TEK Ethyl acetate approach [CIELO]

[merkin]

Thanks shroombee, appreciate the details as I am not educated in these things! Will also take your advice re the 50g chunks

 

[Loveall]

Merkin, perhaps if your yields are low you can try warmer pulls. Don't freeze the ethyl acetate, keep it room temperature.

I thought freezing would be fine for people but now I'm not so sure based your results. Old cactus powder may break down into stuff that is getting in the way of the extraction. I don't know. Or maybe you need to make sure the extract is free of debris and/or droplets.

Did the water evaporate and you get to check out what precipitated. Also, any news on the filter stuff?

 

[merkin]

I will try again with another 100g in two 50g batches as before to see if the results are any different. Maybe one cold and one room temp - is there any difference in the tek if using room temp EA?

As for the evap theres basically what looks like a hard tackcky 'dirt' or 'grime' layer on the bottom of the petri dish. Nothing really worth scraping even. The filter paper has a few grains of something, but again, less than a mg. The two blobs kinda soaked into the paper - same size but now embedded. Gonna write this one off and start again.

Gotta get me some crystals!

Re: cleaning and reusing the solvent - roughly what volume of Na Carb water to volume of EA? In that part of the tek you also mention sodium carbonate and then 'excess calcium carbonate' - is that intentional or typo?

 

[Loveall]

That was a typo, fixed.

I use excess soda was so that some remains undissolved in the water. Around 30g of sodium carbonate per 100ml of water should work.

Good luck.

 

[merkin]

Thanks Loveall. Sorry to be a pest with all these questions, but I don't have much background knowledge of these things! So I hope two more is not too much:

Is the cold temp of the EA important only for the pulling? ie Doing the whole pull procedure as fast as possible while the bottle remains super frosty and then once its pulled its OK to let it warm up before getting to the Citric Acid part (and where I can use the stirrer as per shroombee). I am guessing its important to do the entire pull sequence in as little time as possible as the water/cactus sludge is slowly warming up?

When cleaning the solvent - roughly how much/proportion of the saturated sodCarb solution per ml of the Ethyl Acetate?

---Did 50g run---
50g cactus, 12.5g lime 150g water with ice formed in bottle.

6x60s Pulls ~ 400ml EA total, filtered twice through coffee filter, icy freezer cold EA. First "pull" was pretty much 0ml solvent recovery from ~100ml added.

Mag stirring to vortex, added 6g citric acid at once, stirred 6min approx, still cloudy, vortex not visible. Added 1g more acid 2x, total 8g. Cleared a bit but not properly. After ~9 min stopped stirring and filtered after removing stirbar. Big blob of redddy brown stuff (what I saw before the first try but it was a lot less then) on filter and much more residue on bottom of beaker. Very gooey/sticky.

Solvent liquid still not completely clear. Should have done more acid?

Much more action this time from the mag stirring. My liquid from pulls is much more yellow and cloudy than Loveall's beautiful clear green. Will let everything dry and/stay as is (solvent & cactus).

** edit:
Added another photo. As that gooey red stuff slowly dries into the filter its starting to look very different and definitely sparkly. I'm starting to have a good feeling about this now - hope thats not citric acid in there! Can't believe how much more "stuff" there was with the 50g than my first try with 100g. Shroombee, thanks for the info on the stirring, I think its made a huge difference. Maybe my source powder is much more 'sanchez' and hence the dirty river water look.

 

[grollum]

@merkin

The cold temperated EA is a result of Loveall's optimization approaches and gave a more simple and stable process in Loeveall's attempts. It worked without the cold EA several times as well before. Doing the EA pulls in a certain time is needed to not pull to much unwanted stuff. Since EA is quite aggressive the longer you let it sit, it will pull more unwanted stuff.

I am wondering why your EA pulls are so cloudy already before salting with citric.
The resulting extract looks to me like it could be mostly citric acid.

If there is to much plant matter and other unwanted stuff in the EA after pulling from base it might make the crystallization harder or even prevent it.

What type of filter do you use?
In my case the EA always was a clear green liquid before salting.

 

[Loveall]

Thanks Loveall. Sorry to be a pest with all these questions, but I don't have much background knowledge of these things! So I hope two more is not too much:

Is the cold temp of the EA important only for the pulling? ie Doing the whole pull procedure as fast as possible while the bottle remains super frosty and then once its pulled its OK to let it warm up before getting to the Citric Acid part (and where I can use the stirrer as per shroombee). I am guessing its important to do the entire pull sequence in as little time as possible as the water/cactus sludge is slowly warming up?

