A short update:

I have completed the first part of the "theory test." The powdered mix was placed in a funnel lined with coffee filters, ( I know, I know.... I forgot to order the 11 cm filter paper; I only have the 5 cm quantitative filter paper) with a 5 cm quantitative filter paper between some of the coffee filter to prevent the vacuum from pulling the coffee filters apart.

I measured 100 mL of room-temp acetone, and began to "wash" the powder by slowly pouring the acetone through the mix. At first, there was no need to use the vacuum. The solution freely flowed through the mix, while I used a scoopula to gently stir the powder. After the first 100 mL, I was concerned. There was very little discoloration to the acetone. I am generally used to seeing hints of "greenish-yellow" when I use acetone to pull directly from the plant material. So, I used another 100 mL of acetone, and washed the product once more. Again, very little discoloration. Beginning to question the effectiveness of this method, I flushed one final 100 mL through the powder. This time I utilized the vacuum so that I could remove as much of the acetone from the filters/powder mix.

After I had removed the majority of acetone from the mixture (85% or so) I placed the powder mix back in a jar to soak in acetone over night. (results from this part will come later...)

I reduced the ~300 mL of acetone to about 50 mL, and noticed some slight particulate matter. I assumed it was powdered magnesium sulfate that had managed to slip through the coffee filters, so I used a qualitative filter and vacuum to remove the particulate material. At this point, I felt that even 60 mL (after rinsing the filter paper) was a larger volume than I wanted to work with, so I decided to reduce it down further. As I was transferring the beaker to the hot plate, I managed to spill ~20 mL. I was irritated, but proceeded to carry on. So, now we're at 2/3 the amount that would have been potentially extracted from the three washes.

I reduced the 40 mL of acetone down to about 10-15 mL, and noticed that there was that "discoloration" that I was "used to seeing." [SEE 1st IMAGE BELOW] Satisfied, I decided to proceed with the titration. Upon initial titration, I did not notice any precipitation. Disappointed, I covered it with a watch glass, parafilm, and placed it in the freezer to see if any precipitation would occur. My hopes of this procedure were diminishing.

This morning/noon, I decided to check on the experiment. To my surprise, I saw that there was a collection of white precipitation that was suspended and attached to the sides of the beaker! [SEE 2nd IMAGE BELOW]

SO. I am going to allow another 24 hours of precipitation, and then I will filter and analyze to see if it is indeed mescaline sulfate, or just some unexpected side product.

Take Care!
ACY

Update:

The beaker that has about 10 mL of acetone and currently precipitating "mescaline sulfate" is still in the freezer.

I've been dealing with some complications unrelated to the extraction as well as working on a different project, so I have not been able to put the amount of time into this experiment that I would like to. But, we get what we get, right?

In the mean time, I decided I would push a little further. I had frozen the 3 x ~230 mL portions of reduced cacti tea. I pulled out one of the "2nd" cook jars and let it thaw while I was doing other work. After it had thawed, I placed it on the hotplate to reduce. ~6 hours later, I had slowly reduced it to 30 mL and separated into two 15 mL portions. They have almost become the consistency of a tar, but I am just going to hydrate a bit if I feel that it is needed. One of them was left on the hotplate a little longer than preferred, so its consistency is much more thick - almost hard-ish. I have seen similar characteristics from evaporated resin, so maybe it'll be interesting.

Another consideration is dissolving the tar into minimal acetone and using vacuum filtration to remove particulates prior to the calc hydroxide and mag sulfate additions. I am also debating separating the two 15 mL portions into 4x 7.5 mL portions so that I can test out a few different variations.

I will still have ~230 mL from the first cook and ~230 mL from the second cook that are in the freezer. Pending the test results, I'll either extract, or just reduce to a resin.

Take Care,
ACY

Pic: 15 mL of thick tea (resin)

Mostly busy with other things, today - but I took a few breaks in between to see what results i may find. I filtered the precipitate, which was basically nothing... so i wondered if I had poor proportions of sulfuric acid to solution, so i began to evaporate the acetone. It became cloudy and I put it in the freezer... we'll see, but it doesn't look promising.

