TEK Ethyl acetate approach [CIELO]

[shroombee]

So I’m not fully confident in my results. Maybe it’s not fully dry yet. But I have a final weight if 1.29 grams off 100 gram cactus(Pretty high) and these crystals are very sticky. I can mold them into a ball, and my fingers are slightly sticky after doing so.

1.29% appears to be a reasonable yield with this tek when everything works as expected. My experience is that multiple crash attempts usually result in less yield. So I'm guessing you may have some plant oils or citric acid in there.

Did you do a few washes with fresh ethyl acetate when the product was sitting in the coffee filter before evaporating?

If I were to do a bio assay, it would be safe to assume that at worst case I’m eating a big ball of citric acid right?

You would probably be eating a big ball of Sour Patch Kid candy and maybe a little cactus oil. All the ethyl acetate should evaporate clean, and it's used for food processing anyhow. Did you use food safe ethyl acetate?

In case any lime got into the solvent, what's the reaction of lime with citric acid?

Also, the filter has an oily stain leftover where the crystals were collected. Attached is pic.

When I put my earlier (failed) attempts into the frig, after several hours I would get a small bubble of water or oil droplets spread across the bottom of the dish. These attempts didn't have enough acid and I didn't mix thoroughly. If our attempts are similar (you didn't get crashing and you put the salted solvent into the frig), you might be looking at some separation of plant oils from the solvent.

Try washing your product a few times with fresh ethyl acetate. Dissolve the product in 10 ml of ethyl acetate. The ethyl acetate may turn cloudy. You should have substantial solid material that won't dissolve - that should be mescaline citrate. Decant the cloudy ethyl acetate washes and evaporate (or you can pour it all through a clean coffee filter to separate). The wash evaporation might be a hard clear film. Maybe a little oil.

Evaporate the solids separately (this should be mostly good stuff). You can use a little water to get all the solids out of the wash container.

 

[Loveall]

So I’m not fully confident in my results. Maybe it’s not fully dry yet. But I have a final weight if 1.29 grams off 100 gram cactus(Pretty high) and these crystals are very sticky. I can mold them into a ball, and my fingers are slightly sticky after doing so.

Flavor is a little more bitter than earlier, but still a sour forefront. They are slightly off white in color.

If I were to do a bio assay, it would be safe to assume that at worst case I’m eating a big ball of citric acid right?

Also, the filter has an oily stain leftover where the crystals were collected. Attached is pic.

I don't think that yield is necessarily too high, we have been getting 1% regularly. Citric acid should not crash from ethyl acetate that has some water in it until >5% I believe. I don't think you got close to that.

I think you have mostly product, with some impurities from the solvent/water. Maybe your extraction had more water than usual (maybe because of the squeezing?) pulling more stuff that is not easy to rinse away/remove with the ethyl acetate filter rinsing method.

First thing I would try is pressing the xtals with a clean new filter. Does more oil move to the paper? If yes I would rub the xtals holding the filter with the palms of my hands and rubbing.

You can also drop the product in fresh ethyl-acetate and stir that for a while. Any remaining excess citric should definitely go into solution. Hopefully the sticky stuff does too. Decant/filter and see if the product feels/tastes better.

Or you can dissolve in minimal water. You can check pH then. Decant anything that doesn't dissolve and dry slowly, see if you get long needles.

Or you can bioassayed as is. As long as ethyl acetate has evaporated, I don't think there is anything other than citrate salts, a small amount of residual citric acid, and plant residue.

I wonder if we can make the process more robust by adding CaCl2 to the initial paste. That would keep even more water out of the pulls I believe, maybe avoid the "water" droplet issue you saw (?). I did not see a benefit to doing that, but never had your issue either. Or maybe simply letting the solvent sit in the fridge before salting so the droplets can collect and be decanted off would help avoid the issue you encountered.

 

[Loveall]

In case any lime got into the solvent, what's the reaction of lime with citric acid?

There should be no lime in the solvent pulls. If there were, the result would be inactive calcium citrate (used a as a calcium supplement "citracal" for people with weak bones at 1 g/day).

If lime were getting into the solvent the pulls would never end since there is a large source of calcium. It should not happen unless crumbs of the paste itself are falling into the extract unnoticed.