When cleaning the solvent - roughly how much/proportion of the saturated sodCarb solution per ml of the Ethyl Acetate?

---Did 50g run---
50g cactus, 12.5g lime 150g water with ice formed in bottle.

6x60s Pulls ~ 400ml EA total, filtered twice through coffee filter, icy freezer cold EA. First "pull" was pretty much 0ml solvent recovery from ~100ml added.

Mag stirring to vortex, added 6g citric acid at once, stirred 6min approx, still cloudy, vortex not visible. Added 1g more acid 2x, total 8g. Cleared a bit but not properly. After ~9 min stopped stirring and filtered after removing stirbar. Big blob of redddy brown stuff (what I saw before the first try but it was a lot less then) on filter and much more residue on bottom of beaker. Very gooey/sticky.

Solvent liquid still not completely clear. Should have done more acid?

Much more action this time from the mag stirring. My liquid from pulls is much more yellow and cloudy than Loveall's beautiful clear green. Will let everything dry and/stay as is (solvent & cactus).

** edit:
Added another photo. As that gooey red stuff slowly dries into the filter its starting to look very different and definitely sparkly. I'm starting to have a good feeling about this now - hope thats not citric acid in there! Can't believe how much more "stuff" there was with the 50g than my first try with 100g. Shroombee, thanks for the info on the stirring, I think its made a huge difference. Maybe my source powder is much more 'sanchez' and hence the dirty river water look.

Like grollum said, cold EA is to reduce plant stuff and make the crystallization more robust, should still work with room temp, but it will need more citric and product before washes will be more sticky.

For solvent reclaim I use 1 part saturated water for ~ 5 parte EA.

Your pulls should not be cloudy like grollum said. How long did you stir the cactus paste (I do it for a few minutes, and it is a bit of work on the wrist)? Make sure paste is smooth/homogenous with no white clumps of lime. It looks like maybe you got some lime in EA (?), that won't happen if the initial paste is well stirred and all the lime is mixed in.

In this case I would have let the extract settle in the fridge for a couple days (not sure if you tried this already), to see if the clouds settle, and then decant. Some of the brown stuff may settle too. It is important to try to get the extract clear before salting.

Product could be the real thing. Since you salted while cloudy there may be some calcium citrate (a health supplement known as citrical I believe). I think there should be some real product there. I do not think there is any citric acid since that is all dissolved. I would was the product you have with some fresh ethyl acetate see if you can remove some of the brown.

Your cactus material may be more difficult to work with. I was thinking that if it was stored for years, it could have broken down into stuff that only have and we haven't encountered yet (that's why it is not green). Just a guess.

There is a way to treat the paste in the microwave before pulling. That also works and I've tested it with my cactus. It could help finish breaking down some of your paste into simpler saponified molecules (?). I think may be with trying in your case. If it works better, could be a way to make the TEK more robust. To try this:
- Make the paste as usual
- Microwave in short spurts mixing in between microwave runs. Goal is to reduce water by 2/3 (if you added 150g of water, microwave until only 50g remain). Watch microwave closely so it doesn't boil over. Paste will go from crumbly to smooth to crumbly again. Cool this treated paste in the fridge and it is ready for extraction.

 

[shroombee]

Loveall makes everything look like fun. So I pulled out my lab toys to get back into the game. :lol:

Results from my latest Run #6. This is a followup to Run #5, in which I reported the process and results here.

Purpose

Investigate yield with 15 minute basing time versus 72 hour basing time of Run #5 and 24 hour basing time of Run #4;

Constants with the previous runs we're comparing with

- Same source material. Run #6 was powered with Run #4 and #5 to eliminate variations across cactus chips;
- Pull technique was 30 seconds very light stirring, rest 2 mins and 30 seconds, then decant;
- All materials are at room temperature;
- Decant with some pressure on the french press to squeeze an extra 10-15 grams of solvent out of each pull;
- About 100 grams solvent added per pull, except the first pull in which 150 grams of solvent is used;
- I'm retrieving basically the same amount of solvent that was added for each pull (except the first pull in which the cactus holds on to some solvent);
- Salted with 15 mg per gram of extract;
- Aggressive stirring with magnetic stirrer for 10 minutes;

Results

1) Total yield was 1.604% (802 mg out of 50 grams Peruvian Torch).

2) There is NO DIFFERENCE in yield between 15 minute basing, 24 hour basing, and 72 hour basing. Yields between Run #4, #5, #6 are well within the margin of error in my weighing, filtering, and collection techniques.

