TEK Ethyl acetate approach [CIELO]

[Loveall]

I just took it today. A Sunday afternoon 250mg dose and definitely feeling it

Nice. Enjoy your journey! :thumb_up:

Thanks. It was a good time at the beach

 

[Loveall]

Quick report: I took 250mg around 12:30pm and another 250mg at 5pm.

Felt strong energy throughout my body. Made love to my wife for a much longer time than usual thanks to the flowing energy from mescaline, sex and orgasm where both strongly enhanced. Beautiful visuals at night if focusing inwards. Felt effects until 6am .

No stomach discomfort, feeling refreshed the next day despite the intense experience and only getting a couple hours of sleep.

Good stuff. Feeling grateful and thankful today.

 

[downwardsfromzero]

Here's a tantalising update: butyl acetate is showing more than a hint of promise. A small test run with a completely rotten PC pach has indications of interesting crystals. This was somewhat confounded by an excess of citric acid having been added - way in excess of its solubility in BuOAc. Nonetheless, the finely powdered citric acid reformed into larger crystals, most likely from the dissolved water in the solvent. Crystals of a noticeably different appearance formed promptly next to the heap of citric acid, as well as on the walls of the jar after overnight refrigeration.

Presumably, an ice cold acetone wash or three might clear up much of the excess citric as well as the residue of butyl acetate, which has the added disadvantages of being not only far less volatile than ethyl acetate but its lower surface tension and higher viscosity make it somewhat sticky as solvents go. These physical properties also led to a spillage due to its behavior on pouring being somewhat different from expectations.

That stuff eats ABS, acrylic and polystyrene for breakfast, btw

It's possible to include some numbers for this experiment although the lack of a final yield figure, as well as certain wild deviations from the CIELO method, make this somewhat pointless in my view.

One small technical development that might be of interest: the cactus/lime mixture was initially far too liquid. It was possible to correct this by addition of a little extra lime and some straight-from-the-jar Epsom salts. This reacted to produce gypsum (plaster of Paris) and magnesium hydroxide and brought the mixture to an easily workable, smooth paste consistency.

After all the pulls had been made, the mixture retained roughly 75 wt% of solvent relative to dry cactus mass. On standing overnight it separated into two (unworkable) liquid phases and some sludge. Butyl acetate will hydrolyse rather more slowly than ethyl acetate, fwiw.

The pulls themselves were a pleasant, crystal clear, pale yellow-green colour - something of a surprise considering the revolting brown sludge that the starting material was.

 

[Loveall]

Here's a tantalising update: butyl acetate is showing more than a hint of promise. A small test run with a completely rotten PC pach has indications of interesting crystals. This was somewhat confounded by an excess of citric acid having been added - way in excess of its solubility in BuOAc. Nonetheless, the finely powdered citric acid reformed into larger crystals, most likely from the dissolved water in the solvent. Crystals of a noticeably different appearance formed promptly next to the heap of citric acid, as well as on the walls of the jar after overnight refrigeration.

Presumably, an ice cold acetone wash or three might clear up much of the excess citric as well as the residue of butyl acetate, which has the added disadvantages of being not only far less volatile than ethyl acetate but its lower surface tension and higher viscosity make it somewhat sticky as solvents go. These physical properties also led to a spillage due to its behavior on pouring being somewhat different from expectations.

That stuff eats ABS, acrylic and polystyrene for breakfast, btw

It's possible to include some numbers for this experiment although the lack of a final yield figure, as well as certain wild deviations from the CIELO method, make this somewhat pointless in my view.

One small technical development that might be of interest: the cactus/lime mixture was initially far too liquid. It was possible to correct this by addition of a little extra lime and some straight-from-the-jar Epsom salts. This reacted to produce gypsum (plaster of Paris) and magnesium hydroxide and brought the mixture to an easily workable, smooth paste consistency.

After all the pulls had been made, the mixture retained roughly 75 wt% of solvent relative to dry cactus mass. On standing overnight it separated into two (unworkable) liquid phases and some sludge. Butyl acetate will hydrolyse rather more slowly than ethyl acetate, fwiw.

The pulls themselves were a pleasant, crystal clear, pale yellow-green colour - something of a surprise considering the revolting brown sludge that the starting material was.