On the other hand, I had been soaking the "used" powder rexture in acetone for a few days so I decided to see if there was anything there. I filtered, reduced, and began titrating...

GLORIOUS while precipitation began forming just as it "should." With each drop, More and more white fluffs... and then it happened. One drop too many?

All of a sudden the solution became totally colorless, and all the precipitation coagulated, as micelles - little oil droplets that separated from the solution. I instinctively just thought to add more acetone, but it didn't resolve much. Disappointed, I covered it and stuck it in the freezer to see what happens. It looks like "something is happening" but hard to say what.

My error was that one extra drop...


Either way, it helps test the theory. If I had just stopped when it seemed like it was maxed out, I'd probably have a neat little collection. Doh! oh well. I have a few more chances...

Take Care,
ACY

Little update.

The over-titrated sample was put in the freezer just to see what would happen. A colorless precipitate formed on the sides of the glass. I let it sit for a few days, and then decided to check it out.

I poured the solvent into a beaker and began evaporating to see if there was anything interesting that had remained in the solvent. Meanwhile, the precipitate on the inside of the jar began to dry. This image was taken just before placing under reduced pressure. I've yet to check on it today.

I plan to make some marquis reagent and see how it reacts. I won't have time to get the things I need to make the reagent until next week, but I'll share the results. If it's anything interesting, then I'll likely send to benz for a full analysis so it can be fully analyzed.

Take care,
ACY

Thanks for continuing to update the progress ACY.

It can be challenging to refine an extraction process due to the fact that cactus material varies so much in content between cuts. Have you ever considered taking a single cutting and dividing it into sections and then performing different extraction processes on those sections? That method might give the clearest picture of which extraction process is most effective.

YES!

Actually, I have it prepared.

I have a nice chunk of resin that I am going to split into 4 portions. I'll keep one as is. I'll try one via the "theory test" method, but I am going to let the acetone soak for a long period of time, and I am going to consider another method. And I'll do a typical toluene liquid extraction for comparison.

I want to collaborate with a few of the other chemist prior to taking this approach, because I am not an "organic chemist" by specialty. On paper, I am an analytical chemist. So, before I make it more complicated for myself, I am going to ask Mindlusion to give me some guidance, and then I will get back to you on the 3rd method. BUT. It may be interesting....


Take Care,
ACY

Thats excellent ACY. Thanks for sharing your findings.

You're welcome! And, thank you for making sure that I am doing proper research and testing the theory against one that has already been proven to work.

No two cacti are the same, so it is hard to validate a procedure based on a singular experiment, or an experiment that is only tested on one type, or clone, of cacti. Since most people are extracting for the reason of "I want mescaline, how do i get the most, and the fastest." That mindset, with an unknown experimental procedure, could lead to lackluster results. Since the method is unknown, yet, I am using very small amounts of material so that I am not at (much of) a loss, if it fails.

So, I decided that I would do the series of different extractions from one source of resin. I will record the starting mass of the resin, and then divide the pieces and record the mass of those - adjusting if needed. The resin still has some plant matter in it, so I will likely have to adjust the exact results based on how much plant matter is found in each. (reconstitute the small amount of resin in acetone, filter, remove solids, record mass of removed solids, and then adjust the final yield to reflect the removal of the solid.)

I am getting the needed materials to make some marquis reagent and see if the method is indeed pulling mescaline or just solids that precipitate from the solution. The other option is TLC. I have some UV active silica plates and the needed things for a mobile phase, but I lack the UV light that is needed. So I am going to try reacting the mescaline with the reagent on a TLC plate and determine by that method. The reagent should make the mescaline visible. The other option, is spotting the "mescaline sulfate" directly to the plate, spotting the caffeine comparison, and then developing the plate. After developing, since I don't have the UV light, I may make a dilute solution of the marquis reagent in methanol and quickly submerge the plate after the mobile phase has traveled the desired length. That may act as dye and display the spots (if the substance is mescaline).

