TEK Ethyl acetate approach [CIELO]

[downwardsfromzero]

Loveall, your other option might be to use slightly less CaCl2 after the NaOH. 80g for 45g NaOH is a considerable excess. One of the earlier tests with drying the paste using CaCl2 also had lower yields - IIRC. Do you think you could whizz the paste with a stick blender to break up the big lumps?

 

[Loveall]

Loveall, your other option might be to use slightly less CaCl2 after the NaOH. 80g for 45g NaOH is a considerable excess. One of the earlier tests with drying the paste using CaCl2 also had lower yields - IIRC. Do you think you could whizz the paste with a stick blender to break up the big lumps?

I think previous lower yields where from drying the extract (remove water chemically from ethyl acetate).

I forgot to mention I tried blending the paste (metal blade electric blender) but it was too wet.

Maybe I can simply partially dry it in the oven? Or add more CaCl2 untill it chemichally dries enough to blend (?).

One could ask why bother if the lime paste is working. It's because I think it is worth to make the tek robust and saponification with NaOH helps make very large white xtals. It should be a great starting point for a very robust process I believe. Could be helpful for whole cactus and different cactus sources.

Maybe excess CaCl2 also allows to chill the moist paste to 0F without freezing it solid. Having everything at 0F could make the extract even cleaner (?).

 

[Loveall]

One more option is to microwave the lime paste until it changes color (sign of chlorophyll saponification?). Then (if needed) add CaCl2 until sandy consistency - the microwave may liquefy the paste. Then chill paste to 0F (CaCl2 should avoid freezing) and extract with chilled ethyl acetate.

Since the paste doesn't see NaOH it should not coagulate and hopefully not lower yields.

This may give the extra robustness we want, and it is only a couple extra steps. On the other hand, it may not be as good as NaOH at breaking down plant matter to keep it out of the extract. I think the size and color of the crystals will tell us.

I'm gonna try this next week

 

[Loveall]

On second thought, I won't add CaCl2, too many variables.

Going back through the tread, we established that microwaving removed the green from the extract (also had NaCl, but going to assume that is not needed for now - we'll see). Back them we didn't know that excess citric acid helped with xtalization and we went through a learning cycle to figure that out.

Now I'm putting our learnings into one experiment:

- Lime paste (300g water, 25g, 100g cactus)
- Microwave to remove ~100g of water. This should also breakdown chlorophyll.
- Add 36g of salt per 100g of water remaining
- Cool the paste in freezer
- Pull with chilled ethyl acetate (0F).
- Drop in excess citric acid (4mg/ml)

This may give good yields and huge white crystals. Microwaving to breakdown plant material and cold pulls could give to a robust process that minimizes plant matter and makes things easy/repeatable

Edit: on second thought, I want to put the paste in the freezer. Using NaCl will allow that. So going back to the past from post #1 and pulling with chilled ethyl acetate + salting with excess citric acid drop in method.

 

[downwardsfromzero]

One small question - what size of crystals do you use when adding the citric acid? Some commercial citric acid monohydrate has crystals in the 1-3mm size range whereas anhydrous citric acid is more powdery.


And a further thought - probably another unnecessary complication but there is stuff called soda lime. It is a mixture of solid sodium hydroxide and calcium hydroxide produced by slaking (hydrating) calcium oxide with sodium hydroxide solution, or by treating slaked lime with concentrated sodium hydroxide solution. I now briefly ponder whether this would prevent the paste from coagulating while still breaking down the chlorophyll without needing to microwave. It would then only require a small amount of CaCl2 afterwards to neutralise the excess NaOH.

If someone happened to have soda lime this might be worth trying at least once. It should be fairly readily available due to its use for carbon dioxide removal from closed breathing environments, such as SCUBA rebreathers.

 

[Loveall]

Citric acid grains are about 1mm. Could be the monohydrate.

I did the paste approach in post #286 (microwave + sat NaCl + freezer). Pulled with chilled ethyl acetate. So paste and solvent are all at ~0F.

The paste is almost colorless very minor yellow tint (see first picture). So I think we kept a lot of plant stuff out (there could still be colorless compounds not course).

Dropped in citric acid (3mg/ml), and a thick white cloud emerges and the solution becomes milky (second picture).

This microwaved/chilled process seems very clean. By minimizing plant stuff it should make the process robust for other users and also better for whole plant dry powder. It will also make larger white xtals and the solvent more easily reusable.

It will take 24h for xtals to form and measure yield. I'll update early next week. The NaCl paste was slightly congealed so yields may suffer a little. Going back through the thread, adding CaCl2 gave more sandy paste, so maybe that would be better if we have a yield issue here.

To be clear, the published TEK works so far without Microwaving, cold (not freezing) paste and chilled (~0F) solvent. Just chasing some potential improvements now.

