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Ethyl acetate approach [CIELO] Options
 
Loveall
#1381 Posted : 3/21/2023 6:38:49 AM

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cyantific wrote:
With full spectrum tea, cacti species plays a big part of the experience… with CIELO would you be able to tell difference?


All lab tested CIELO TEK results have given mescaline citrate only (I'm aware of 4 results, two published on the nexus while the other two have remained anonymous).

I don't think we can claim with certainty that the cactus species necessarily changes the experience: published plant lab analysis results only show traces of other alkaloids, while the mescaline dose is variable. Therefore, different mescaline levels + set/setting alone may explain the different plant experiences without having to invoke other alkaloids. Just pointing out a possibility here, I don't think we can claim this for sure either.

Maybe plant chemistry other than mescaline does matter, but there is no hard analytical data to support that at the moment (that I'm aware of).
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endlessness
#1382 Posted : 3/21/2023 11:05:46 AM

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Recommendation that could potentially be added to the wiki: After washing with EA with sodium carbonate solution, wash it again with just water, otherwise you are possibly going to get sodium citrate contamination in your mescaline . This is what I got with my last extraction, I just confirmed it with NMR. Mind you, I did not freeze the Ethyl Acetate to remove water after washing, so you might reduce the sodium carb contam that way too but it is very easy to simply wash it again with just water after washing with sodium carb solution.
 
Loveall
#1383 Posted : 3/21/2023 11:12:34 AM

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endlessness wrote:
Recommendation that could potentially be added to the wiki: After washing with EA with sodium carbonate solution, wash it again with just water, otherwise you are possibly going to get sodium citrate contamination in your mescaline . This is what I got with my last extraction, I just confirmed it with NMR. Mind you, I did not freeze the Ethyl Acetate to remove water after washing, so you might reduce the sodium carb contam that way too but it is very easy to simply wash it again with just water after washing with sodium carb solution.


Interesting, was the EA with sodium carbonate cloudy during the extraction/before salting?
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endlessness
#1384 Posted : 3/21/2023 11:36:15 AM

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Hmm honestly I didn´t pay attention, I was trying to do a really quick extraction so I took some shortcuts, I didnt measure the amount of sodium carb so it was prob really concentrated solution, and after wash I decanted and just used it to extract straight away. If you use only a dilute solution and you freeze to remove excess water after, you´re prob not gonna have this issue in a significant way, but I think its important to keep in mind, a second water-only wash is a very simple addition to the work flow and would def prevent this issue.

if this does happen to anybody, sodium citrate is practically insoluble in alcohols including methanol, Im not sure mesc citrate solubility in ethanol or IPA, but its def soluble in methanol, so I separated it this way, soaking in methanol to dissolve mesc citrate and leave sodium citrate behind, but I have a rotovap to make sure no methanol is left when I evap it, I would avoid using it otherwise... But if mesc citrate is at soluble in IPA or ethanol one could use that instead.. Or just re-a/b and issue is solved. But better avoid it in the first place
 
Twilight Person
#1385 Posted : 3/21/2023 6:09:54 PM

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So later I want to try cacti powder + CaCO3 and see if it also forms a nice paste (and try finding out if that gives a more-full-spectrum-extract or not)

So from what you say Ca(OH)2 works good, while Na2CO3 gives a bad consistency, unable to make the TEK easy.

Then what is this more of the origin: probably more the effect of the Ca(OH)2 which has the positive effect? Or the Na2CO3 which has the negative?

In case that it is only Na2CO3 which is bad (and not *only Ca(OH)2 which is good), did you also check if you can do:

cacti powder + NH3(aq)?

I think NH3 is terrible to work with, but just on a theoretical level it would also just freebase the alkaloids, but not phenolic OH- groups. So whatever would remain should still be a 'full spectrum' in the ethyl acetate.

I think these primary amines have the least basicity compared to secondary / tertiary, so NH3 would work still pretty good and not interfere with any R-OH.




And question #2:

If I want to try the benzoic acid / toluene way, would I just substitute the same moles? I guess as you try to precipitate mono-mescaline citrate it should be just the equimolar amount with benzoic acid?
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starbob
#1386 Posted : 3/21/2023 8:36:47 PM

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Regarding washing and possible sodium citrate contamination; I had multiple cases where a small opaque third middle layer formed which i threw away with the bottom water layer. Only one case was this layer significant enough ~200mL that I saved it to try to recover. And it took a very long time (days) for the cloudiness to settle before i decanted again and froze and strained it but i never added it to my washed & dried EA for fear of unknowns.

Edit: woops Shocked i didn't realize there was a bunch of comments here previously on cloudy washed EA, I'll have to go take a closer read
 
Loveall
#1387 Posted : 3/22/2023 8:08:13 AM

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Twilight Person wrote:
So later I want to try cacti powder + CaCO3 and see if it also forms a nice paste (and try finding out if that gives a more-full-spectrum-extract or not)

So from what you say Ca(OH)2 works good, while Na2CO3 gives a bad consistency, unable to make the TEK easy.

