TEK Ethyl acetate approach [CIELO]

[Loveall]

Freezing removes a lot of water, can be up to 2.5%. Also, some of that ice can have some EA too. You many need to add a little water back to dissolve the EA.

The cacti you have look solid. You should be getting xtals.

Sorry if this has been asked before, but what EA are you using? Do you have a picture of it or namebrand? Same for the citric acid. If your technique and cactus is good, I wonder if your TEK materiala are the issue...

 

[downwardsfromzero]

I hope the EA isn't maybe contaminated with ethanol or something?

Also there was that problem with the expired lime - but you got new lime so it hopefully is nothing to do with that :?

 

[Loveall]

I tried an alternative partial drying method to the fridge rest.

Since the fridge rest removes ~ 0.5% of the water, I added 0.3% of Sodium Carbonate drying agent by weight. Idea was to create a solid filterable hydrated mass that would be easier to separate than fridge decanting.

Unfortunately a water layer still formed with partial chemical drying (see image). Decanting was still needed. TEK worked as usual with this decanting substituting the fridge rest.

So no clear benefit, but an option. I guess if one doesn’t have a working fridge (doubledog?) this could be an alternative. Could enable a jungle TEK along with sun drying and mortar/pestle grinding.

 

[doubledog]

For jungle TEK, probably some potash would be better than calcium carbonate, at least water solubility (drying strenght) would be higher. Of course, solubility in EA should be checked to avoid contamination.

I guess if one doesn’t have a working fridge (doubledog?) this could be an alternative.

What keeps me not trying this tek is mainly extreme strong smell of EA. Still main discovery (imo) of CIELO is how to prepare Lime paste - this is the most important part. Lime paste could be then extracted with various solvents.

 

[Loveall]

For jungle TEK, probably some potash would be better than calcium carbonate, at least water solubility (drying strenght) would be higher. Of course, solubility in EA should be checked to avoid contamination.

I guess if one doesn’t have a working fridge (doubledog?) this could be an alternative.

What keeps me not trying this tek is mainly extreme strong smell of EA. Still main discovery (imo) of CIELO is how to prepare Lime paste - this is the most important part. Lime paste could be then extracted with various solvents.

The lime paste was used before for limonene extractions. I think main discoveries of CIELO were (1) room temp EA is very effective at pulling mescaline from lime cactus paste (no emulsions, great penetration with partial water mixing), and (2) after reducing EA water content by ~ 0.5% (e.g. with cold rest), simply adding excess solid citric acid selectively and cleanly precipitates monomescaline citrate.

 

[Twilight Person]

All of the plants are good performers, over the years Ive weeded out anything not worthy. The last time I extracted them I got a good yield, just shy of 6g from 10kg fresh see here Dazzling Crystals - Preparation - Welcome to the DMT-Nexus

I used to run successful extractions with lime and limonene back in the day so Im somewhat familiar with how the paste should feel etc. Why no alkaloids now is leaving me a bit perplexed. Perhaps the EA has a lot of water in it.

Hello sir!

I tried the limonene route too but i got 0 separation of limonene/paste. Obviously i added more Limo but it just absorbed more and more and so i switched to EA to not waste the whole batch. How much limonene did you use per pull on how mich paste? And then how many pulls?

Cheers

 

[antichode]

Hi Twilight

I have not performed 69 Rons limonene tek in over a decade, that's what I meant by 'back in the day'. However when I did I got reasonable and consistent yield from it and never had a problem extraction the limonene. From memory it was about 300ml per pull or something along those lines, total of 1L limonene.

I stopped using that Tek because I could not scale it up easily, the mixing and separating became difficult with large amounts of cactus and the preparation was time consuming, slicing and drying etc. I ended up moving on to the old classic STB Ala foaf and that has been very reliable over the years. Blending fresh cactus and adding excess Lye, pulling with Xylene while hot and then salting with sulfuric acid has served me well for many years. and one can scale it up to quite a lot, 30-50kg fresh material works well! Ive also done this method many times with Limonene however with limonene it takes SO MUCH work to get the alkaloids into the solvent and then also to salt them out. You have to mix it mechanically with a paint mixer on high over and over to get everything out, it really is a PITA. The trade off for not having to deal with xylene is a lot more work!

I like that this tek falls somewhere in the middle. I can deal with the smell of EA, it's not so bad and being able to form crystals is why I used sulphuric acid originally. I would personally prefer to be performing this process with liquid instead of dry cactus but I understand why it is this way the speed of the whole process makes up for its shortfalls from what I can see, even if I have not been able to join all the dots just yet

 

[antichode]

Since nothing would precipitate from my EA I washed the solvent with water, collected it and then reduced the volume down untill it would not go much further. A sticky goo remained which I left to cool. The next day I see crystals forming in the goo. I assume these are citric acid but idk. What should I dissolve the goo into from here? I have IPA or azeotropic ethanol, or EA?

