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TEK Ethyl acetate approach [CIELO]

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starbob said:
I thought it might be interesting to try CIELO with ascorbic acid, so I tried a rough solubility test with EtAc and the result was much worse than citric acid. I used L-ascorbic acid 100% food grade, roughly 10mL dry pure EtAc, and ~55mg ascorbic acid, but it would not dissolve. I was shooting for the CIELO equivalent 5g/L proportion like the tek roughly is currently. Perhaps some dissolved but a lot did not. I tried heat for awhile >55C but didn't help. Added 0.1mL distilled water at a time, shaking, returning to heat awhile, shaking and checking, and ultimately ended at 0.4mL (4% of EtAc volume) before it fully dissolved. It didn't precipitate any out after chilling a bit and left at room temp, so maybe I could have done 0.05mL water increments and ended at 0.35mL with some precipitating out after cooling.🤷‍♂️

I think I'll try a 2.5g/L proportion with ascorbic acid in a CIELO tiny batch. I assume that will be OK with the typical water content in the CIELO extract and given however much ascorbic acid will be consumed by the mescaline ascorbate crashing.
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Great to hear of experimental results, even failures and difficulties. The poor solubility of ascorbic acid in EA is rather predictable given its high proportion of polar oxygen atoms. This may help with crystallisation since it makes it likely that the M ascorbate will be a hydrate, so moist EA may be advantageous in this situation (fingers crossed on that!)

Looking forward to hearing how it goes since this is something I specifically didn't bother with on account of that poor solubility.
 
Monohydrate I think. I’ve been pushing the batch size up bit by bit. I can get consistent results now with 600g of powder in three litres of EA. Freebase in 200g batches in a food mixer till soufflé like then do three solvent pulls in one batch using a paint mixer and a tall HDPE jug. Really whipping the crap out of it! Three pulls this way seems to get everything. I use a fine cheese cloth to strain and squeeze out the paste and solvent recovery is good doing it this way. No fridge rest since the updated hydration recommendations and Fluffy crystals every time
 

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antichode said:
Monohydrate I think. I’ve been pushing the batch size up bit by bit. I can get consistent results now with 600g of powder in three litres of EA. Freebase in 200g batches in a food mixer till soufflé like then do three solvent pulls in one batch using a paint mixer and a tall HDPE jug. Really whipping the crap out of it! Three pulls this way seems to get everything. I use a fine cheese cloth to strain and squeeze out the paste and solvent recovery is good doing it this way. No fridge rest since the updated hydration recommendations and Fluffy crystals every time
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Wow you nailed the TEK 👏

Lol at the spoonfulls of very pure mescaline citrate 👌
 
Orion said:
Last time I used this method to convert mescaline HCL at a fairly high concentration in solution and got goo. This time I used the cactus it was created from as per the usual tek. I it also created goo. When I checked the PH after adding the recommended amount of citric I noticed it was actually close to neutral. This is an important factor. I have added enough citric acid to get the PH up (confirmed with a PH paper) to see if it can crystalize the goo over time.

The cactus is a Bridgesii, some think it may be a lumberjack and it has always had quite high yields.

I think what might be happening for some people with high yielding cactus is that there is so much mescaline and the solution actually more alkaline than you think. Then when you add the citric acid you are crystalizing at too high of a PH and creating trimescalne citrate instead of monomescaline citrate. This is why PH testing is important.

I wonder if both trimescaline citrate and monomescaline citrate can be crystalized by an IPA re-x as some people have recently shown ? I feel like it's quite important to know as it affects dosages.
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Twilight Person said:
Good news! If you remember I tried some CIELO and miserably failed as i constantly posted pictures from goo. Then i tried this etoh rex method (or ipa as it now seems better??) and at least got some solid stuff to work with... But still not pretty happy as the marvelous CIELO crystals make up 50% of the reward and that white chunks are just not as nice.

So while my cacti are now sleeping i took that one who was still awake (the white thing, remember?) and slashed him to powder...

Just tried a different way of water removal which was FREEZER. I know the tek says freezer removes too much water, but well i had nothing to loose and after filtering off the diffuse ice that is formed and threw the citric inside, voila = the true CIELO crystals formed.

I have no clue what is the reason, maybe something wrong with fridge or whatever, but probably from now will always go with 'freezer decant' as anything else gave goo. Just in case somebody else has same problem, maybe just try that 1x.

Cheers :Aşk: :Aşk: :Aşk:
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Brennendes Wasser said:
Apparently there is quite a little water in the crystals, as Endlessness found like 7 % water via NMR. Also the crystallization does not work if 0 % water is present - well the same amount of precipitate was at least formed in a test I did, but it was just a white coating across the glass. In any way the crystals also contain some water, so I wanted to make a small experiment.