Take Care,
ACY

Hey folks,

This is a little bittersweet. We'll do the bitter part first:

I am going to be turning my direction of focus and interests away from "independent research" over the next few weeks/months/years..... I dunno how long it is going to take.... But, I have made the choice to put my energy into earning a career. It is undermined how long that may take. If you have questions about the TEK or any of the experimental procedures that have been relayed - feel free to shoot me a PM. (I will still receive an email notification if someone sends a PM)

I am a little bit bummed that I didn't get the formaldehyde that I would have needed to make the marguis reagent and test the sample from the last experiment. I'd really like to know if it worked o results, but I surely hope that one of you have taken it further than myself! Keep pushing! If someone else wants to test some of the residue from the precipitation of the last experiment, let me know and we'll figure something out. It's not a lot - maybe 15-20 mg. It is not a dose that would "get you high." It would only serve as data. If the test shows favorable results, then I will published the proposed method in a more detailed report.

Sweet:
I appreciate all the contributions that everyone has made to this thread - you've all helped gather data and form new ideas. I have enjoyed watching this thread grow and I hope that someone else will jump in and pick up where I leave off.

I'll be back once a career has been landed and I have comfortably settled in to the new location. I don't know where I am going; but I am going! LOL. I am going somewhere and I'll figure out where I'll be.... once I am there. There's no way to know until I go!

Anywys.... thanks!
Take Care,
ACY

Best luck with the career and everything that you are looking for. Even though I have only been a member of this forum for a short time, I have greatly appreciated your contributions here. Hopefully it will not be long before you return.

Thank you!

I still have the notifications set for this thread - so it turns out I'll still get notifications of posts. I am not going to be GONE, I am just going to be occupied.
I'll still share a few minutes to reply to anyone who has a question, or just wants to say hello. However, I mean to say that I will not be able to deliver any new data to the thread until I am in a position to do so.

If I end up coming across some ~40% formaldehyde, I'll pick it up, mix the reagent, and share the results of that analysis. I'm just geared in a different direction, right now. I feel like I am going to be more productive, overall, if I maintain discipline and persistence. Sometimes the nexus can be distracting. I'll be working on a project and then I'll get an email that "someone posted to XYZ topic," and curiosity tends to lead me away for 10 minutes or so.

Well, that 10 minutes could have accomplished a lot more than my lengthy posts. LOL, ya know?

Take Care
ACY

Few updates:

1) reagent confirmation of mescaline for the experimental extraction that I had last discussed. THEN, I had an idea:

OK, I use the microwave to cook out the water from magnesium sulfate.... magnesium sulfate is slightly acidic... what if.... I made a slurry of calcium hydroxide, magnesium sulfate, and 90% isopropyl alcohol, and then cooked that in the microwave? That should make a buffer... but what ratios? So, that will have to be adjusted, as I was just trying to see the qualitative results, I did not measure the isopropyl, calcium hydroxide, or magnesium sulfate heptahydrate.

But, i poured a random amount of isoproyl in a glass pyrex dish, added the calcium hydroxide and mixed it up. after the consistency was to my approval, I dumped in some Epsom salts. I mixed all of it together and tossed in the microwave. I did 3x 5 minute cooks, and it appeared to be dry, and able to be smashed into a fine powder. I mixed 2 grams of the powder into a total volume of 20 mL distilled water. The pH was 11.8. OK, well... why not? the pKa of mescaline is like 9.5, so that's at least +2 from the pKa... it should convert some of the resin tea to free base.

I took an amount of resin and attempted to reconstitute with a small amount of acetone. It was partially dissolving, but mainly just clumping and goo-like, so I just began adding the powder. As the powder was added the, resin began to break down to very small bits (maybe plant matter, too). I added all of the powder and added additional acetone. I closed the extraction container and periodically shook the hell outta it last night. I also placed it on the hot plate, low setting, and allowed it to warm to about 40 C. It's been sitting for about 14 hrs, but I'll likely let it sit until about 8 pm this evening.