That's an interesting result. Maybe anhydrous acetone is good enough to clean up the xtals you got. If you get enough you can bioassay.

Those secondary xtals sure sound like the active product shroombee and I are getting with ethyl acetate (with Metta-Morpheus and grollum pending).

Edit: Did cloudiness form after adding citric acid?

 

[downwardsfromzero]

Did cloudiness form after adding citric acid?

It's hard to say because the citric acid had been finely ground before addition as an attempt to make up for its poor solubility. Because of the small amount of what can reasonably be suspected to have been weak material there would only have been a low concentration of dissolved alkaloid making any additional cloudiness rather hard to discern.

The solvent pulls have stood in the refrigerator for a couple of days now and there are very clearly visible small, super-sparkly crystals around the side of the jar. Solubility tests with ice cold acetone are in the pipeline, as is a follow-up extraction with a larger amount of dried, powdered but nonetheless still pre-decayed material from specimens that were previously confirmed as active.

If you get enough you can bioassay.

A reasonable estimation of the absolute maximum yield from the cactus used I would put at 100mg.

On standing overnight it separated into two (unworkable) liquid phases and some sludge. Butyl acetate will hydrolyse rather more slowly than ethyl acetate, fwiw.

The cactus paste on standing for a couple more days has shifted from the fruity ester scent of the butyl acetate to the altogether more sickly aroma of butanol. We can safely conclude that calcium hydroxide does indeed catalyse hydrolysis of butyl acetate, and by extension this will undoubtedly be the case with ethyl acetate as well.


>>>>Does anyone have solubility data for mescaline citrate in ethanol?<<<< Pretty please!


Handy link: Solubility of citric, malonic, and malic acids in different solvents from 303.2 to 333.2 K (downloads pdf)

 

[Loveall]

I don't have solubility data for mescaline citrate in ethanol. Don't have high % ethanol to measure it either.

 

[shroombee]

I have 200 proof ACS/USP ethanol (at least until I break the seal and open it).

Given I have slightly impure mescaline citrate, what would the steps be in getting us to usable solubility data?

 

[downwardsfromzero]

I don't have solubility data for mescaline citrate in ethanol. Don't have high % ethanol to measure it either.

No worries!

I have 200 proof ACS/USP ethanol (at least until I break the seal and open it).

Given I have slightly impure mescaline citrate, what would the steps be in getting us to usable solubility data?

Thanks for the offer.

For a rough figure, measure 10g of solvent into a beaker then keep adding increments (ideally, measured) of solute with stirring until some doesn't dissolve. Some guesswork might be necessary at first in order to determine a sensible size for the increments. With weighed increments the amount of solute added divided by 10 gives the solubility per gram of solvent. Otherwise, weigh the solution, etc.. It is, of course, helpful to measure the temperature of the solution at this point.

This can be tedious and time-consuming if the solute dissolves only slowly. If you have azeotropic (190 proof) ethanol, use that because the hygroscopicity of absolute (200 proof) EtOH will skew your results anyhow. Most people - myself included - will find it easier just to use azeotropic ethanol. That's not to understate the usefulness of a figure for both kinds of ethanol, of course, but if you have a specific purpose for your absolute ethanol I'd suggest saving it for that.

Perhaps you could do a simple water re-x on the mesc.citrate first if you think it's too impure.

https://www.crystallizationsystems....ization Systems_White Paper on Solubility.pdf >>> links to a pdf about solubility testing methods.


Now all I have to do is remember why I thought I needed the solubility data in the first place

 

[shroombee]

Thanks for the offer.

Happy to help!

if you have a specific purpose for your absolute ethanol I'd suggest saving it for that.

I don't necessarily have a purpose for 200 proof ethanol. That's just what the supplier offered. I'm planning to use it for e-mesh DMT ethanol and to play with psilocybin extraction. How long does it stay 200 proof once I open it?

Perhaps you could do a simple water re-x on the mesc.citrate first if you think it's too impure.

I'm fairly certain it is not 100% mescaline citrate. When I bio-assayed 2 weeks ago, the first 1-2 hours was sedating/stony so that matches the effects and timing descriptions of non-mescaline alkaloids. The product is fairly white though, if that's any indication that at least it's not terribly impure.