3) I didn't observe any notable difference in the texture or workability of the cactus with the different basing times. Except I recovered slightly less solvent with Run #6 than prior runs. Run #5 recovered 94.8% of solvent (622 grams recovered out of 656 grams added). Run #6 recovered 92.0% of solvent (610 grams recovered out of 663 grams added). Why the difference? I don't know. Some guesses:

. A) Different basing times;
. B) Temperature difference. Room temperature is about 10 degrees warmer in June than April when I ran the previous experiments;
. C) Run #6 was powdered with run #4 and #5, but Run #6 sat around for 2+ months. Could the powder degrade or oxidize, thus affecting how much solvent it holds on to?
. D) May have been slightly more aggressive with my stirring;

In any case, the small difference in solvent recovery had no effect on the yield.

I think this is a very important result for this tek. It tells us the 8 minute mixing time plus 15 minute resting is more than enough basing time to get maximum yield. After mixing, any basing time between 15 minutes and 72 hours is fine.

And this result evolves some previous thinking where it was believed that long basing times with lime break down more cactus material or allows more mescaline to freebase. At least with this tek, that's not the case. Long basing time is not necessary and it does not increase yields.

Next Steps

Powder a new batch of cactus to run the following experiments:

1) Repeat 15 minute basing with 6 x 3 minute pulls to get a baseline yield on this new source material;
2) Shorter pull times;
3) Chilled ethyl acetate;
4) Slow diffusion;
5) Maybe try the microwave;

 

[Loveall]

Thanks shroombee. I have also found that a few minutes of basing time gives same yield as 24h.

If you try the chilled extraction (and/or microwave breakdown) I suggest you test dropping in citric acid and letting it slowly diffuse. Long crystals may grow over 24h without as much plant stuff (chlorophyll, etc).

The largest xtals I've gotten so far (+10mm in diameter) minimized plant stuff with microwave (remove 2/3 water with several pauses/mixes) and chilled extraction (all in) simultaneously. I did a warm pull salted separately and some precipitate formed but it was not large xtals. I think chilled ethyl acetate is important to get the larger crystal growth.

 

[MtHighlands]

Just a cross post on my attempt at this tek. Ran into some issues, not sure what happened.


I got promoted today . So it great to be able to post in here. I really like the idea of this tek. Thanks Loveall, Shroombee, and others for your efforts here. I’ve been following closely and this has been a fun exploration.

 

[shroombee]

Thanks shroombee. I have also found that a few minutes of basing time gives same yield as 24h.

Oh I see here in this post that you already confirmed 10 minutes basing yields the same as 24 hours. Guess I could have saved myself a test run. :roll:

If you try the chilled extraction (and/or microwave breakdown) I suggest you test dropping in citric acid and letting it slowly diffuse. Long crystals may grow over 24h without as much plant stuff (chlorophyll, etc).

The largest xtals I've gotten so far (+10mm in diameter) minimized plant stuff with microwave (remove 2/3 water with several pauses/mixes) and chilled extraction (all in) simultaneously. I did a warm pull salted separately and some precipitate formed but it was not large xtals. I think chilled ethyl acetate is important to get the larger crystal growth.

I might jump to the all-in and if it doesn't yield the same, then work backwards and troubleshoot.

 

[merkin]

@merkin
If there is to much plant matter and other unwanted stuff in the EA after pulling from base it might make the crystallization harder or even prevent it.
What type of filter do you use?
In my case the EA always was a clear green liquid before salting.

OK, thanks I will look into that side. Maybe things will improve when I try my own source materials.

I used coffee filters at begining and a '1893' Qualitative at end to catch residues.

Like grollum said, cold EA is to reduce plant stuff and make the crystallization more robust, should still work with room temp, but it will need more citric and product before washes will be more sticky.

For solvent reclaim I use 1 part saturated water for ~ 5 parte EA.

Your pulls should not be cloudy like grollum said. How long did you stir the cactus paste (I do it for a few minutes, and it is a bit of work on the wrist)? Make sure paste is smooth/homogenous with no white clumps of lime. It looks like maybe you got some lime in EA (?), that won't happen if the initial paste is well stirred and all the lime is mixed in.

In this case I would have let the extract settle in the fridge for a couple days (not sure if you tried this already), to see if the clouds settle, and then decant. Some of the brown stuff may settle too. It is important to try to get the extract clear before salting.

Product could be the real thing. Since you salted while cloudy there may be some calcium citrate (a health supplement known as citrical I believe). I think there should be some real product there. I do not think there is any citric acid since that is all dissolved. I would was the product you have with some fresh ethyl acetate see if you can remove some of the brown.

Your cactus material may be more difficult to work with....