I'll perform vacuum filtration, reduce the volume of acetone, add more acetone to the plant material, and then do that titration thang!

So, we'll see. This mighta made my life a while lot easier. From start to stopping point (this excludes that I had already prepared the resin months ago), it took about 30 mins - because my wife came home mid-process and I stopped to talk to her for a bit before I got to the stopping point. Sure, every fer hours I'd go check on the extraction and give it a good shake. But that took about 45 seconds of my time. I'm not worried about that.

I did not take pics, sorry! I was not really concerned about the documented part, at the time. I was curious if it works, or not. Due to still not having pulled the tone from the mix, I cannot confirm that it works. But, based on the previous extraction, and confirmation via reagent, I am hoping that it works.

I'll post some pics of the final product, if there is any.

Take Care!
ACY

Inorganic footnote:
By mixing calcium hydroxide with magnesium sulfate you'll form (under aqueous conditions) sparingly soluble calcium sulfate and practically insoluble magnesium hydroxide. Fortunately, calcium sulfate is still a good dehydrating agent and magnesium hydroxide should still act as a base - as you appear to have found.

Now you've got me waiting on the results as well

Indeed! That was intended, the precipitation of Mg(OH)2.... I should have clarified. By testing in water first, I was curious if I had accounted for enough calcium hydroxide to effectively buffer against the conversion and precipitation. Ca(OH)2 is poorly soluble, as you know. To be honest, I was just curious what might happen? Either way, We'll know this evening. The first pull had been collected, filtered, and reduced down to a decent volume for titration. I had been letting the mix soak for an additional pull, which I will filter and reduce to a similar volume. I am going to perform separate titrations on each of the pulls to see if there was any significant reason to do the second pull.

If I yield nothing from either.... - then it didn't work!!! LOL. I'll be sure to let you know if it goes well or goes poorly, either way.

To be honest, I was just curious: "What if?"

I've also contemplated adding anhydrous magnesium sulfate to an "almost dry" resin and then allowing it to completely dry, then crunch it up into a powder. Since it'll still be the salt of mescaline (no base, yet) it could even be dried in the microwave..... - I wondered: "Could I add ammonia to isopropyl alcohol or ethanol and then run the ammonia through the powdered mix, converting to freebase? Then I wondered what resultants may occur, ammonium sulfate? I quickly googled (and probably will again) and I didn't find much - Will isopropyl alcohol react with ammonia at a pH of 11 or 12?

I know that ammonium sulfate is not very soluble in acetone, but I still need to look at the solubility in IPA. From what I gathered (quick searck; if I am wrong, please let me know), ammonia can react with acetone, so that would not be the ideal solvent - even though it WOULD be the ideal solvent. If the ammonia reacts with free sulfate prior to the sulfuric acid titration, it might crash the ammonium sulfate out before filtering. If my sources of information about acetone and ammonia, or isopropyl and ammonia are wrong - please correct me.

These have been brief considerations and I have not put a whole lot of time into the research. I have had a lot of other things going on.


ACY

This experimental 'what if' thinking is very pleasing. There are so many permutations of what can be done!


And... any news?


Some unusual chemistry can happen with microwaves; you'd be treading into unknown territory by microwaving your cactus resin. If there's unreacted magnesium sulfate left, it might do some kind of Lewis acid catalysis to things in the resin amenable to such reactions, for instance. Not that I'm saying this is something to be overly worried about but I do think it deserves consideration and probably some background reading. Accidentally derivatising your mescaline would be a sad loss of yield :/
You may recall that ammoniacal ethanol has been used in soxhlet extractions of cactus powder described variously around here - for instance:
https://www.dmt-nexus.me...&m=874669#post874669
so this should work reasonably well, at a guess.

No.

Correct.

Thanks DFZ!!!


SO! Y'all wanna hear the big update?

