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TEK Ethyl acetate approach [CIELO]

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shroombee said:
Loveall said:
I do think we may need better water control in the TEK. I'm going to test chemical drying to again (extract and reclaim). If I see no issues, I suggest we add these steps to the TEK. Even if there are no improvements in my particular case, it could make results a lot more uniform for everyone. Can't hurt to control one of the variables better anyway.
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The inconsistent results people are seeing may be due to water, other alkaloids, plant matter, or a combination of all three. Maybe there's others?

Before recommending a chemical drying process, can we investigate the degree in which water impacts xtalization. For example, take an extract and split it into four jars. Use one as a control and add a different amount of water to each of the other three. Then salt with citric acid. Note the ease/difficulty of xtalization and resulting yield.
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I think adding water after extracting adds more variables, since that is not what will happen when people extract.

The best thing to do would be to split into two jars right before salting. Chemically dry one side. Add citric acid and see if there are any difference.

Unfortunately, since the TEK usually works as-is for you and me, the result may be null (no significant difference: crystals in both jars). Ideally we get someone that sees goo or gets clouds with no precipitation in the undried jar and xtals in the dried jar.

I could be wrong, but I think that a chemical dry is best practice in the lab, because the result will usually be matched or better to no chemical dry. There are also _Trip_'s observations with water.

I think my issue was using MgSO4 as a drying agent in some teste.Turns out it is not recommended for ethyl acetate loaded with an alkaline product. I now thing Na2CO3 or CaCl2 are much better options.

The other variables are also important. Perhaps doing the chemical dry would remove the water content variable so we can better compare different cacti sources, etc.
 
FYI, that some work with CIELO has been done in mycotopia. Seems to be working ok (on the second attempt)


I haven't found time to do new Chemichal dry splits before salting (using CaCl2 or Na2CO3, NOT Epson salt). Will get to it sometime. Hoping for less process noise and more uniform results for everyone with an added Chemichal dry.
 
I too was hoping to find time to do another run this time drying the solvent before salting. But unfortunately I have been flat out at the moment. I still hold the theory that water maybe influencing yields. Now that the Tek is making rounds it'll be good to see what others find.

Good work Loveall and all involved. Thanks for the update.
 
Did another run,(after combining all pulls) I split the ethyl acetate pulls 50/50 into 2 different jars. One jar of EA was dried with calcium chloride and then the calcium chloride was filtered out before salting with citric acid.

Yields did not change between the two jars (15-10mg difference). However the 'drier' EA formed crystals faster. The jars where left for 24hours before they were cleaned and evaporated.

Keep in mind the microwave option was utilized. So 2 thirds of the total water content was steamed off during microwaving step. The limitation here is that a difference in yield man not have been observed due to already low water content.



In addition, I usually use the green skin layer only (no wax, no spines, no white pulp) for this TEK, however this time my dry powdered cacti material included the wax layer and spines (inner white pulp was removed). Although this saved preparation time yields dropped from over 3% to .7% using the same cacti material as previously used. (2% drop to .5% in HCL equivalency approx).
This may have been a bad run or the wax and spines could account for 75% of the weight and contain no mescaline. Food for thought.
 
Thanks for the experiment _Trip_. Did the CaCl2 pellets swell and seem to absorb water or did a water layer form temporarily at the CaCl2? Do you know what was the time gap in xtalization time?

Since you saw no net negative, I think chemichal drying could help folks that are getting more gooey results, very slow xtalization, or even no xtalization at all.

Based on your result, when I do the experiment, I'll add citric in small amounts, see if without excess citric there is a bigger gap in xtalization time. When water is present, excess citric may be important to get a "manske" going (with naptha/DMT/acetone/fumarate it is not possible to add high amounts of fumaric since it won't dissolve in naphtha, and in that system the water content is very important). I'll also skip the microwave step too, that may enhance the differences.

