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TEK Ethyl acetate approach [CIELO]

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downwardsfromzero said:
grollum said:
The jars from my second attempt were sitting in the fridge for a day and collected what I think was water at the bottom.
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It might be a good idea to collect some of this 'water' and send it for analysis - could it perhaps contain N-acetyl mescaline?
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At some point I will leave an extract in the fridge for 24h to see if drops for and/or yield is decreased. I think that should inform us on the potential reaction.

I have seen the drops before, but they showed up quickly (after a few minutes) and I had stirred agressively without resting before decanting. With gentle stirring and resting they did not show up. In that case I'm pretty sure they were water that came through as smaller droplets while decanting. The 24h situation still needs to be tested though.
 
grollum said:
In my first and second attempt I was stiring before every pull. And maybe not gentle enough. So will only stir once at the beginning and more gentle.
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To clarify: I very gently stir every pull for 30 seconds then let the solvent sit for 2.5-3 minutes, then decant. But even that gentle stir is probably unnecessary since the cactus is so well broken up if all the pulling is done within 30 minutes. After 30-40 minutes the cactus begins to stick together and thus we conjecture it would be slower for the mescaline to migrate out to the solvent.

Just like hot water pulling goodies out of tea leaves within a few minutes, we don't have to stir the water vigorously. Same with the mescaline freebase and ethyl acetate. The ethyl acetate seems to be very effective at pulling the mescaline without physical agitation.

When do you stop? When clear or when the dissolution is not working anymore? I think I should really get a magnetic stirrer.
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I've added 5 mg/gram, 15 mg/gram, and 20 mg/gram with different attempts and they all resulted in precipitation within a few minutes of vigorous magenetic stirring. I added the 5, 15, or 20 all at once (nothing incremental). Yields were all basically the same. The only difference is more of the 5 mg/gram xtals stuck to the walls, requiring a warm water wash to get the last of the xtals out of the jar. The 15+ mg/gram xtals pretty much all come out of the jar by knocking them off the sides with the spinning stirring bar then rinsing with ethyl acetate, thus no warm water wash/evaporation step is needed.

I believe the 5 mg/gram xtals are a little fluffier, thus more sticky. The 15/mg and 20mg/gram xtals are smaller and more dense, thus they don't stick to the jar walls as well.

I did a comparison in Run #3 - Jar (B) versus (D) of 5 mg/gram versus 20 mg/gram and the 20 mg/gram had visibly less precipitate. But after filtering, washing, and evaporating, I found the yields were basically the same. The 5 mg/gram just looks like more when floating around in the jar because it is less dense.

grollum said:
shroombee said:
I conjecture that if water is interfering with xtalization, another way to minimize its influence is to add fresh ethyl acetate to the extract before bombing with citric. It is not necessarily efficient use of the solvent, but for initially testing the hypothesis it may be a direction to consider. For those having difficulty, perhaps split the next run's combined pulls into 2-4 jars and salt them separately, trying different amounts of added fresh ethyl acetate before salting.
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Thought about that too. The jars from my second attempt were sitting in the fridge for a day and collected what I think was water at the bottom. So this might be what is going wrong so far for me.
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Gentle, fast pulls and bombing with plenty of citric acid appear to be the primary differences between my successes and head-scratchers. Bombing immediately rather than letting the extract sit around may be a secondary difference.
 
Loveall said:
Thanks shroombee, I agree. Do you squeeze the paste (if yes, is it a gentle squeeze?) Or simply gravity filter. The pull technique is important. I think 3 minutes of rest after gentle mixing is a sweet spot because (1) it is long enough time for any stirred stuff (e.g. water droplets, small plant particles) to fall back into the paste and (2) it is short enough to not pick up a lot of soluble plant gunk which can interfere/slow crystalization.
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Before pouring the solvent, I push the screen down on the french press so I feel a light resistance. I pour the solvent out of the french press and as the last of the solvent is running out, I use a little pressure to press the screen in further to recover less than 10 grams additional solvent.

I think the best metric for describing the process is how much I recover per pull. These are metrics from my most recent run, Run #4. To recover nearly the same amount of solvent as I added requires light pressing. I have not tried 100% gravity filtering where I let all the solvent trickle out over a minute or two. That might be just as effective and less finicky to describe for the tek.

Pull #1: Added 153.9 grams, recovered 107.7 grams (the last 5-10 grams is due to the light final pressing, the solvent loss is normal on the first pull);
Pull #2: Added 101.1 grams, recovered 102.3 grams;
Pull #3: Added 102.9 grams, recovered 104.8 grams;
Pull #4: Added 100.6 grams, recovered 101.8 grams;
Pull #5: Added 101.4 grams, recovered 101.6 grams;
Pull #6: Added 101.7 grams, recovered 111.8 grams (may have pressed a little firmer on this one);

An unrelated note: After mixing the water, lime, cactus and letting react for 24 hours in a sealed jar, the cactus is a little dry and crumbly. Maybe like cookie dough? I break it up with a fork before starting the first pull. If folks are seeing wetter cactus after basing for 24 hours, that could be investigated as a deviation from what we believe to be "ideal" conditions. I'll take a photo next run.
 