How does a water re-x clean the product? I dissolve in water, pour in a dish, evaporate slowly to get nice clear xtals. But won't the impurities still be mixed in?

 

[Loveall]

I'm fairly certain it is not 100% mescaline citrate. When I bio-assayed 2 weeks ago, the first 1-2 hours was sedating/stony so that matches the effects and timing descriptions of non-mescaline alkaloids. The product is fairly white though, if that's any indication that at least it's not terribly impure.

That would be different than the mass spec results we have so far. Are you sure mescaline wouldn't come online that anyway? I feel an excited energy as it comes on, but it could be different between folks intially as the dose I'm the body ramps up. It would be interesting if you had an analysis done.

I still plan to send a sample for analysis on the more finalized TEK after we:

- Settle on the basing time (10min, 24h, longer?)
- Rest and decant in fridge overnight before salting. I think this may help get more consistent results, especially if folks go against current recomendations and squeeze too hard with the french press (which is subjective) or pull right after stirring).
- 6.66mg/g salting
- Allow a few more xtals to form overnight

Also, I'm getting tired of rinsing the walls with water. The needle xtals are pretty, but it is an extra step. I'm gonna go back to salting in the shallow baking dish so I can simply scrape after the fresh ethyl acetate washes.

 

[AiL762]

Don't mind me, subbing for now so I don't lose or flat out forget about this. Looking forward to reading and giving it a try!

Thanks ahead of time!

 

[shroombee]

Results from my latest Run #5.

Purpose

1) Investigate yield with 72 hour basing time versus the 24 hour basing time of Run #4;
2) Determine yield from pulls #1-4 versus pulls #5-6;
3) Is there any difference with getting xtals in the high freebase pulls (1-4) versus low freebase (5-6);

Constants with the previous run we're comparing with

- Same source material. Run #5 was powdered with Run #4 to eliminate variations even within the same cactus specimen;
- Pull technique was 30 seconds very light stirring, rest 2 mins and 30 seconds, then decant;
- Decant with a little pressure on the french press to squeeze an extra 10-15 grams of solvent out of each pull;
- Same amount of solvent was added and recovered per pull;
- I'm retrieving basically the same amount of solvent that was added for each pull (except the first pull in which the cactus holds on to some solvent);
- Salted with 15 mg per gram of extract;
- Aggressive stirring with magnetic stirrer for 10 minutes;

Results

Total yield was 1.60% (799 mg out of 50 grams Peruvian Torch).

1) There is NO DIFFERENCE in yield between 24 hour basing and 72 hour basing. Yields between Run #4 and Run #5 were well within the margin of error in my weighing, filtering, and collection techniques. I also didn't observe any difference in the texture or workability of the cactus between 24 and 72 hour basing;

2) 88% of the total yield is retrieved in pulls #1-4. The other 12% from pulls #5-6. For the material I'm using, pulls #5-6 would give me nearly 200 mg product from 100 grams cactus (12% of 1,600 mg). So its possibly worth the extra 6 minutes of pulling effort and additional solvent. Or I might try 4 pulls where the 4th pull is more solvent and/or additional pulling time. Or maybe 4 pulls of around 4.5 minutes each (total 18 minutes equaling 6 x 3 minute pulls);

3) There is no xtalization or overall yield difference in salting pulls #1-4 separately from pulls #5-6. I thought the freebase concentration or a different water content might complicate xtal formation, but not so;

Next Steps

I can do one more run using this same source material. I think I'll try a 1-hour basing and keep everything else the same.

Edit: Took a while, but I finally got around to doing a followup run with 15 minute basing. Results are here.

 

[Loveall]

Thanks, excellent data shroombee. One question how many grams of solvent where you recovering (~75g?).

We can use it to calculate the p value.

Wolfram alpha solves it to be p = 0.334

So with each pull we recover ~1/3 of the mescaline remaining.

For this value, 6 pulls would be recommended to get >90% of the total Mescaline.

More precisely, after 6 pulls, you where at ~ 1-(1-p)^6 ~ 91.2% recovery of the grand total.

Therefore, there should be only ~78mg left in the paste after 6 pulls. A 7th pull would recover ~ 26mg - not worth doing in my opinion.

Looking forward to your next result with 1 hour.

 

[shroombee]

One question how many grams of solvent where you recovering (~75g?).