Pull number 1 was destroyed. LOL. It's ok. It was an accident. I had a migraine that had been lasting 3 days, but getting stronger each day. Today was inevitable, but I am out of my proscribed med, so.... as part of a combined effort of molecules- I asked my wife if she would mind getting me "your favorite looking mushroom from the albino penis envy bag." She brought me three different bags of regular PE and i laughed and said that there is another one in the back. And asked for one of those.

She opened the freezer (i'm laying on the couch with blanket wrapped around my head) and I hear that unforgettable sound of glass breaking. I said, "are you ok?" She said, "yes, but what ever was in that thing isn't." Me: "The beaker?" Her: "I guess." Me: "the large or small one?" Her: "the large one."

Doh! accidents happen. I came and helped clean up and retreated to the couch. She picked a mushroom... one hell of a ride later.... wow. No headache.



Oh right. SO. Our data will be relying on anything that might have been in the second pull - which has not yet been filtered and reduced. I'll get to it tomorrow. If the second pull yields anything at all, then I will do a 3rd pull for comparison and also begin prepping the other half of that resin for the same procedure.

And I'm down a 1000 mL beaker.


ACY

I'm getting ready to work on this dry tek again. Earlier we got a potential yield of 70mg from 279g fresh (0.38% dry estimate). Interestingly, adding phosphoric acid precipitated a little more from the acetone pulls. This could be interpreted as having a pH issue during the sulfuric acid step titration step.

You can get different salts at different pHs. I now believe that the mescaline salt that crashes in cold water/acetone is in this form:


I think this means that we want a pH below 7.6 (two units away from neutral mescaline) and above 4.0 (two units away from HSO4-). If the pH is too high the salt trivially doesn't form from the free base, but if it is too low, the salt that can form is (mescalineH)(HSO4) which looks more water soluble (due to the O-H bond in HSO4-). Also, even if one could recover this low pH salt, it could be unpleasant and maybe even corrosive.

From a pure pH point of view pH ~ 5.8 seems ideal (averaga of the 2.0 and 9.6 pKas of the species above) with a wide range of 4 to 7.6 from the "two units" pKa consideration. However, we don't want excess sulfuric acid either, so a pH towards the top of this range (7) seems ideal.

Therefore I will shoot for a pH of 7. Notice that dg in the dual solvent thread advises to have a pH in the 6-7 range when preparing to crash mescaline sulfate from up to 50% water/acetone solutions and he has good experimental results.

Here are my thoughts on his tek so far:

- (Optional for dry powder?): perform acetone wash and dry. Edit: there are claims that natural mescaline salts are soluble in acetone so this is not recommended.
- Treat fresh ground cacti or wetted power with Ca(OH)2, this breaks down mucilage and free bases the mescaline, setting the stage for the dry acetone pull.
- When drying with MgSO4, limit the amount to 1x the Ca(OH)2 mass to keep the pH high. Dynamics of this may be tricky, more epson could be ok. It may be a good idea to avoid time/heat to limit mescaline carbonate formation while drying the FB.
- After pulling with acetone, avoid over titrating with sulfuric. Using pH paper strips shoot for pH ~ 7 (acetone can break electronic meters)

A question I have is do we really need to dry the basified paste? If we pull the wet paste directly with acetone, most of the Ca(OH)2 and other stuff should stay behind as the water molecules are surrounded by acetone (?). The minimal TEK would be,

- Make a Ca(OH)2/water paste with cacti powder and react (time/heat/microwave)
- Pull the moist basified reacted paste with acetone (settle in freezer and decant)
- Add dilute sulfuric slowly until pH ~ 7. Crystalize in freezer.
- Decant/filter and recover goods. An optional water re-X could clean things up if desired.

Something else I'm considering is using IPA for the pulls of the basified dry powder and titrating with HCl. That may also work. Since only one mescaline salt type can form with HCl, the titration step should not suffer from too much HCl causing a low pH, and also any excess HCl evaporates (much wider process window vs sulfuric?).