Finally, based on your results I'm leaning towards adding a chemichal drying step before xtalization as an option. While not "necessary", it would standardize the process (professional labs do this) and be insurance for people that end up with a lot of water in their extract for whatever reason. I'll also test washing soda straight out of the arm and hammer box.

Shroombee, I think I concluded that drying was worse in general for xtalization by mistake. I had used MgSO4 to dry the solvent. I have since learned that is not recommended for ethyl acetate. It is also acidic and could have crashed some product during the drying stage. We should be using alkaline drying agents that will keep the product in the solvent as FB. I think now that my issue was choosing the wrong drying agent. The observation I had was for epson salt in particular, I should not have made a general statement. CaCl2 and Na2CO3 should be better choices.
 
Loveall said:
Thanks for the experiment _Trip_. Did the CaCl2 pellets swell and seem to absorb water or did a water layer form temporarily at the CaCl2? Do you know what was the time gap in xtalization time?

Since you saw no net negative, I think chemichal drying could help folks that are getting more gooey results, very slow xtalization, or even no xtalization at all.
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I did not notice the pellets swell per say, the process seemed no different than using MgSO4 to dry, say acetone. I added quite a bit of CaCl2 pellets and since there was little water content in there already there was no noticeable swelling. I did not see a temporary water layer form.

Hard to judge the time gap as both initially crystalized quickly but more crystals formed faster in the dry EA. It was a visible difference but trying to quantify times and percentages with the naked eye would be near impossible. As you mentioned using the smallest amount of citric acid would be the best way to figure out a time difference. Recording a time lapse on a camera would work well to keep track of the difference.

I should mention that 10-15mg was the negative in the dry EA (but i think 10-15mg could have gone either way). Close to 400mg formed in both jars so a loss of 3.75%. There was a very slight decrease in volume of EA so I gather the CaCl2 did its job and removed a little water.

As previously found, CaCl2 breaks down into a separate goo layer after sitting in EA for a longtime. I believe it reacts with the water and other alkaloids and forms a green sludgy layer. So I recommend filtering out the CaCl2 sooner rather than later. Note filtering was done with lab filters. (What's interesting and there's a photo link in one of my previous posts I recommend people have a look, when CaCl2 is added after salting it seemed to helped additional mescaline citrate crash out but unfortunately I couldn't separated it from the sludge layer of CaCl2 to confirm it). Again makes me think excess water may be an issue.

Loveall said:
Based on your result, when I do the experiment, I'll add citric in small amounts, see if without excess citric there is a bigger gap in xtalization time. When water is present, excess citric may be important to get a "manske" going (with naptha/DMT/acetone/fumarate it is not possible to add high amounts of fumaric since it won't dissolve in naphtha, and in that system the water content is very important). I'll also skip the microwave step too, that may enhance the differences.
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I think skipping the microwave step would be the best way to test the theory on if water is causing an issue or not.

Loveall said:
Finally, based on your results I'm leaning towards adding a chemichal drying step before xtalization as an option. While not "necessary", it would standardize the process (professional labs do this) and be insurance for people that end up with a lot of water in their extract for whatever reason. I'll also test washing soda straight out of the arm and hammer box.
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I definitely think its a good idea (a cheap option too), but yes maybe not necessary, especially for the microwave option. However I would bet it makes a difference if one chooses not to microwave. I don't have too much more material to play with of the same cacti, but I'll continue to test what I can.


I was surprised by the difference in skin only vs the addition of the wax layer and spines. I would like to test this difference again before testing a non microwave test/ dry EA. But I should have enough material left to do maybe both. I will keep ya posted.
 
Yeah that's a good idea, something I should have done.

Edit: Just for those interested, I can confirm from my own experience that if using the green layer of the cacti only you can see 4 times the yield from one extraction. The wax layer and spines seem to hold a bit of weight to them. I am yet to experiment with the whole cacti material including the white inner pulp (dry and grounded) but i will soon. I would wager yields decrease further.

I acknowledge this information is more or less known but its good to put a rough number to it for this extraction. Especially since it appears, at least in my experience, to be purer and higher yielding than an A/B extraction.