 

[shroombee]

There should be no lime in the solvent pulls. If there were, the result would be inactive calcium citrate (used a as a calcium supplement "citracal" for people with weak bones at 1 g/day).

If lime were getting into the solvent the pulls would never end since there is a large source of calcium. It should not happen unless crumbs of the paste itself are falling into the extract unnoticed.

Okay - just wanted to be sure in case Metta-Morpheus decides to bio assay his product.

 

[shroombee]

Finals results from Run #4 (I realized I should call these "Runs" to avoid confusion with different batches of cactus).

Summary: 50 grams powdered Peruvian Torch, 24 hours basing, 6 x 3 minute pulls, combined pulls split into two jars, salted with either 15 mg/gram or 5 mg/gram, aggressive mixing with magnetic stirrer. Photo shows the two coffee filters.

Run #4, Jar (A)
- Salted with 15 mg/gram;
- 390 mg of nearly white fluffy xtals from coffee filter;
- 27 mg of evaporated residue from the jar which was slightly oily, so I'm tossing this;
- Total yield: 390 mg out of 25 grams = 1.56%

Run #4, Jar (B)
- Salted with 5 mg/gram;
- 393 mg of nearly white fluffy xtals from coffee filter;
- 17 mg of evaporated residue from the jar, which seems like legit product;
- Total yield: 410 mg out of 25 grams = 1.64%

For comparison, here is Run #3 (22 hours basing, 6 x 10 minute pulls):

Run #3, Jar (B)
- Salted with 5 mg/gram;
- Yield 1.46% (actually should be a little lower because I forgot to wash the xtals)

Run #3, Jar (D)
- Salted with 20 mg/gram;
- Yield 1.41% (actually should be a little lower because I forgot to wash the xtals)

Observations:

- There is no green ring on the coffee filters for Run #4 versus Run #3, possibly due to the faster pulls not extracting green material from the cactus. In Run #3, the green ring for the 20 mg/g salting was thicker than the jar salted with 5 mg/g;

Edit: There is a faint green ring for Run #4, Jar (A) which was salted with 15 mg/g. Jar (B) has a couple green marks. The ring being more prominent from the jar having the additional citric acid is consistent with Run #3. The green is less for Run #4 versus Run #3, possibly due to the faster pulls not extracting green material from the cactus.

- 5 mg/g citric seems to have slightly higher yield than 15 or 20 mg/g;
- 5 mg/g citric needs a jar wash and evaporation to get the last bit of xtals whereas 15+ mg/g does not yield anything substantial with the jar wash;
- Average of 1.6% yield from Run #4 seems high. Although 6 pulls may have helped;
- I will repeat these tests and if I get the same results I should have the product analyzed;

Why is the yield from Run #4 higher than Run #3? Some differences to consider:

- Pulls are 6 x 3 minutes for Run #4 and 6 x 10 minutes for Run #3. From looking at the pH strips, it appeared the longer 10 minute pulls had more freebase (greener pH strips). Maybe not?

- With 6 x 3 minutes pulls, the cactus stays crumbly. With 6 x 10 minute pulls, the cactus gets sticky around pull #4. Perhaps the stickiness makes the pulls less effective.

- Run #4 was a fast process where I salted the extract immediately after pulling and filtered the xtals out of the solvent a few hours later. Run #3 was slow. I didn't salt the jars for nearly 48 hours. After getting xtals I put the jars in the frig and so didn't filter the xtals for 24 hours. There is possibly a pattern where taking longer to salt and filter xtals may reduce yields. Not sure if this is just coincidence.

 

[Loveall]

Wow shroombee, this is great. Did you get a chance to taste the xtals? Will you be doing the warm water and slow evaporation to see what you get that way? Looking forward to any analysis or bioassay results should you do that in the future.

I have also observed that yields are slightly better if pulls are quick and the paste is not given time to become sticky. I updated the experimental tek to have 3 minutes pulls. Also updated the reaction paste time to 24h. Your yields are great (assuming the analysis comes back same as mine).

One question: how long do you think it took for xtalization to complete and for the solution to become clear with aggressive stirring?

Do you know what kind of yield you would get with a limo or xylele tek with the cactus you are using?

Thank you so much for your contributions to this process and dedication.