Then what is this more of the origin: probably more the effect of the Ca(OH)2 which has the positive effect? Or the Na2CO3 which has the negative?

In case that it is only Na2CO3 which is bad (and not *only Ca(OH)2 which is good), did you also check if you can do:

cacti powder + NH3(aq)?

I think NH3 is terrible to work with, but just on a theoretical level it would also just freebase the alkaloids, but not phenolic OH- groups. So whatever would remain should still be a 'full spectrum' in the ethyl acetate.

I think these primary amines have the least basicity compared to secondary / tertiary, so NH3 would work still pretty good and not interfere with any R-OH.




And question #2:

If I want to try the benzoic acid / toluene way, would I just substitute the same moles? I guess as you try to precipitate mono-mescaline citrate it should be just the equimolar amount with benzoic acid?


Aomnia can react with ethyl acetate, I wouldn't use it.

Excess benzoic acid is fine, don't worry about moles. This is a lazy approach, just drop in about a teaspoon.
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Orion
#1388 Posted : 3/24/2023 8:18:29 PM

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Hmmm so far not so good. Settled out the water and poured the solvent into a second vessel, added excess citric acid monohydrate and it clouded up. Goo was produced around the grains of citric acid at the bottom and agitation made no difference. I checked the PH and it was still alkaline so I assumed it was the trimescaline form. Adding extra citric acid didn't change anything. An addition of anhydrous citric acid just sat in a clump at the bottom and wouldn't dissolve.

I Rebased the precipitate again with lime after dissolving it in minimal water, pulled and settled for 24h in the fridge and used a pipette to draw off the solvent without any droplets. Added very finely ground citric acid monohydrate and made sure the PH was acidic. Now I have a cloudy solution with lots of goo droplets, no crystals so far.
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endlessness
#1389 Posted : 3/24/2023 8:35:45 PM

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So did you do the fridge step to precipitate water or just at room temperature?
 
Orion
#1390 Posted : 3/24/2023 8:45:42 PM

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endlessness, freezer then fridge like you did the first time. Second time was 24h in the fridge.
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endlessness
#1391 Posted : 3/24/2023 9:05:48 PM

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I never had the issue of the goo, there is some recommendations on the tek in that case.

How long has it been since you added the citric acid? Wait at least a day .
 
Orion
#1392 Posted : 3/25/2023 1:24:33 AM

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It's been a good 5 hours, I'll wait and see for now.

A couple of ideas about this tek in general:

1: I personally would only use dried outer green flesh. There are a lot of impurities in the core and very little mesc.

2: Less material requires less solvent and you could save a lot this way.

3a: With a much smaller amount of material you could make a fully dried paste a couple of hours by fanning the cactus lime paste. This would save 24 hours in the fridge.

3b: This also eliminates the water variable from the base paste, as there isn't any added to begin with. Only bottled ethyl acetate is being used which usually has the right hydration level to begin with.
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_Trip_
#1393 Posted : 3/25/2023 2:38:11 AM

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Orion wrote:
It's been a good 5 hours, I'll wait and see for now.

A couple of ideas about this tek in general:

1: I personally would only use dried outer green flesh. There are a lot of impurities in the core and very little mesc.




I agree with many of your statements Orion. However what makes you say the core has impurities?

Using the core only yields the cleanest crystals (even without a wash) when using the Cielo tek. But your right it has very little mescaline. I found only 13% of what was in the green layer was found in the core. That new study posted recently seems to indicate there may be slightly more.
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Toshido
#1394 Posted : 3/25/2023 4:11:07 AM

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Orion wrote:

1: I personally would only use dried outer green flesh. There are a lot of impurities in the core and very little mesc.


This research seems to show that although there is less mescaline, there is still mescaline to be had.

SOURCE: https://anoniem.org/?htt...9/fpls.2023.1066595/full

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Loveall
#1395 Posted : 3/25/2023 3:37:34 PM

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Orion wrote:
Hmmm so far not so good. Settled out the water and poured the solvent into a second vessel, added excess citric acid monohydrate and it clouded up. Goo was produced around the grains of citric acid at the bottom and agitation made no difference. I checked the PH and it was still alkaline so I assumed it was the trimescaline form. Adding extra citric acid didn't change anything. An addition of anhydrous citric acid just sat in a clump at the bottom and wouldn't dissolve.

I Rebased the precipitate again with lime after dissolving it in minimal water, pulled and settled for 24h in the fridge and used a pipette to draw off the solvent without any droplets. Added very finely ground citric acid monohydrate and made sure the PH was acidic. Now I have a cloudy solution with lots of goo droplets, no crystals so far.


Orion, sorry you are having this issue. I'm pretty sure we can figure this out, as many people are getting xtals reliably.

Side note: I'm a fan of your previous work on the nexus, thank you for that.