Loveall, thanks for the feedback and doing the pull calcs.

Solvent addition and recovery for Run #5:

Pull #1: Added 150.7 grams, recovered 117.6;
Pull #2: Added 100.1 grams, recovered 100.6;
Pull #3: Added 101.5 grams, recovered 102.4;
Pull #4: Added 101.6 grams, recovered 102.4;
Pull #5: Added 100.7 grams, recovered 98.3;
Pull #6: Added 100.9 grams, recovered 100.2;

For clarification on my process and the precise numbers:

Pulls #1-4 were combined. Pulls #5-6 were combined. Then split into the following jars and salted separately:

Jar (A): 50% of the volume of combined pulls #1-4;
Jar (B): 50% of pull #1-4 plus 50% of pull #5-6;
Jar (C): 50% of combined pull #5-6;

Thus yield of (A) + (C) should equal (B) if freebase concentration or other factors don't affect success of xtalization. Which is what I observed.

Yield of (A): 353 mg (pulls #1-4, 88.5% of A+C yield)
Yield of (C): 46 mg (pulls #5-6, 11.5% of A+C yield)

Total yield was 399 mg for (A) + (C). Yield of jar (B) was 400 mg.

 

[Loveall]

Thanks shroombee.

We only expect ethyl acetate to carry a few % of water (~3%). I think because of this the ammount of water in the paste does not change enough to make the later pulls have less water in a significant way.

I have another question about salting: How long did you wait to allow it to complete after the 10 minutes of stirring? I believe a small ammount(~100 to 200mg if starting with 100g of cactus) keeps on crashing over 24 to 72 hours. Wondering if you see the same in your examples.

 

[shroombee]

We only expect ethyl acetate to carry a few % of water (~3%). I think because of this the ammount of water in the paste does not change enough to make the later pulls have less water in a significant way.

Makes sense.

I have another question about salting: How long did you wait to allow it to complete after the 10 minutes of stirring? I believe a small ammount(~100 to 200mg if starting with 100g of cactus) keeps on crashing over 24 to 72 hours. Wondering if you see the same in your examples.

After salting with 15 mg/g, I waited less than 30 minutes before filtering. After filtering through the coffee filter, I noticed there are small xtals suspended in the extract that got through the coffee filter.

On jar (C) (pulls #5-6) I let those xtals settle a couple days, carefully decanted the solvent, rinsed the jar with warm water, then evaporated at 95 degrees in the dehydrator. There isn't much yield there. About 17 mg that scrapes up to a thin tacky line of paste at the edge of the razor blade. I figure half of the weight is xtals and the other half is plant oils or whatnot that contribute to the tackiness. I haven't decanted (A) and (B) yet because the amount of settlement visually appears to be the same or less than (C), and thus expected yield is not worth the effort.

But I don't think I'm seeing additional crashing. I think this minor yield is the tiny xtals settling. With 100 grams of cactus it might amount to 100 mg of crude product?

BTW, I believe conveniently recoverable yield may be slightly (2-3%) higher using 5 mg/g rather than 15 mg/g. This is because 5 mg/g provides larger xtals that can be caught by the coffee filter and washed out of the jar. 15 mg/g gives smaller xtals that slip through the coffee filter and float in the extract, requiring the wait and decant process. I base this conjecture on yield and observational differences between 5 mg/g and 15 mg/g. I'll investigate this further in upcoming runs.

 

[Loveall]

Interesting. With 5mg/g it may take longer to finish xtalizing compared to 15 mg/g.

To avoid small xtals passing through the filter AND to adjust for the longer xtalization time, maybe 5 mg/g AND allowing 24h+ to crash is the way to go (?).

 

[shroombee]

Interesting. With 5mg/g it may take longer to finish xtalizing compared to 15 mg/g.

To avoid small xtals passing through the filter AND to adjust for the longer xtalization time, maybe 5 mg/g AND allowing 24h+ to crash is the way to go (?).

This should be easy to test. Combine pulls, split into two separate salting jars, salt both. Filter and rinse the first jar immediately. Wait 24 hours before filtering and rinsing the second jar. Compare yields.

I'm fairly certain it is not 100% mescaline citrate. When I bio-assayed 2 weeks ago, the first 1-2 hours was sedating/stony so that matches the effects and timing descriptions of non-mescaline alkaloids. The product is fairly white though, if that's any indication that at least it's not terribly impure.