There is a way to treat the paste in the microwave before pulling. That also works and I've tested it with my cactus. It could help finish breaking down some of your paste into simpler saponified molecules (?). I think may be with trying in your case. If it works better, could be a way to make the TEK more robust. To try this:
- Make the paste as usual
- Microwave in short spurts ....

Thanks for the suggestions.

I stirred the paste about 3 minutes with the ice cold water in french press. One thing that may have led to problem is that I halved the tek amounts - but the 150g water to 50g/12.5g lime/cactus mix was far more liquid than paste - so after sturring a bit I decided to ad-hoc put in some more cactus powder and a small bit of lime on end of a teaspoon to make the paste thicker. Might have screwed up here? But ultimately I need to get the clarity addressed.

Question: Will a lengthy delay at the EA stage as you suggest (before salting) affect the result - ie leaving it a few days or so to settle in fridge? Or is there plenty time to refine that solvent solution before adding acid? Basically I guess the question is how stable is the solvent pull mixture over say a few days or does it deteriorate.

Washing the result - would I just mix that around with EA and decant in a manner similar to cleaning dmt fumarate with acetone? Or must it all dissolve in hot water and evaporate?

The good part though:
As this was yesterday, the red 'gooey' stuff has mostly dried away and the texture is now more hard crunchy, crumbly and crystally. Based on the marquis reagent test I would say things are looking promising and well worth more tries! I will try the microwave process too.

Thanks for all the help, I'm feeling a lot more positive about this after this round. I will persist with the icaro powder I have as my fresh harvested pedros are going to need some time to sit in the dark before getting processed. I have some huge cuttings now so in time I will have that to use and my tek skills will have hopefully improved by then.

*** edit:

Ermagawd! I got cystals! Just checked the left over EA bottle from the rightmost solvent above (labelled "R:..." ) and there are some beautiful little babies and one stunning cluster! It basically just sat on the shelf since yesterday morning, clarified itself and delivered this unattended.

Any ideas about how I might process or clean or re-x the original red colored residue which is now almost fully dried and crunchy and a lot more clear/whitish. The mesc is definitely hanging around in there I'm really sure now. Fully excited but a bit confused as to what it all means!? Feel like I'm stumbling about in the dark in aladdin's cave


marquis:

 

[Loveall]

I have not noticed any issues in delaying salting. On the other hand the extract needs to be clear before salting: that is very important, I would not break that rule (funky things happen otherwise).

I would mix the paste longer than 3 minutes. I go for 10 minutes. If you mix the water and lime together first, all the lime is wet. Then add the cactus on top of that without Dela delay, before the milk of lime starts to settle. I've updated the TEK.

Adding the extra lime may have been an issue. After the cacti absorbs the water it is going to be harder for that lime to get incorporated. I think that is why your extract was cloudy: the extra lime was free/dry enough to move into the ethyl acetate. In my own experiments when dry lime is the issue it looks just like your pictures.

I think you eventually got xtals because the solution didn't fully xtalize initially (because of like/gunk). Later with more time it xtalizes further.

To wash your first yield (brown stuff) rinse with fresh ethyl acetate.

The xtals you eventually got are beautiful, congrats.

 

[merkin]

...the extract needs to be clear before salting: that is very important, I would not break that rule (funky things happen otherwise).
The xtals you eventually got are beautiful, congrats.

Thanks Loveall. You are totally right about the clarity. Also about the lime part. I read shroombee's post in the other thread and followed that this time (make lime water and then add cactus and mix well and rest). You definitely need that in the tek for people like me I think you have a lot of experience in this sort of tek (and chem in general) and you do things instinctively or understand much more of the underlying principles which you omitted but are essential for noobs and uneducated idiots like me. The closest I got to this type of 'dry' tek (?) was doing Gordotek once.

But now I understand what I didn't before. The pics below will show progress. I continued doing shrombee's 'stir & bomb' method so as not to change too much, but spent much more time on the pulls - also following his method (room temp - stir 30" - wait 3'...). It was much more leisurely and peaceful and I think it allowed me to be a lot more accurate and careful (not worrying about freezing stuff warming too much etc).

I will try and clean what I made before, but still happy to lose it all in the interests of learning. The crystal farm is still growing so whatever I left in there is a lot. My next run I will try your technique for adding the acid since I would love to see all those crystals. I understand the difference now between the slow version crystals and the smaller 'powder' I got this last time. But the marquis test is the most perfect Ive ever seen with that 'powder'.