Edit: I think I see a faint green ring on your picture of run #4. About 2/3 of the way up. Visible near the ~one to two o'clock position on both (left one is easier to see).

 

[shroombee]

Wow shroombee, this is great. Did you get a chance to taste the xtals?

Xtals taste mildly bitter. Not as bitter as the typical sticky, sometimes oily product I get from lime/limo vinegar or HCl salting. Texture is fluffy and the pieces break up easily.

Will you be doing the warm water and slow evaporation to see what you get that way? Looking forward to any analysis or bioassay results should you do that in the future.

I have a couple more runs to do with the 100 grams I powdered with this Run #4. At least one of the runs I'll do a warm water, slow evaporation. Bio assay maybe this weekend. 8) And will send a sample for analysis.

I have also observed that yields are slightly better if pulls are quick and the paste is not given time to become sticky. I updated the experimental tek to have 3 minutes pulls. Also updated the reaction paste time to 24h. Your yields are great (assuming the analysis comes back same as mine).

Have you done a 24 hour basing with 3 minute pulls yet? Next run I will salt 4 pulls separately from the last 2 pulls to see how much 2 extra pulls is giving us.

BTW, I saw you wrote in the tek to intermittently mix during the 24 hour basing. I haven't tried that. I put the cactus in a sealed mason jar and let it sit until ready for pulling.

One question: how long do you think it took for xtalization to complete and for the solution to become clear with aggressive stirring?

I wrote about this a bit in a post from last night. I'm fairly certain all the xtalization is complete by the time I stop magnetic stirring after 5 minutes. I checked and saw lots of snow orbiting the jar and it appears the solvent is clear. But hard to tell if it's 100% clear because there is so much snow floating around. After 5 more minutes spinning and then letting the snow settle for 5-10 minutes, the solvent is definitely clear.

So when does the solvent first become clear? It could be as quick as 3 minutes? Maybe less? I'll pay attention to this on the next run.

Do you know what kind of yield you would get with a limo or xylele tek with the cactus you are using?

I don't have good data on this batch using lime/limo tek. And even if I did, we wouldn't know the purity of the end products to make a fair comparison. I haven't played with xylene. Best approach is to have this yield analyzed.

Thank you so much for your contributions to this process and dedication.

You too - thanks for being the inspiration and having patience as we worked through the initial issues!

I think I see a faint green ring on your picture of run #4. About 2/3 of the way up. Visible near the ~one to two o'clock position on both (left one is easier to see).

Good catch. I updated my previous post to comment on this.

 

[Loveall]

shroombee, I updated the TEK based on your input.

Mildly bitter is also how I would describe the taste of what was sent for analysis and came back as mescaline citrate.

 

[metta-morpheus]

I based another 100 grams last night, and will run the pulls when I get home from work. Will be around 18 hours of sitting. I am gonna try digging out my digital ph meter, maybe both the dry and liquid meters, to try getting more precise ph readings on both the ethyl and the paste.

Has the ph already been tested for the paste, or is it even relevant?

Also, my crystals are still quite sticky after several more washes. A side observation, I spilt a little of the green ethyl solution, and after the ethyl evaporated, it left a little sticky residue. Maybe some of that made it into my crystals?

 

[downwardsfromzero]

Exciting stuff.

I've mulled over some of the technical aspects in the past 24hrs. Forgive me if you've covered these simple ideas in the thread already but I'm in no frame of mind (fortunately in a good way ) to go through the thread to check.

The difference between the 3 minute pulls and the 10 minute pulls is paramount. With the longer pulls there is over 3 times the contact time with the lime, which despite its poor solubility is still as we know a strong base. This will react with the ethyl acetate to form calcium acetate and ethanol - and further base will dissolve to maintain equilibrium. I think the calcium acetate is likely to be behind the stickiness that develops - perhaps along with the ethanol which will increase the 'wetting' of the paste by the solvent.

In a similar vein, given enough time freebase mescaline will react with ethyl acetate to produce ethanol and N-acetylmescaline. It seems you've intuited this already by going straight from pulls to salting, but I think it's important enough to state for anyone who might be interested in testing this method themselves. N-acetylmescaline would represent a technical loss of yield. There's every chance it would remain in solution after the salting and it would be interesting to see if it's a component of the oily evaporation residue.