Marquis can be very helpful to understand what is happening so I'm going to also use it for this work.

Edit: I also want to mention that this kind of dry Tek was tested in a different thread over a decade ago by 69ron. However, he added fumaric acid to acetone which didn't work, and the fumaric salt was claimed to be soluble in acetone. At that point the work went towards limonene pulls without having to dry the paste completely (and subsequently different limonene salting methods of which FASI is the most modern/straight forward I believe). It doesn't look like they tried sulfuric/acetone back then (or if they did, results - either good or bad - were not reported as far as I can see).

Ok, I gave this a try.

1) 100g of dry cacti powder was mixed with 25g of Ca(OH)2 and 315ml of water forming a paste. The mix was microwaved (1700W) 5 times for 1 minute stirring each time. The paste went from clumpy to smooth. 30g of water evaporated in this step (based on mass losses)

2) Two 300ml pulls of acetone where done on the alkaline water paste. The paste became clumpy and was easily filtered. The filtered pulls had a deep green color (more so the first one) and were combined and put in the freezer. Sediment formed overnight and was decanted/filtered.

3) Resulting filtrate showed an alkaline pH of (on paper strip). Sulfuric acid (pH down aquarium product 9.6%) was slowly added drop wise (heavy couding observed) down to a pH of ~6 which is when the clouding stopped forming (pH strips were used because acetone can break some digital meters). I was planning on stopping at pH~7 as discussed above, but clouds kept on forming and only stopped at pH~6 🤷‍♂️

4) Acidified liquid was put in the freezer overnight and the fine precipitate was collected in a coffee filter and dried, resulting in an off-white slightly green chalk-like powder when dry.

5) Steps 2-4 were repeated with two more pulls (this time the pulls were less green, nothing precipitated in the freezer before adding sulfuric, and the resulting powder was a lot whiter, but only ~ 10% more came through).

6) Resulting dry powder was combined and dissolved in very hot water (from a boiling source). Luckily the green material did not dissolve and was filtered out.

7) Filtered water was evaporated in an oven at low heat resulting in crystals, along with some remaining impurities (see image for result after scraping).

Got 2.9% yield which seems way too high (expecting 1% or so). The crystals could be many things, hopefully they contain some mescaline. Marquis has been ordered, will report back on that result when available. Also, may send these out for analysis to see what came through with these steps.

Got a strong deep orange reaction indicating presence of mescaline 😍 (images below, first a few seconds after adding Marquis, second a few minutes later - matches this).

Purity is unknown, will bioassay and report back. Not sure how many other salts came so I'll also send a sample out for analysis.

Will also tune the process a little. Some things to try next:

- Microwave longer and remove more of the initial water (easily measured by tracking the weight after each microwave run). Less water could make the acetone pull cleaner. At some point there is a concern of complete drying and damaging the paste in the microwave though (which can also be tested).
- Chill the acetone and Ca(OH)2 base paste before pulling. Mescaline FB should be very soluble in acetone so colder pulls could work well and be cleaner (as is done for salvia acetone pulls). Note that cold 99% IPA would also do a good job of pulling mescaline FB (that could also be tested).

For completeness, I went back to the titrated acetone from the previous post. It was evaped to a sulfuric gunky syrup, based with NaOH/water and pulled with Limonene. FASI showed some clouding, but it was minimal (maybe 30mg, I'll measure it and report back). I think this indicates that > 97% of available mescaline was precipitated from the acetone solution during titration.

The nice thing about this process is that by being OK with some water in the initial paste we don't need to deal with chemical drying. The small amount of water present during the pull does is not very miscible with the acetone perhaps keeping things cleaner, and if Mescaline FB is more soluble in acetone than in limonene then the pulls can be very efficient. Reducing the volume of acetone pulls was not required making the process relatively straightforward. Downsides are that final purity is unknown even though the product is white and fluffy. This just means we get to do more experiments to figure it out and/or see what the analysis says 🙂

Nice work Loveall. I think I see a drytek in my future