acid and citric acid) there is soak the mimosa for al last 2 weeks and freeze 5 or 6 times( i dont have the time to do it) I am thinking in filter the most gross with a bubblebags then squeez in the hidraulic press the biomass(i have a chees pressfilter). If i do another extraction after press the biomass will be a lost of time? And my idea is boiling the acidic water to reduce before the base step, for a more easy volume to work, or will be better reduce under pressure in the rotovap at low temp?

Here in Brazil the medicines mans in the jungle make a "Ayahuasca Honey" that in a kind of ceromoni (feitio) boils 3 days the vine and reduce. Is extremly potent.. my doubt is if i boil the acidic water i was loss dmt?

Thanks

Thank you Loveall

Another water extraction should not be a waste of time. Boiling down the water should not reduce dmt.

However, for the TEK in this thread, you do not need to separate the bark from the water. You base it all together and suck the solvent from the top later. If you separate the acidic water from the bark you are doing a different procedure.

I would recommend simply sticking to this TEK and not separate the water and bark.

Thanks man, but really i think need to do it, i know is a diferent procces, but i have a lot of gallons and kgs of bark , and i dont want to work with big volumes of solvent , i will make the extraction with ethyl acetate evap the solvent in roto and use it again, evap and again ,again ...until the solvent dont pull any more. I think the ethyl acetate makes a more "full spectrum". And if i want purify dmt rex in heptane
I will update the journey. Maybe i will make other tread for not step this.

Thanks and love