Thanks for the info. Sounds like you are starting with 50g of cactus based on the solvent volume used right?

Do you know yet how much you are getting in pulls #5 and #6?

Are we sure that 24h paste reaction is better than say only 10 minutes? At one point I got better yield with longer paste reaction time. However, I would like to verify that early result since I was changing a bunch of variables and I'm not sure I was being that consistent with the pull technique.
 
Loveall said:
Thanks for the info. Sounds like you are starting with 50g of cactus based on the solvent volume used right?
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Yes - doing 50 gram runs because we're still experimenting with pull times, basing times, et cetera.

Do you know yet how much you are getting in pulls #5 and #6?
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Not yet. On my next runs I will salt pulls 1-4 separately from 5-6.

Are we sure that 24h paste reaction is better than say only 10 minutes? At one point I got better yield with longer paste reaction time. However, I would like to verify that early result since I was changing a bunch of variables and I'm not sure I was being that consistent with the pull technique.
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I have two runs planned where I will test different basing times. Run #4 was 24 hours basing and 3 x 6 minute pulls. I have two 50 gram containers of cactus that were powdered with Run #4 so I'll be testing with the same material.

Was thinking of testing 10 minutes, 1 hour, 72 hours. But I only have two runs of 50 grams. So I'm open to suggestions of which basing time to try first, and then what to try second based on the results of the first run's yield.
 
Dang this thread blew up! Yall are making me want to find some cacti powder. Sadly there are still other experiments I havent gotten to yet ugh.

I can't wait to try out this tek Loveall, great pioneering work with the ethyl acetate tek. Who ever thought cacti xtals could be crashed after so many many failed attempts?! Honestly this same principal can probably be applied to most other alkaloids too with some minor adjustments. Very cool. :thumb_up:
 
Kash said:
Dang this thread blew up! Yall are making me want to find some cacti powder. Sadly there are still other experiments I havent gotten to yet ugh.

I can't wait to try out this tek Loveall, great pioneering work with the ethyl acetate tek. Who ever thought cacti xtals could be crashed after so many many failed attempts?! Honestly this same principal can probably be applied to most other alkaloids too with some minor adjustments. Very cool. :thumb_up:
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Thanks Kash. And thank for your work on cacti too.

I think of this is an adaptation of bufotenine TEKs, where that alkaloid is crashed from dry acetone and citric acid. It is the nexus learning, sharing, and expanding as we have fun. And yes... there have been A LOT of failures LoL, but I think this time we may have found a practical option for cacti extraction. Looking forward to other people's results to see if we can verify shroombee's reliability improvements 🤞. I'm just happy and thankful to be a part of the flow.
 
shroombee said:
Was thinking of testing 10 minutes, 1 hour, 72 hours. But I only have two runs of 50 grams. So I'm open to suggestions of which basing time to try first, and then what to try second based on the results of the first run's yield.
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How about 10 minutes and 72 hours?

69ron's Limonene TEK claims we only need to "mix the paste for about 5 minutes" when using that solvent, so maybe that is also enough time here (?).

I kind of hope 10 minutes (or 5 minutes) has the same yield. Then we could do speed runs (raw cacti to dry white crystals in 1 hour?). It is kind of silly, but would be fun to do:

- 10 minutes alkaline paste
- 20 minutes pulling
- 5 minutes salting
- 5 minutes filtering/washing
- 20 minutes drying (squeezing filter between paper towels too speed up the dry)

Also, just a note since I brought up bufotenine. With that tek, the alkaline paste is completely dried. However, when I completely dry mescaline and try to pull with acetone or limonene it doesn't work (have not tried it with ethyl acetate). This is reversible though, and adding water makes the pull work. It is as if some water is needed to keep mescaline in a true free base form (?). Also, we have found that mescaline likes some water to precipitate from ethyl acetate.
 
Did my speed run today. Was fun! Used 15mg/g for salting to minimize xtals on walls. Still got some on the walls (a small uniform dusting) which I'll recover that later.

Yield was 1.05% after a grand total of 56min 🌵♥️✨
 
Loveall said:
Did my speed run today. Was fun! Used 15mg/g for salting to minimize xtals on walls. Still got some on the walls (a small uniform dusting) which I'll recover that later.

Yield was 1.05% after a grand total of 56min 🌵♥️✨
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Nice! This process wins the title for Fastest Tek. :thumb_up: This was a 10 minute basing? Is the yield comparable to yields from 24 hours basing?

In my experience, the dust from a 15 mg/g salting does not amount to much.