 

[The Traveler]

Love this TEK Loveall!

Thank you all for contributing to it.


Kind regards,

The Traveler

 

[downwardsfromzero]

Love this TEK Loveall!

Thank you all for contributing to it.


Kind regards,

The Traveler

Maybe Loveall's flask icon could now be a golden-green colour? With little sparkles in it? [YOUTUBE]

 

[Loveall]

Thanks The Traveler and DWZ

So far the 0F extract is xtalizing right on schedule. Needles are growing large and white . Here is a picture 4 hours into xtal growth. Will post yield early next week.

 

[downwardsfromzero]

OMGgggggg!! That is gorgeous - indeed!

 

[merkin]

OK, couldnt resist trying this but hit a bit of a snag - no crystalisation...

Have ~900ml cloudy solvent (olive-green tinted yellow). Been sitting at room temp (10-18°C) for over 28hrs now. Added an extra 3g of citric acid two hours ago so there is a little layer of it visible at the bottom of the bottle. Im a bit oncerned I added too much acid.

Does the 4mg/g and 20mg/g refer to g of Ethyl Acetate or g of cactus powder?

My starting material is/was definitely good but now pretty old (over 10 yr). Previously delivered around 1.5%+ tan sanchez through xylene/hcl teks but been in storage since so maybe this is a problem too.

Any recommendations of way forward - or should I just leave it alone and wait longer? thnx

 

[shroombee]

Have ~900ml cloudy solvent (olive-green tinted yellow). Been sitting at room temp (10-18°C) for over 28hrs now. Added an extra 3g of citric acid two hours ago so there is a little layer of it visible at the bottom of the bottle. Im a bit oncerned I added too much acid.

Does the 4mg/g and 20mg/g refer to g of Ethyl Acetate or g of cactus powder?

Are you sure the layer at the bottom is citric acid? It might be small xtals. Did you let the citric acid diffuse slowly or did you stir to dissolve?

The mg/gram refers to the amount of citric acid per ethyl acetate. Since you have about 800 grams of solvent, you only added an extra 3.75 mg/gram, so you should be fine. Solubility of citric acid in ethyl acetate is over 50 mg/gram.

Any recommendations of way forward - or should I just leave it alone and wait longer? thnx

If the solvent is still cloudy you can leave it alone, or you can aggressively stir and that should immediately cause xtals to precipitate from the solvent.

Loveall, one thing we might advise in the tek for first-timers is to aggressively stir after adding the citric acid to get quick xtals. These won't be the big, beautiful xtals that you're getting in your latest experiments, but I think adding citric followed by aggressive stirring is more reliable. At least that's what I've found in my successful runs. Slow diffusion to get big xtals is a more advanced process that can be attempted after one has had some successful aggressive-stirring runs. Thoughts?

 

[Loveall]

Have ~900ml cloudy solvent (olive-green tinted yellow). Been sitting at room temp (10-18°C) for over 28hrs now. Added an extra 3g of citric acid two hours ago so there is a little layer of it visible at the bottom of the bottle. Im a bit oncerned I added too much acid.

Does the 4mg/g and 20mg/g refer to g of Ethyl Acetate or g of cactus powder?

Are you sure the layer at the bottom is citric acid? It might be small xtals. Did you let the citric acid diffuse slowly or did you stir to dissolve?

The mg/gram refers to the amount of citric acid per ethyl acetate. Since you have about 800 grams of solvent, you only added an extra 3.75 mg/gram, so you should be fine. Solubility of citric acid in ethyl acetate is over 50 mg/gram.

Any recommendations of way forward - or should I just leave it alone and wait longer? thnx

If the solvent is still cloudy you can leave it alone, or you can aggressively stir and that should immediately cause xtals to precipitate from the solvent.

Loveall, one thing we might advise in the tek for first-timers is to aggressively stir after adding the citric acid to get quick xtals. These won't be the big, beautiful xtals that you're getting in your latest experiments, but I think adding citric followed by aggressive stirring is more reliable. At least that's what I've found in my successful runs. Slow diffusion to get big xtals is a more advanced process that can be attempted after one has had some successful aggressive-stirring runs. Thoughts?

Where the pulls done with freezing ethyl acetate? 1 minute each? Is the powder outer skin or whole plant?

If it is cloudy and not xtalizing, yes try shaking to make sure all the citric acid is dissolved and see if xtals form like shroombee suggests.

I think some plant matter is getting in the way of xtalization. Eventually it should xtalize, especially with more citric acid as it forces the issue. You can shake in 3g at a time, and if nothing xtalizes do that again. We've tested up to 20mg/g (which I needed with hole plant, no microwave, and room temp pulls), and as shroombee said we can go higher.

