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TEK Ethyl acetate approach [CIELO]

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Let me know if that filters absolutely crystal clear.

As a lifelong laziness expert, I must say that shaking and de-hissifying a jar for some amount of time, then settling, filtering, and continuing to look at cloudy solvent; is nowhere as lazy as stirring once, letting sit with a loose cap for an hour, then putting in a freezer until the debris plug and water freeze at the bottom, and then decanting absolutely crystal clear solvent.

Sounds like a pre-experiment may be coming.
 
Loveall said:
There may be a nice lazy way to reuse EA after all 🤞

Motivated by lazyness, I added washing soda powder straight to some used EA (no water). Nothing seemed to happen, but them I started seeing tiny bubbles. I shook and relieving pressure resulted in a hiss.

The neutralization is a lot slower than with a water layer, but it is happening. Eventually after a bunch of waiting and shaking the pH paper came out neutral and the hissing stopped. Shaking makes things go by faster.

The neutralized EA is a bit cloudy but not too bad. Gonna let it settle and see how it looks tomorrow.

If this works, we can skip the water separation. Simply decant off/filter the neutralized EA from the washing soda/sodium citrate solids.

I'll be testing this further and report back. Note that this process would also dry the EA, but I don't think that matters since the paste has a lot more water (overwhelming any potential effects from the EA carrying a bit of water I believe).
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Nope, doesn't really work. Cloudiness in the solvent for reuse doesn't go away nicely as with a water layer. Standard TEK prevails this time.
 
Cheelin said:
Std Tek Wins Another Round?

How’s it feel to be right the first time, again & again?
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Well, it took a while to get where we are today, which builds on other people's work. Lots of early tests didn't work out too; For exple at the very beginning salting was done with 10% sulfuric acid which sort of worked but not really 😅.
 
Yes, science is built on the shoulders of predecessors.

But, the initial concept - so far as from when it was finalized here, circa early-mid 2021, has basically remained constant. Relative to other diy M extractions. the standard processes are what scientists call “robustly elegant”!
 
Loveall, I have too much on my plate to work on this idea, atm, but it is likely to be a relatively lazy and effective approach to minimizing the darkness of, and chlorophyll components in, used solvent. Biologists and others are well aware that light degrades chlorophyll. If the extracted chlorophyll in used solvent is determined to be problematic, perhaps by exposing jars of used solvent to intense light, or extended periods of household lighting, the chlorophyll will degrade to filterable sediment.




Results for reprocessing crappy product can be found in post 702.
 
Update on the solvent washing experiment: i have washed, frozen, and decanted standard process used solvent jars of both 5g citrate/100g material and 15g citrate/100g material. Both jars had carbonate-ice pucks in the bottom, but there were also floating ice crystals in the still cloudy solvent layer. So, not as quick as “freeze and decant” to get crystal clear washed solvent. The good news is that the pH is similar to that of fresh solvent, and after filtering off the ice crystals and letting the decanted solvent warm to room temp, the solvent is clearing slowly but nicely.

The washing method is not a slamdunk (but still well within the laziness zone). My detailed method for doing this is in post 716 (not yet complete).
 
It’s becoming clear (lol) that this sodium carbonate used solvent wash is something that takes time to complete. It certainly rehabs solvent to a level that yields equivalent quality and quantity of product as fresh solvent, at least as so far indicated in my 5g runs, and will be tested extensively in larger future runs.

But, short of centrifuging or microfiltering it, it takes its sweet time clearing. So, build some time into your washing plan.


I have a few tests running to try to reduce clouding and/or increase clearing time. I’ll update if any improve the turnaround time.


Chemists, in beer/winemaking a process called fining is used to clarify the product (e.g. Fining @ Improved Winemaking ). Can you think of any fining materials that would work in this instance and be easily removed from the solvent?
 
Sodium carb clears up for me overnight. Haven't had many issues. My water is saturated with sodium carb with some undissolved, not sure if that matters. If cloudy after neutralizing and separating the water, adding solid carbonate alone (no water) and shaking /settling may help.

I like the sunshine idea.

Thee was a report that dilute sulfuric + phosphoric broke down chlorophyll in oil, so I'm trying that I'm EA. I used pH down from the pet store (9.6% sulfuric) and 10% phosphoric from the home brew shop (drink additive). It changed the color from green to yellow, bit still pretty dark. Gonna do water pulls, see if the broken down chlorophyll can be removed this way.

I don't know about clarifying agents for EA from the wine industry.

We've been told that activated charcoal filtered with DE should work, so there's that.

I've reused the same EA up to two times (3 total). It becomes dark and it's difficult to see what is going on. However, it still works and yields are fine. Still, would be nice to clarify because each time it gets darker and more difficult to see what is happening.
 
Well my jars aren’t, this time, molasses-slow clearing going on. I did 2 jars about 3 weeks ago (sodium carb-water + freezing), but just set them aside without paying attention to them, moderately dark hue, but crystal clear. I’ll keep searching for a reliably repeatable method, including trying your suggestion.

Bright sun or equivalent ppfd lights (which I have). I’ll play with this later, if necessary.