 

[Loveall]

I based another 100 grams last night, and will run the pulls when I get home from work. Will be around 18 hours of sitting. I am gonna try digging out my digital ph meter, maybe both the dry and liquid meters, to try getting more precise ph readings on both the ethyl and the paste.

Has the ph already been tested for the paste, or is it even relevant?

Also, my crystals are still quite sticky after several more washes. A side observation, I spilt a little of the green ethyl solution, and after the ethyl evaporated, it left a little sticky residue. Maybe some of that made it into my crystals?

I wonder why you got sticky stuff on the xtals. Could be from the squeezing, or maybe not all cacti are as clean with this tek (what kind of cacti do you have?). Sometimes when gunk dries it changes and is not as soluble. I assume you did not let the xtals in the filter dry before washing, right? I think the ideal washes should be done while the xtals are still wet with solvent (since once it evaporates residual citric acid and goo may be harder to get back into solution).

This time you could let the solution settle in the fridge for a few hours before salting. If any droplets or paste particles settle at the bottom, you can decant them before salting. One time I almost didn't see some paste crumbs that gotten into extract, I imagine they would have made a mess while salting. They were easy to decant off, and then I salted without issues.

You may already know this, but ethyl acetate can dissolve plastic pH meters and break them, I've broken one of the cheap plastic pH meters this way I did brush some pH paper on the paste early on and it was purple, the expected pH level of lime.

 

[metta-morpheus]

Ethyl acetate can dissolve plastic pH meters and break them, I've broken one of the cheap plastic pH meters this way I did brush some pH paper on the paste early on and it was purple, the expected pH level of lime.

Duly noted sir. I will not bother breaking mine then. I will report back later, hopefully with good results!

 

[Loveall]

Exciting stuff.

I've mulled over some of the technical aspects in the past 24hrs. Forgive me if you've covered these simple ideas in the thread already but I'm in no frame of mind (fortunately in a good way ) to go through the thread to check.

The difference between the 3 minute pulls and the 10 minute pulls is paramount. With the longer pulls there is over 3 times the contact time with the lime, which despite its poor solubility is still as we know a strong base. This will react with the ethyl acetate to form calcium acetate and ethanol - and further base will dissolve to maintain equilibrium. I think the calcium acetate is likely to be behind the stickiness that develops - perhaps along with the ethanol which will increase the 'wetting' of the paste by the solvent.

In a similar vein, given enough time freebase mescaline will react with ethyl acetate to produce ethanol and N-acetylmescaline. It seems you've intuited this already by going straight from pulls to salting, but I think it's important enough to state for anyone who might be interested in testing this method themselves. N-acetylmescaline would represent a technical loss of yield. There's every chance it would remain in solution after the salting and it would be interesting to see if it's a component of the oily evaporation residue.

There could be something to this. It may explain shroombee's earlier results where what didn't crash right away (too low citric acid) and rested while troubleshooting never gave very good results (?).

I just measured yields from 24 hour pulls and only got ~0.7%. Looks like I lost 0.3% somehow, maybe because of the reactions you mention and/or maybe because the paste congealed.

The more tests I run, the more I like the quick pulls and quick salting (current experimental TEK version). That is working very well so far.

The process is incredible fast. Starting with the alkali paste, the pulls/salting/xtalization can all be done in 45 minutes. After one hour I find myself looking at washed white xtals in the filter. If the filter is folded and squeezed dried with a paper towels (like we do with harmalas), dry edible xtals that don't smell like ethyl acetate are available after two hours or so

Metta-Morpheus, maybe don't let the extract sit without salting for too long based on what DWZ is saying. A few minutes should be enough to make sure no cacti crumbs came through or that no water drops are forming before salting.

DWZ, if you want, you can read the TEK's "lab notes". I tired to summarize most of the thread results there for convenience. See if you find any issues with our logic and tentative conclusions. Also, feel free to update that section with your thoughts or observations.

 

[metta-morpheus]

So here is today’s try. I used a magnetic stirrer throughout. Did not squeeze material at the end.

Added 4.5 g citric to about 750 ml green ethyl acetate extract. Instantly saw clouding. Let stir for about 5 minutes

Stopped stirrer. Saw minor salt on glass, and once again the oil/water. Added 1 1/2 grams citric in half gram increments every 3-4 minutes while stirring. A little more goo and salt showed up.