The xtals may look odd. They could be transparent stuff sticking to the wall, white blobs floating around, or long needles. However, when the cloudiness disappears, the precipitate is active mescaline citrate in our experience.

shroombee: You think shaking is more robust? I hadn't considered that. I think once we add the microwave and freezing paste/ethyl acetate the amount of unwanted plant matter will be so low that it won't be an issue anymore. I could be wrong and shaking may be better at the beginning.

 

[starway7]

those crystals look good!:thumb_up:

Ive alwayshad aproblem extracting near pure mescaline...that smelly ..[exylean]..coud be smelled a block away!

In the end i had to just take dryed ..peruvian cactus..in capsuls... and... wow..did it work well/...

At the time..I was in the south central or south east part of Arizona...Benson...

I remember starting to come up while i was in the public library ..i decided it was time to leave!

I then rode my bike after leaving the library.....an was I comming up fast!... i remember standing with my bike waiting to cross a busy street...

It seemed ..i could NEVER decide!....when to cross safely!.....my ..[Depth perception].. was distorted some by the peruvian torch!..


Finally i crossed the street safely... and rode my bike for three miles ..in the Arizona sun..till i turned off on a side road looking for a place to rest and be alone...


I breifly stopped peddling my bike under a tree for shade..


While standing there a gentle breeze blow through a near by tree..it sounded like thousands and thousands of voices ..all talking at the same time...!



Everything i looked at appeared alive! the rocks on the ground...plants...even the dryed out grass seemed alive!

It was so cool! I kept thinking about the thousands of deceiced native americans in spirit all around me..

I looked towards a nearby mountain range..where ..cochice made his last stand...against the american calvery!


Wanting to rest and be alone ... i rode into a cemetery and sat under a tree... taking a break still stoned...just reading the names on the grave markers...

After being there for a while..i car full of teens came into the cemetary ..i got a little parinoid and left rideing my bike 4 or 5 miles back to the RV park i stayed in..

So i rode my mountain bike 5 miles back the the RV park...
{knowing that I would not looked stoned!].. as long as i rode my bike and did not try walking all the way..

After getting back to my RV i remember putting on the most beautyfull .piano music.. ive ever heard

I was on the come down some but far from baseline...as i listened to the music i closed my eyes and experianced an emotional constant climax of pleasure..as I observed in closed visuals a constant ribbon of rainbow colors that merged with the piano music i was playing!

I remember even crying ..the emotion packed CEV rainbo ribbon in my mind.. . was endless! ..and so beautyfull..

It was like all the pain in my life was leaving in the form of tears ..from my eyes!

The colorfull closed eye visions [of an endless rainbow ribbon of emtional colors.. ] and piano music experiance ..it was so beautyfull..i cant compleatly explain it compleatly...

Any way thats howi came down fron the [peruvian torch powder]

Ive heard that the [pure mescaline crystal expeiance] is even more forgiving!

The last timei tryed an extraction of mescaline cacti was this method below..

It seemed like alot of work.. and it was har to get pure crystals ..and that ..[exyline].. smelled Bad!

 

[shroombee]

shroombee: You think shaking is more robust? I hadn't considered that. I think once we add the microwave and freezing paste/ethyl acetate the amount of unwanted plant matter will be so low that it won't be an issue anymore. I could be wrong and shaking may be better at the beginning.

I think shaking is more robust than 24 hour diffusion, regardless of the pulling process (pull time, temperature, microwave, etc). In my experience, aggressive stirring after bombing with citric acid forces xtals to form within minutes. In my case I use a magnetic stirrer. I imagine aggressive shaking in a sealed container also works to speed up the reaction.

I'd like to see people have a quick, successful first run, even if the xtals are not big or need to be rinsed off the glass, etc. Once the quick process works for them, then use the slow diffusion process to try for the xtal pr0n. :lol:

 

[Loveall]

shroombee: You think shaking is more robust? I hadn't considered that. I think once we add the microwave and freezing paste/ethyl acetate the amount of unwanted plant matter will be so low that it won't be an issue anymore. I could be wrong and shaking may be better at the beginning.

I think shaking is more robust than 24 hour diffusion, regardless of the pulling process (pull time, temperature, microwave, etc). In my experience, aggressive stirring after bombing with citric acid forces xtals to form within minutes. In my case I use a magnetic stirrer. I imagine aggressive shaking in a sealed container also works to speed up the reaction.

I'd like to see people have a quick, successful first run, even if the xtals are not big or need to be rinsed off the glass, etc. Once the quick process works for them, then use the slow diffusion process to try for the xtal pr0n. :lol:

Understood. I also have seen quick crystal formation after shaking and the solvent becoming clear pretty quickly. It is pretty cool.

merkin, let us know what happens to your clouds. I think we will get them to crash.