 

[antichode]

I ended up dissolving that yellow goo in IPA, it dissolves with some stirring however the crystals stubbornly stuck around untill I heated everything. I then added more IPA untill precipitation happened all at once and 3G of fine white powder settled out. It’s definitely active as I’ve had a little finger dab and it kept me awake and unmistakably in a cactus headspace for a good while. I’ll do a little a/b on it at some stage to separate out any impurities.

 

[antichode]

And in other news I finally have crystals straight from EA. I dried and processed 2kg of cactus (not including the core) down to 150g and made sure to be thorough with mixing at every stage. Cleared it well and added citric while cold the popped it back in the fridge once it clouded up. It precipitated quickly in the fridge so the crystals are small but it’s looking good so far

 

[merkin]

And in other news I finally have crystals straight from EA. I dried and processed 2kg of cactus (not including the core) down to 150g and made sure to be thorough with mixing at every stage. Cleared it well and added citric while cold the popped it back in the fridge once it clouded up. It precipitated quickly in the fridge so the crystals are small but it’s looking good so far

These are the droids you are looking for , nice one!

Usually no need to put it back in fridge after salting. I do it cold as well and crystals start growing well within an hour.

 

[antichode]

What’s the best way to recrystallise the citrate salt?

 

[merkin]

I think you can do it with just minimal distilled water?

 

[Loveall]

And in other news I finally have crystals straight from EA. I dried and processed 2kg of cactus (not including the core) down to 150g and made sure to be thorough with mixing at every stage. Cleared it well and added citric while cold the popped it back in the fridge once it clouded up. It precipitated quickly in the fridge so the crystals are small but it’s looking good so far

Congrats! So what do you think was the cause of your goo earlier?

PS: As merkin said, no need to use the fridge during salting.

 

[antichode]

I’m guessing a combination of attention to detail with the initial pulls and then perhaps my technique when decanting, perhaps not careful enough.

I’m now using my food mixer for the paste and the pulls. I use the silicone spatula for the paste which gets it fluffy in no time and the sound of it (as it mixes) changes (as you have noted in the thread). Then I swap to the stainless steel K beater and mix the solvent pulls at a reasonably quick rate. Saves on the elbow grease and I think it’s meant more alkaloids into the solvent. Silent still separates well, I just put a strainer over the top of the bowl and tip it through a coffee filter then proceed as usual.


The latest extraction I have done as you suggested and salted at ambient temperature, crystals started forming within a few hours. I knew this powder was weaker so I’ve opted for 300g with 2qt of solvent. The mixer helps to get everything in contact with the solvent and recovery of solvent is still easy. I think getting the right feel for paste consistency does make a difference. I used 690g of water for this run (about 230g per 100g cactus, slightly less that the tek suggests). Perhaps my initial attempts were too wet

 

[antichode]

In the jar is 2.7g from 150g of dry powder (no core)
and 4.6g from 300g dry powder (including core). Better than I expected on the last run and pretty solid for the core and everything.

Hats off to you all, this is a good process!

 

[_Trip_]

Same plant?

 

[antichode]

no different plants, the last extraction on 300g powder was a mixture of maybe three different varieties, the higher yielding one in the jar is from a pachanoi

 

[_Trip_]

I thought that might be the case. In my experiments its usually around the 13% mark for what the the white core contains in comparison to the green layer (per foot). I.e if the green layer contains 1% the white contains .13%. I think recently either in the literature or someone else on nexus found similar results in the 10-20% range.

 

[Loveall]

I’m guessing a combination of attention to detail with the initial pulls and then perhaps my technique when decanting, perhaps not careful enough.

I’m now using my food mixer for the paste and the pulls. I use the silicone spatula for the paste which gets it fluffy in no time and the sound of it (as it mixes) changes (as you have noted in the thread). Then I swap to the stainless steel K beater and mix the solvent pulls at a reasonably quick rate. Saves on the elbow grease and I think it’s meant more alkaloids into the solvent. Silent still separates well, I just put a strainer over the top of the bowl and tip it through a coffee filter then proceed as usual.


The latest extraction I have done as you suggested and salted at ambient temperature, crystals started forming within a few hours. I knew this powder was weaker so I’ve opted for 300g with 2qt of solvent. The mixer helps to get everything in contact with the solvent and recovery of solvent is still easy. I think getting the right feel for paste consistency does make a difference. I used 690g of water for this run (about 230g per 100g cactus, slightly less that the tek suggests). Perhaps my initial attempts were too wet

Interesting. Thanks and welcome to the xtal party . Hope you enjoy the tek.