That would be different than the mass spec results we have so far. Are you sure mescaline wouldn't come online that anyway? I feel an excited energy as it comes on, but it could be different between folks intially as the dose I'm the body ramps up. It would be interesting if you had an analysis done.

With the mescaline acetate or HCl using lime/limo, I get a combination of the anxious energy with a couple hours of moderate sedative effects. Maybe it comes in waves, I haven't paid that much attention. I get onset yawns with shrooms too so maybe it's an individual thing. This weekend I might try 500-600 mg of citrate and I'll see how that compares to the 300 mg from a couple weeks ago. Will also have analysis done soon.

Quick report: I took 250mg around 12:30pm and another 250mg at 5pm.

Felt strong energy throughout my body. Made love to my wife for a much longer time than usual thanks to the flowing energy from mescaline, sex and orgasm where both strongly enhanced. Beautiful visuals at night if focusing inwards. Felt effects until 6am .

No stomach discomfort, feeling refreshed the next day despite the intense experience and only getting a couple hours of sleep.

In general, psychedelics do seem to activate sexual energy. And in my experience, mescaline is a strong aphrodisiac. I appreciate that it is non-addictive though, and I don't feel the need to chase the mescaline aphrodisiac high.

 

[Loveall]

I tried this approach starting with fresh whole peruvian and bridgesii (mostly SS01xS002xbridgesii seeds from misplant).

Cacti were stored in a paper bag in the garage over 5 months. 2649g were chopped into stars (1st image) and dehydrated with spines and all (second image, near the end of dehydration). After grinding, 120g of cactus powder was obtained (3rd image). The cactus was 95.4% water.

The CIELO tek was used to extract this powder. Observations/results:

1) More citric acid was needed for xtalization compared to san pedro outer skin chips (had to go up from 6mg/g to ~ 20mg/g). Not sure why this is, but that is what happened. I've updated the tek to be 20 mg/g so it works in more situations.
2) Almost all of the product stuck to the wall. A lot of it looked like water drops (especially towards the top of the jar), but is solid xtaline (4th image).
3) Final product is xtaline and slightly bitter but a little sticky (5th image). Not sure if that is because whole plants were used or because this is peruvian/bridgesii instead of San Pedro pachanoi.
4) Bioassay and analysis pending. Expecting an active product based on experience with San Pedro skin chips.
5) Yield was 960mg (0.8%). I think this is a good yield if using whole plants (instead of outer skin chips) based on reference data.

Overall, very happy with how easy it was to extract my peruvian x bridgesii plants from last year

 

[shroombee]

Nice work Loveall!

1) More citric acid was needed for xtalization compared to san pedro outer skin chips (had to go up from 6mg/g to ~ 20mg/g). Not sure why this is, but that is what happened. I've updated the tek to be 20 my/g so it works in more situations.
2) Almost all of the product stuck to the wall. A lot of it looked like water drops (especially towards the top of the jar), but is solid xtaline (4th image).

I'm thinking I like 5 mg/g (if it crashes) because the xtals are bigger and get caught in the filter. Whereas 15+ mg/g produces smaller xtals and thus decanting is necessary if you want every last bit of product. Did you observe tiny xtals floating in the extract after you ran it through a filter? Maybe the tek should point that out as two salting options.

Do you mind if I start an FAQ section of the tek to answer questions like "will longer basing time yield more product", et cetera. I'd like to add experimental data to the answers to show people we tested some variations.

Odd that all the product stuck to the walls. Perhaps there are more plant oils present?

5) Yield was 960mg (0.8%). I think this is a good yield if using whole plants (instead of outer skin chips) based on reference data.

Loveall, you're observing higher yields with CIELO than the other teks you've tried, correct? And if so, are the general numbers people report for extraction yield all too low because they all leave product on the table using less effective teks? And had everyone been using CIELO, we would generally be quoting higher numbers for average mescaline content?

Sort of like, we've all been looking at the night sky without a telescope, and reporting that there are thousands of stars in the galaxy. But then someone invents the telescope and we realize there are billions?

I've never worked with fresh cactus before. Is there any special technique for cutting those clean stars without poking yourself with the spines?