Also, just a note since I brought up bufotenine. With that tek, the alkaline paste is completely dried. However, when I completely dry mescaline and try to pull with acetone or limonene it doesn't work (have not tried it with ethyl acetate). This is reversible though, and adding water makes the pull work. It is as if some water is needed to keep mescaline in a true free base form (?). Also, we have found that mescaline likes some water to precipitate from ethyl acetate.
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I've read that freebase mescaline may oxidize under drying conditions and then becomes inactive, so I haven't looked much into teks that dry the paste.
 
Yeah was about 10 minutes of paste, maybe a little less.

After a while, a little bit more crashed from the salted and filtered extract. Not much though. I'll recover that (plus the little bit on the walls) at some point.
 
Loveall said:
After a while, a little bit more crashed from the salted and filtered extract. Not much though. I'll recover that (plus the little bit on the walls) at some point.
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Does this imply the extract should be left to sit for some period of time before filtering? On my last run I let the salted extract sit for at least 45 minutes before pouring into the filter.
 
shroombee said:
Loveall said:
After a while, a little bit more crashed from the salted and filtered extract. Not much though. I'll recover that (plus the little bit on the walls) at some point.
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Does this imply the extract should be left to sit for some period of time before filtering? On my last run I let the salted extract sit for at least 45 minutes before pouring into the filter.
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In my case yes, this is one thing that limited the speed run yield (which was ok though). Salted pulls were pretty clear based on how light was shining through, but still kept on crashing for a while.

One can always filter and keep the extract to see if anything keeps on crashing.

One important thing I forgot to mention: I did decant the pulled extract one extra time before salting as some small water drops formed / stuck to the bottom of the jar pretty quickly in the combined pulls. This check/step is part of the general TEK.
 
Loveall said:
One important thing I forgot to mention: I did decant the pulled extract one extra time before salting as some small water drops formed / stuck to the bottom of the jar pretty quickly in the combined pulls. This check/step is part of the general TEK.
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Interesting... I haven't seen water droplets form this quickly. I wonder if your observations are related to the 10 minute basing?

I've also had the theory that more combined pulls (I'm doing 6 right now) reduce the overall percentage of water in the combined extract because pulls #5 and #6 absorb less water. This theory is not based on any scientific knowledge or tests yet. Just a conjecture because I'm the only one who does 6 pulls, and with appropriate salting I am getting immediate crashing with excellent yields.
 
shroombee said:
Loveall said:
One important thing I forgot to mention: I did decant the pulled extract one extra time before salting as some small water drops formed / stuck to the bottom of the jar pretty quickly in the combined pulls. This check/step is part of the general TEK.
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Interesting... I haven't seen water droplets form this quickly. I wonder if your observations are related to the 10 minute basing?

I've also had the theory that more combined pulls (I'm doing 6 right now) reduce the overall percentage of water in the combined extract because pulls #5 and #6 absorb less water. This theory is not based on any scientific knowledge or tests yet. Just a conjecture because I'm the only one who does 6 pulls, and with appropriate salting I am getting immediate crashing with excellent yields.
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I tried to be gentle, buy I may have squeezed a bit too much, causing the tiny droplets. They were very small and stuck to the glass.

They are hard to see, had to shine a flashlight and look at a certain angle to see them. However they stuck to the glass and were easy to decant off to the next jar which is where I did the salting.
 
Speed run update:

- 115mg more xtals crashed overnight. The process appears to be done. I'll keep an eye on the salted extract for a week to make sure it is really done crashing.
- 106mg where recovered from the walls of the speed run crashing jar with using warm water and slowly evaporating it to needles.

So a delta of 0.22% out of 1.27% total yield (~1 in 6 parts) was left behind during the speed run in this example.

So far I'm finding 10 minutes for the paste is enough. I am starting to think that letting the combined pulls rest overnight in the fridge and decanting could help make the process more robust for some people (less water/stray particles that could interfere with xtalization). I don't see any indication of FB mescaline reacting with ethyl acetate in the fridge after one night. I also think that even though the bulk of the crystalization is indeed fast, allowing a longer crystalization in the fridge (overnight) can get a little more yield. Finally, rinsing the walls also helps with yield even at 15mg/g crystalization (in my example).

Next, I plan to put this all together and see if I get 1.2% + yields repeatedly. I will try one more long pasting too where I don't change anything else.
 
A little update, a bread dish that had water evaporating from the stuck crystals is showing little crystal spider webs. It has been sitting about a week, and when it evaporated After about 2 days, it turned to a sticky goo. But I just left sitting, and checked it yesterday. There are several little spots of spiderweb looking crystal dotted throughout the goo puddle. It’s still to sticky to scrape up, similar consistency to acacia spice goo. But now I’m confident my cactus has goodies in it. I’ve yet to try the bit of crystal I was able to get in the beginning as plans fell through on Friday. Will report when bio assayed.
 
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