Decanted liquid to new jar, added a small amount (~75 ml)fresh ethyl to jar with goo and salt. Swirled around, then added a small unweighted pinch of citric into it. This seemed to turn a little of the goo into larger chunks of crystal. Tried catching in filter, but all stuck.

Added small amount of hot water to goo and crystal. It all dissolved, even the goo. Glass looks clean, and water looks very slightly off colored. Now evaporating at 170 in the oven.

Out of frustration, I’ve now added an unknown amount (~10g?) of citric acid to the original decanted green ethyl Solution, hoping I would crash something more out. Liquid is still cloudy, only slightly less than after first addition of citric. Hopefully the water dish surprises me, and has something substantial in it.

And side note from yesterday’s run, after leaving the sticky crystal out over night, it has hardened up significantly, to where I can crumble it into a salt looking powder. It now only weighs 1.06, and still is the slightest bit sticky.

 

[shroombee]

So here is today’s try. I used a magnetic stirrer throughout. Did not squeeze material at the end.

A few items to review:

1) What ethyl acetate and citric acid are you using? Lets ensure there is nothing unusual there;
2) After combining all the pulls, are you doing a final filtering before salting to ensure no cactus material snuck into the extract?
3) How did you get the citric acid to dissolve with your first salting? Gently stirring?

I didn't get to post this before you pulled and salted. I was going to suggest splitting your combined pulls into different jars so we can try some salting strategies. Even though I'm getting good yields now, I'm only using 50 grams per run and splitting the extract into a few jars to try different processes. Some ideas:

1) Salt immediately with 5 mg/gram. Shake aggressively (or magnetic stir) for at least 5 minutes, ensuring all the citric acid grains have dissolved;

2) Salt immediately with 20 mg/gram. Shake/stir aggressively as above;

3) Let unsalted jar sit for 24 hours at room temperature and observe if any droplets appear;

Added 4.5 g citric to about 750 ml green ethyl acetate extract. Instantly saw clouding. Let stir for about 5 minutes

Stopped stirrer. Saw minor salt on glass, and once again the oil/water. Added 1 1/2 grams citric in half gram increments every 3-4 minutes while stirring. A little more goo and salt showed up.

So this is about 6.7 mg per gram of solvent, which should be sufficient. I've bombed at up to 20 mg per gram of solvent from the start and gotten good results.

What does the salt look like? Curious that you're getting oil/water during salting. When you say "a little more goo", is that the oil/water? Or something else?

Out of frustration, I’ve now added an unknown amount (~10g?) of citric acid to the original decanted green ethyl Solution, hoping I would crash something more out.

And side note from yesterday’s run, after leaving the sticky crystal out over night, it has hardened up significantly, to where I can crumble it into a salt looking powder. It now only weighs 1.06, and still is the slightest bit sticky.

It's helpful to take some notes and weigh things along the way when troubleshooting this stuff.

What does the powder taste like?

 

[Loveall]

Thanks Metta-Morpheus. Let's keep the tek as experimental until/if we address these recurring droplets after salting.

Unfortunately I have not encountered this before so I cannot troubleshoot it.

What kind of cactus are you using? I'm using simply non-PC San Pedro. Not sure if that matters though.

As I understand it, adding more ethyl acetate helped before, right? It also seemed helped a bit in the more recent run. I wonder if one of the things below could help make the process more robust:

1) adding CaCl2 or NaCl to the paste (~100g). This would separate the ethyl acetate and water better. I did try this and it still works, but removed it as I saw no benefit. It could help those who see the droplets though.
2) adding a solvent drying step before salting would make the process more robust for everyone so it just works (?).
3) Did you try shaking the droplet back into solubion (not just magnetic stirring).


Mescaline citrate does not evaporate very well at 170F in the oven. Instead of xtals it gives a transparent film that does scrape up to xtals. Room temp evaporation does leave needles.

 

[shroombee]

Exciting stuff.

I've mulled over some of the technical aspects in the past 24hrs. Forgive me if you've covered these simple ideas in the thread already but I'm in no frame of mind (fortunately in a good way Big grin ) to go through the thread to check.

Thanks for your thoughts!