Is that water strongly bound and part of the crystal structure or just like an artefact from crystal formation, that can be removed with force?

85,50 mg Mescaline Citrate in Oven @ 50 °C / 0,04 bar for 24 h

weight afterwards ...

84,57 mg Mescaline Citrate

so even hardcore physico-chemical water removal did not do anything, must be totally locked within the crystal grid.

Could also just verify a little more quantitative by NMR, but I already have no access to any analysis method anymore and the one at my Friend's place is still broken :roll: .
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modern said:
So the still wet crystals ended up forming a goo again. I added isopropanal again and will try to decant once more. Same as last time the crystals precipitate in ambient temperature. This time when decanting I'll keep the crystals in this small beaker if it goes to goo again I'll preform a nano extraction again basing pulling again.

EDIT: There are two different crystals types. One that is soluble in cold iso and one that precipitates in cold iso. I think the precipitate that crashed in ambient temps is some sort of sodium sulfate contamination? The bottom photo is from ambient temps in the iso.
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Hello Friends, Which one do you use? Citric acid monohydrate? citric acid anhydrate?
 
PanSeq said:
What paste ratio are you working with now with the changes?
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170g of water to 100g cactus is working well for me but I imagine every plant and batch is a bit different.

(Ive already dm’d you this but I’ll copy and paste so others can see…)

I initially got goo but changed my approach a little since then and had success. The main difference for me was using a food mixer to freebase the paste. I was not mixing it enough when I got goo. The food mixer really helps. Use a silicone paddle attachment if you can get one. At first I run it on low to mix everything then gradually increase the speed until it’s going full noise and really whipping it around. The paste goes from clumpy to sticky balls then to a soufflé or mousse like consistency. The sound changes and it starts to look like it’s becoming wet again. That’s when it’s ready for the next step.

Then I use a paint mixer to mix the solvent although this is not necessary it’s just that the volumes I’ve been using necessitate a little mechanical help.

If you follow the hydration recommendations the fridge rest is indeed not needed. It’s such an elegant tek!
 
One thing I would like to try is distilling some of the solvent off once it has the goods. Just from a place of curiosity. I’d like to see what the crystallisation is like when the saturation of mescaline is quite high
 
antichode said:
One thing I would like to try is distilling some of the solvent off once it has the goods. Just from a place of curiosity. I’d like to see what the crystallisation is like when the saturation of mescaline is quite high
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With super high saturation, crystalization is quick and beautiful. I have found it to fall out of solution almost instantly with my 7.5% NOID bridgessi, be a consistent brilliant white, with the most beautiful, fluffy crystals I have been able to attain. The higher the concentration the higher the apparent purity and ease of crystalization.
 
antichode said:
One thing I would like to try is distilling some of the solvent off once it has the goods. Just from a place of curiosity. I’d like to see what the crystallisation is like when the saturation of mescaline is quite high
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So, I do t recommend doing this. I had 4L of EA that I distilled down to 1L in a copper pot still. There should be about 15g of alkaloids in there so it’s saturated! But adding citric acid didn’t do anything. The acid just sank to the bottom and didn’t dissolve very well, that was it. I guess I either distilled off too much water or left the water behind? Either way I messed with the balance of it all 😂

I’ve added the distillate back to the mix and it’s now sitting and I’ll check it in the morning.
 
So I have an interesting question for this tek. I've been experimenting with more effective MDMA purification techniques, and discovered a miscibility chart for various solvents. I found out naptha can be used to increase the precipitation of MDMA from isopropyl because they're miscible and a nonpolar significantly reduced the solubility of the hcl salt. I also found ethyl acetate is soluble with virtually every nonpolar. Do you think adding hexane would increase the crash-out of the citrate salt? I do see the problem with retrieving solvents post retrieval, but I'm pretty sure hexane and ethyl acetate have pretty different boiling points so fractional distillation would work well.solvent-miscibility-table (1).png
 
I don't see the point in adding hexane to they ethyl acetate since the mescaline citrate precipitates well if done correctly... BUT I also like to experiment so assuming you have glass distillation apparatus I would substitute the hexane for heptane. The boiling point is near 98-99C so much easier to separate and recover post extraction. You would still need to have the appropriate water content I'd assume?

If you are willing to experiment try with heptane instead. Also most go for this technique due to being 'safest' not everyone likes heptane nor hexane despite being fairly safe unless you breath in a large amount from my understanding.
 
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