Much gratitude to you & shroombee (& other nexians) for all your help in debugging my process/methodolgies here - you helped me learn fast and fix mistakes. I feel like I've hijacked this thread enough now. I understand the tek pretty well now and will only improve from here. The superiority of this tek over the old A/B xylene, HCl titration etc is just phenomenal. Well done and thank you!

Pics: -1- Clear liquid pull (suspect my gold colour is because source material is old - my paste is brown too not green) -2- mesc raining down! -3- marquis test on the 'rain'. Its gonna just get better from here on!

 

[MtHighlands]

Ermagawd! I got cystals! Just checked the left over EA bottle from the rightmost solvent above (labelled "R:..." ) and there are some beautiful little babies and one stunning cluster! It basically just sat on the shelf since yesterday morning, clarified itself and delivered this unattended.

Congrats, my friend. I bet you had giant grin when you saw the crystals crashing out.

 

[Loveall]

Merkin, thanks for your constructive feedback and congrats on the result.

I'll add more details to the TEK. Also, we can switch it back to room temp pulls. The chilled path is indeed a little trickier, we wanted to make the TEK more robust with it, but of it causes difficultues during the process them it doesn't help.

Your old cactus paste color looks a lot like fresh cactus paste + microwave. Seems like time degraded your chlorophyll.

Perhaps microwaving to ensure chlorophyll breakdown is one thing that can make the TEK more robust. It will also ensure a lot of paste stirring during microwaving which will surely produce a paste ready to pull and well mixed.

I think I'll update the TEK in the next few days, but feedback welcome. Wanting to detail the simplest and most robust process we are aware of.

 

[merkin]

Wow!

Final results for the weekend: all cleaned with EA, filtered & dried - a very light white-tan 'powder' with some needle crystals thrown in - total yield 2.876g from 150g cactus powder, almost 2% yield. Loveall, your tek rocks!

Wasting the first 100g of cactus powder last weekend kinda sucks (sadly I didn't heed the nexian Rule #1: "never throw anything out till you're sure" ) but I guess school fees are school fees. I still have over 550g of that Peruvian powder which, while very old, has certainly lots none of it's special power.

Thanks again everyone for the help, next mission: Crystals... onward and upward

PS. This is Mesc Citrate right? Recommended dosage: ?

 

[Loveall]

Yes, this is mescaline citrate.

We *think* it is anhydrous but are not sure. I tried to dry some in an oven and saw no weight change for what that's worth. We also think we are forming the full salt because all 3 pKas of citric acid are < than the pKa of mescaline.

Comparing to other mescaline salts:

- Mescaline HCl: 248 grams per mol of mescaline
- Mescaline Sulfate dihydrate: 278 grams per mol of mescaline
- MescalineCitrate: 275 grams per mol of mescaline

So Mescaline Citrate is 90% as strong as Mescaline HCl (e.g. 2g of mescaline citrate are equivalent to 1.8g of Mescaline HCl). Mescaline citrate roughly equivalent to mescaline sulfate.

As for dosing, guidelines are here: Mescaline - DMT-Nexus Wiki

You can convert your current powder into long needles by dissolving it in warm water and letting it evaporate slowly. I recommend you try this if interested in the needles.

I always wash the xtals before the EA dries. Seems to work well that way.

Also, I have updated the TEK to be room temperature, since the chilled approach was giving people problems.

To all who got the TEK to work: Please feel free review and update as needed, especially if there are details that are missing that could help others.

Congrats on the result merkin. And many thanks to shroombee who has really helped make this TEK practical and accessible

 

[Loveall]

TEK is a lot more wordy now. Hopefully this makes it clearer and more likely for folks to get it right on the first try.

To everyone who is getting xtals: Please feel free to edit the TEK if you can add a detail that was important to you. Also, add (but do not replace) pictures if you think they are representative of what others may see if and if it would be a different looking picture from what is currently in the TEK. If you fundamentally disagree with a step let's discuss here first.

Thanks.

 

[shroombee]

Final results for the weekend: all cleaned with EA, filtered & dried - a very light white-tan 'powder' with some needle crystals thrown in - total yield 2.876g from 150g cactus powder, almost 2% yield. Loveall, your tek rocks!

Congratulations - that's a great yield!

I think chlorophyll itself and maybe other plant stuff interacts with mescaline in solution and makes it more difficult to crystalize.

I'm not sure chlorophyll interferes with the xtalization because my extracts are a beautiful deep emerald green and I xtalize fine with 5 mg/g. Just something I noticed from looking at other people's extract photos. I'll take some daytime photos on my next runs to show the deep green color.

Edit: I xtalize fine with 5 mg/g and aggressive stirring. I haven't tested slow diffusion yet with all the latest process refinements.