 

[merkin]

Thanks for the tips!

Are you sure the layer at the bottom is citric acid? It might be small xtals. Did you let the citric acid diffuse slowly or did you stir to dissolve?

1. Not sure of precipitate, I assumed citric acid due to the look (similar granular crystals) and the fact they were there since the acid was added.

2. Just dropped citric acid into liquid through a funnel and placed bottle on shelf without too much disturbance to crystalise.

See pic: after overnight left alone, cloudy section formed the lower half of the liquid in the bottle with the top part much clearer. There is some golden colored residue loose on the bottom, side view of same residue sticking to glass.

Where the pulls done with freezing ethyl acetate? 1 minute each? Is the powder outer skin or whole plant?

Yes, close to freezing (overnight in freezer) and about a minute. Powder was originally bought so I'm not sure of the composition.

If the solvent is still cloudy you can leave it alone, or you can aggressively stir and that should immediately cause xtals to precipitate from the solvent.

If it is cloudy and not xtalizing, yes try shaking to make sure all the citric acid is dissolved and see if xtals form like shroombee suggests.

OK, it looked liked first pic (bottom half volume is cloudier than top) - I was following the "leave undistrurbed" after adding acid. Now I have given it a vigorous shake-up, not for too long and left alone again. Hopefully some action later. I did not add more acid but will try that too after leaving it and not seeing anything. Is the crystalisation after shaking quite fast?


-- LATER --

After the photos and reading response, I added three batches of around 3-4g of citric acid (now up to around 15g into 900ml) with vigorous shaking in between. Not sure if all the acid dissolved during shaking or something else precipitated during the same. The liquid appears markedly clearer and there is a pile of crystalline/granular stuff on the bottom, but again, it looks to me like undissolved citric acid? Similar loose grains.

 

[Loveall]

merkin, it is looking good to me. Those sticky xtals in the 3rd picture look like the kind of product we can get. 15mg/g of citric will dissolve into ethyl acetate with enough shaking/time. The cloudiness disappearing is a sign that mescaline citrate is precipitating.

You can shake a few more times to make sure the citric acid dissolves if you are still seeing what look like granules. With time and shaking the liquid should become completely clear.

You may have whole plant, not sure. When I used whole plant I had to add 20mg/g (mentioned on the TEK's xtalization appendix). Extract from whole plant was more difficult to xtalize.

The extract looks a little greener that I would expect for cold extraction - Did you also use ice water so the paste would be cold when extracting?

After the solution is clear, you can proceed with catching the xtals and seeing if any are stuck to the walls (I think I see some, they can look very transparent). If you wash with a small amount of fresh ethyl acetate (jar walls and filter) most extract color should be removed. You can dissolve the product in hot water and let it evaporate slowly, you should get needles that way.

Would be very interesting if you report on the yield. If it is low you can try another pull on the spent paste.

I'm thinking we should add a microwave step before pulling. Also add a salt to the paste so it can be at freezing temps but not form ice and remain a paste for extraction. I'm getting a lot easier/cleaner xtalization with these updates (it's not really a lot more work). TEK can work without these changes, but with these updates it should be more robust in general.

 

[doubledog]

One idea is to dry the paste enough with CaCl2 so it can be ground in a blender to fine particles again. That should do it. Limonene was not good at pulling dry paste for me, but maybe ethyl acetate is different

Loveall, this would be interesting to find out.
Issues with limonene pulling dry basified cactus are not surprising, considering non polar (lipophilic) nature of limonene. It was discussed on the forum somewhere that even two-phase liquid-liquid extraction is tricky with limonene, as it is difficult to mix it with water properly.

On the other hand, ethyl acetate is a polar solvent, miscible with water to some degree. Its use in decaffeinization of coffee also suggest that it could penetrate dry plant matter (at least I assume that this process needs dry coffee beans, I really don't know)

Another useful information is that mescaline freebase can be extracted from dry cactus powder using ethanol. Maybe EA behaves more like ethanol, than like limonene.

 

[shroombee]

On the other hand, ethyl acetate is a polar solvent, miscible with water to some degree. Its use in decaffeinization of coffee also suggest that it could penetrate dry plant matter (at least I assume that this process needs dry coffee beans, I really don't know)

There are a few methods to decaffeinate coffee beans. They all use water or steam somewhere in the process. With direct ethyl acetate extraction, beans are first steamed and then soaked in the ethyl acetate to remove the caffeine.

How is decaffeinated coffee made? The chemistry of coffee decaffeination

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www.compoundchem.com

Another useful information is that mescaline freebase can be extracted from dry cactus powder using ethanol. Maybe EA behaves more like ethanol, than like limonene.

Does ethanol work on dry power because we're using 70% ethanol and thus there is quite a bit of water present?