A few questions:

- Are you using the TEK ratios? If not what ratios did you use? I'm surprised your first salting was alkaline if you used the TEK ratios (they are designed to oversalt even the most powerful of cacti we have seen at 8%). You are correct that an alkaline extract will create goo instead of xtals.
- How long did you wait for the goo to change after adding more citric acid? It can take a while (days)
- I'm not very familiar with the mini A/B goo recovery, but it should have worked to first order. It is, however a different situation than when using the TEK, so I would not worry too much about it not working.
- Do you still have more cactus powder to try again depending on the answers above? It could simply be that you needed more citric acid added at the original salting step
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Loveall
#1396 Posted : 3/25/2023 3:43:23 PM

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Orion wrote:
It's been a good 5 hours, I'll wait and see for now.

A couple of ideas about this tek in general:

1: I personally would only use dried outer green flesh. There are a lot of impurities in the core and very little mesc.

2: Less material requires less solvent and you could save a lot this way.

3a: With a much smaller amount of material you could make a fully dried paste a couple of hours by fanning the cactus lime paste. This would save 24 hours in the fridge.

3b: This also eliminates the water variable from the base paste, as there isn't any added to begin with. Only bottled ethyl acetate is being used which usually has the right hydration level to begin with.


1) In practice we have seen that spines/wax/core do not cause any issues in product purity or the process itself.
2) True, but the EA can be reused, so it is almost "free". There are some losses from solvent absorption, but the economics justify the extra mescaline in my opinion. I could be wrong though.
3) This is very tricky. Without water, lime particles diffuse into the EA wich are a pain do deal with. Even worse, the mescaline does not move well from a dried paste into the EA. I don't understand why, but experimentally I get little to no yield from a dry paste. Interestinly, if I re-wet the paste and pull again, I get normal yields. Some people say that dry mescaline freebase can salt itself in air with CO2 (?). I don't know, but I can say a fully dry paste does not yield well.
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Loveall
#1397 Posted : 3/25/2023 3:58:46 PM

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_Trip_ wrote:
Using the core only yields the cleanest crystals (even without a wash) when using the Cielo tek. But your right it has very little mescaline. I found only 13% of what was in the green layer was found in the core. That new study posted recently seems to indicate there may be slightly more


I think your results is consistent with the paper. It can change from plant to plant and diameter of cut.

In my opinion it is reasonable to say that core gives a 10-20% boost to yields and worth using on the TEK when reusing solvent.

On the other hand, if I were drinking a bitter tea I would not add the core.
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Orion
#1398 Posted : 3/25/2023 10:46:39 PM

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_Trip_ wrote:
I agree with many of your statements Orion. However what makes you say the core has impurities?


I just mean anything that isn't mescaline but will go into your solvent. May not be too much of an issue with this tek though.

widderic, there definitely is some in there. I suppose it's personal preference. The paper mentions williamsii and pachanoi but I don't think I've seen much of an increase with the bridgesii I use. Personal preference I guess.

Speaking of volumes, I wonder if the concentration is the reason I've got goo instead of crystals ? I have used 400mg of mesc HCl and added water then lime to make a paste and pulled with about 100ml of Ethyhl Acetate. Perhaps this has behaved like spice when the naphtha is too concentrated, precipitating too quickly as a goo ? In the tek the solvent seems to be considerably less saturated before crystalizing. Perhaps that is the reason ? Just a guess.

I will try redissolving the goo in distilled water and evaporating to see if it crystalizes.
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shroombee
#1399 Posted : 3/26/2023 3:02:47 AM

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Orion wrote:
I will try redissolving the goo in distilled water and evaporating to see if it crystalizes.

The TEK lists four options for dealing with goo:

(1) Do an A/B extraction on the goo,
(2) If a TEK execution is suspect, add the goo to cactus paste and do the TEK propely, increasing citric acid by the amount of expected mescaline present in the goo,
(3) decant off the solvent and cover the goo in fresh EA, it has been observed that crystals can grow out of the goo after a few days sitting in fresh solvent and stirring can help the process move along if crystal formation stops and there is still goo left, discard the solvent and add more
(4) if goo forms repeatedly, retry the TEK using fumaric acid instead of citric acid (fumaric may be more robust at forming xtals)


If you repeatedly get goo, try adding dry ethyl acetate to the extract before salting with citric acid. The theory being the additional EA will offset excess water in the extract.
 
Nemooo
#1400 Posted : 3/26/2023 9:05:06 AM
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Some hopefully useful info:
- Drying with K2CO3 is simple, effective and takes 10-20mins. So quicker than chilling and no extra work really than just decanting a second time.

- Conc. sulphuric acid can be used as well. Just add some drops of the acid to some ethyl acetate then add that to the dry ethyl acetate extract (dried with K2CO3). Pulls more colour with it though.

- Fumaric and tartaric acid both quickly form highly crystalline solids from dried ethyl acetate (dry with K2CO3). The fumarate and tartrate salts can be easily recrystallised from 95% ethanol. In both cases after recrystallisation there is a small amount of insoluble crystalline acid material (not the parent acid) and a small amount of brown impurity.

I’d love to take a look at a copy of the NMR files if someone can share them with me? I have topspin.
 
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