EA is a fermentation product, so potentially workable. But, one of the primary fining mechanisms relies on charged particles, and sodium carbonate (edit) is neutral. Also, most of these agents require several days to weeks to settle, so likely no gain for the pain. Brainstorming.

I already tried powdered AC to decolor, pitfa! Just got some granulated, so i’ll test that at some point.

Unless there is a buildup of molecules that interfere with yield or quality, I see no reason why dark hued, but clear solvent is an issue worth spending effort or elapsed time trying to resolve. So, I’ll be initially focused on trying to get a repeatable washing process (so I don’t waste my limited amounts of various yellow used solvent), then move on to testing fresh, green, and yellow solvents against each other, over multiple runs, to see what gives.
 
Loveall said:
Sodium carb clears up for me overnight. Haven't had many issues. My water is saturated with sodium carb with some undissolved, not sure if that matters. If cloudy after neutralizing and separating the water, adding solid carbonate alone (no water) and shaking /settling may help.

I like the sunshine idea.

Thee was a report that dilute sulfuric + phosphoric broke down chlorophyll in oil, so I'm trying that I'm EA. I used pH down from the pet store (9.6% sulfuric) and 10% phosphoric from the home brew shop (drink additive). It changed the color from green to yellow, bit still pretty dark. Gonna do water pulls, see if the broken down chlorophyll can be removed this way.

I don't know about clarifying agents for EA from the wine industry.

We've been told that activated charcoal filtered with DE should work, so there's that.

I've reused the same EA up to two times (3 total). It becomes dark and it's difficult to see what is going on. However, it still works and yields are fine. Still, would be nice to clarify because each time it gets darker and more difficult to see what is happening.
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Update: The sulfuric + phosphoric is removing the color too slowly.

Next I'm going 6o try these aquarium activated carbon baggies. See if they clarify EA without releasing any carbon dust into the solvent 🤞
 
Good stuff. We’ll eventually nail this, in a way that kitchem chemists can handle.

Probably gravity + time will be the lazy solution for clarifying the neutralized solvent.

I’m so tempted to just distill it, but that is a risky proposition for the kitchen, and not really in the lazy zone.
 
Loveall said:
Conclusion is very is simple: Multiple data are consistent with the monomescaline citrate forming in the CIELO Tek because of excess citric acid.
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Backtracking a bit here but my view on this is that as soon as the molecules of citric acid have ionised and protonated the nearest available mescaline molecule, the electrostatic forces are sufficient that the two ions precipitate from the EA as they have become too polar to remain in solution. The lattice energy of crystallisation exceeds the solvation energy of the EA for the respective ions. The upshot is that there simply isn't time (or energy) for the dibasic or tribasic salts to form. It may be possible to form these higher salts by using mesc freebase dissolved in water.

I find it elegant how a trace of water aids this proton transfer that leads to crystallisation, but too much will spoil the formation of crystals.
 
Very nice!

Your comment, Loveall’s orange goo, and my early crappy product are rattling around my skull.

I’m convincing myself that inadequate washing with fresh EA, followed by inadequate drying then water recrystallization, leads to goo/brown sticky crap. Seems water and EA are delicately balanced in this tek, with pH playing some influencing role.
 
I think that as long as the extract is rested long enough for water drops to settle (if any), and decanting those, the process works with excess citric. I've encountered this situation when aggressively pulling and not resting the paste long enough before puring off the EA, and decanting the water worked.

So I think the process window is large enough to not run into issues.
 
Cheelin, I have used gelatin as a clarifier for homebrew. It also works based on charged particles. It removes any hazyness/cloudiness from yeast, hops, or malt, and leaves a beer that is crystal clear to see through. You just toss it in and decant a few days later.
 
Loveall, if your comment was in response to mine, i was referring to issues related to the last step of the process, when not done with same purposefulness of good pastemaking and pulling steps.

Specifically, I think part/all of my crappy product resulted that way due to incorrect and incomplete fresh EA washing of the collected crystals and jar, incomplete drying of the EA in the filter and jar, followed by warm water washing for recrystallization. Basically, “dirty” EA mixing with water and product, entrapping/binding crap in the product. Reminds me of what happens in the hours long boildowns to resin.
 
Thanks HLP. I’m thinking that, since sodium carbonate is uncharged, positively charged gelatin won’t work in this case like it does in beer/winemaking. If you try it and find that it does quickly clarify cloudy EA, let me know and I will order some and test it, too.
 
Cheelin said:
Loveall, if your comment was in response to mine, i was referring to issues related to the last step of the process, when not done with same purposefulness of good pastemaking and pulling steps.

Specifically, I think part/all of my crappy product resulted that way due to incorrect and incomplete fresh EA washing of the collected crystals and jar, incomplete drying of the EA in the filter and jar, followed by warm water washing for recrystallization. Basically, “dirty” EA mixing with water and product, entrapping/binding crap in the product. Reminds me of what happens in the hours long boildowns to resin.
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Ah, gotcha. Yes, definetly want the EA rinses and EA drying before picking product with water, otherwise it will be a mess. I'll add that to the wiki.
 
Might help someone else. The only part of the tek that I can think of that I originally screwed up. Totally on me, and right at the end of the process!
 
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