The difference between the 3 minute pulls and the 10 minute pulls is paramount. With the longer pulls there is over 3 times the contact time with the lime, which despite its poor solubility is still as we know a strong base. This will react with the ethyl acetate to form calcium acetate and ethanol - and further base will dissolve to maintain equilibrium.

For those of us who dropped out of organic chemistry... :lol: Does further base dissolving mean that more calcium acetate and ethanol is formed, causing more base to dissolve, ad infinitum?

I think the calcium acetate is likely to be behind the stickiness that develops - perhaps along with the ethanol which will increase the 'wetting' of the paste by the solvent.

What does the wetting mean? And how does this affect the system?

In a similar vein, given enough time freebase mescaline will react with ethyl acetate to produce ethanol and N-acetylmescaline.

Any idea how much time this reaction takes?

It seems you've intuited this already by going straight from pulls to salting, but I think it's important enough to state for anyone who might be interested in testing this method themselves. N-acetylmescaline would represent a technical loss of yield. There's every chance it would remain in solution after the salting and it would be interesting to see if it's a component of the oily evaporation residue.

It's a loss of yield because the N-acetylmescaline doesn't further react to form mescaline citrate, and thus this N-acetylmescaline remains in solution, correct?

 

[shroombee]

There could be something to [DFZ's post]. It may explain shroombee's earlier results where what didn't crash right away (too low citric acid) and rested while troubleshooting never gave very good results (?).

Right. With my earlier runs, if I didn't get xtals immediately on the first salting, the frig/freezer/waiting process never gave good results. I eventually did get most everything to crash, but yields were much lower than what I'm getting when I bomb the extract with an excess of citric right away and aggressively magnetic stir.

I just measured yields from 24 hour pulls and only got ~0.7%. Looks like I lost 0.3% somehow...

Interesting result. Perhaps a simple followup experiment that wouldn't require much time or cactus:

1) Run #1: 5 fast pulls. Separate the final 2 pulls to get a baseline yield;
2) Run #2: 3 fast pulls, then 2 very slow pulls with sticky cactus (24 hours each);
3) Compare yield of the last 2 pulls of Run #1 with the last 2 slow pulls of Run #2;

This should pretty much answer the question of whether long drawn out pulls are any benefit with this tek.

 

[metta-morpheus]

Shroombee: I am using lab grade ethyl acetate, and pure anhydrous citric acid. And every pull wa filtered twice, as I filtered into a small jar to weigh recovered solvent to check against what was added, and filter again when adding to the final solvent collection jar. And most stirring was done with magnetic stirrer until the very last swirl with the fresh ethyl.

Loveall: I’m using non pc San Pedro chips that I ground into powder. And I did try a bit of vigorous shaking A couple times to try and get rough with it, but the water was the only thing to make the goo dissolve. I don’t think the goo is water now, as once the ethyl was decanted off, the droplets of this goo were very viscous. And cloudy.

I have plenty of this same material left, so I plan on doing a few more runs. I’ll get this right.

 

[shroombee]

Shroombee: I am using lab grade ethyl acetate, and pure anhydrous citric acid. And every pull wa filtered twice, as I filtered into a small jar to weigh recovered solvent to check against what was added, and filter again when adding to the final solvent collection jar. And most stirring was done with magnetic stirrer until the very last swirl with the fresh ethyl.

Sounds good. If you add 500 mg of citric to 100 grams fresh ethyl acetate, how long does it take for the citric acid grains to dissolve with your magnetic stirrer? I'm curious about this, because it takes a couple minutes for all my citric grains to dissolve even when magnetic stirring. And I recall Loveall saying in a prior post that his citric dissolves easily.

I don’t think the goo is water now, as once the ethyl was decanted off, the droplets of this goo were very viscous. And cloudy.

Interesting. I have never seen viscous, cloudy goo in any jar regardless of salting strategy, frig/freezer, etc.

I have plenty of this same material left, so I plan on doing a few more runs. I’ll get this right.

Sorry you're not having success yet. Please consider doing 50 gram runs to conserve cactus, and splitting the combined pulls into multiple jars to try different strategies. I actually feel bad for my many prior runs of cactus in which I used lime/limo and got poor yields. :lol: Such a waste of a precious resource.