So if you want to use less solvents etc and spend less time doing multiple extractions, more preparation time can pay off. Ofcourse there is the same amount of mescaline in your material either way.
 
Hope lots of folks are getting xtals out there with this process.

One "standard" lab technique we haven't tried is a brine (NaCl saturated water) wash of the EA before salting with citric. It should reduce the amount of water in EA and remove impurities. May be useful to deal with different starting plant sources for those that are getting goo or sticky product instead of quickly forming white xtals.

I've read that a brine wash during a workup of mescaline FB in CH2Cl2 does not affect yield. Would expect the same for EA 🤞

I will eventually test this. Will do the simplest version of the TEK (no microwave, no cold, no chem drying) and add a quick EA brine wash split. See if the xtals from the EA that had the brine wash are larger and stick less to the wall. If it works consistently, we could simplify the TEK and converge to this one option (new suggestion in bold)

- Make cactus alkaline paste (20 min)
- Quick EA extraction (30 min)
- Wash EA with brine (10 min?)
- Salt EA with citric (5 min)
- Collect xtals that form in EA (15 min of work one day later)

Interestingly, chlorophyll can be removed by brine.
 
Sorry in advance if this is off topic—if it is of any value, here’s a write up of an experiment in using minerals (in my this case food grade alum/acid bentonite [vinegar then oven baked]) and freezing agar (molecular gastronomy trick to clarify liquids via ghetto ultrafiltration) to reduce the goo-factor in my alcohol/water tar from dried torch chips. Cactus Tar experiment—screwing around with Minerals/Agar/Vinegar. Safe? Efficient?

It was a turning point in my cactus extractions, the results of which had been mixed at best (mostly because of the volume of the final result).
Q9SCo4Ll.jpg


I will study the thread—which I must say is a gold star collaborative effort. I wonder if either using a flocculant/metal sulfate (alum purchased from a Chinese grocery), or adsorption of a fb phase onto acid bentonite, drying, then eluting (that doesn’t sound like a word) into ethyl might be a reasonable step to clean up the “goo”.

Godspeed.
 
Here's a late update from the butyl acetate variation: some tiny, needle like crystals were obtained from the second attempt, which used completely rotten, dried out and partially-eaten-by-beetle-larvae material. This to me indicates that if assured potent material were to be used, the "CIBLO" variation would work. I think the tiny amount of crystals reflects the tiny amount of alkaloid that was left in the remnants of less decomposed plant material. A lot of the bulk will have comprised waxy outer skin and woody veins, neither of which is going to be particularly rich in alkaloids.

It remains to be seen whether the crystalline material recovered after freezing the filtered extract from the first attempt is anything other than citric acid. That attempt was with rotten to the point of complete liquefaction PC pachanoi - another assured way of achieving inconclusive results, it seems 😁 Nonetheless, these crystals still need to be weighed and perhaps a recrystallisation from aqueous acetone might be instructive, largely to see if needle-like crystals form instead of the not-quite-right citric acid-like stuff that appeared at first.
 

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Thanks to Loveall, Shroombee, and all others who have contributed to the development of this tek.

There hasn’t been any discussion on this thread for a while, so i thought I’d contribute my results so far.

I have done several extractions, using different variants of the process and different sources of material, with varying results. Except for one source of material that apparently is nearly devoid of alkaloids (ran it 2 separate extractions), my runs have produced more yield than expected, with inconsistent results in the appearance and “taste” of the product.

I have yet to see the beautiful, white crystals form in the post-salting jar, though crystals do form in the evap dish. I also have not had much precipitate large enough to be collected in the coffee filter paper. Part of this is because I am using the magnetic stirrer approach, which because the precipitate particles seem so small I have left them in the jar, washed-evap’d with fresh EA, and then warm water washed-filtered into a glass dish to evap-crystallize. Using different source materials has likely confounded results as well.

The substantial scrapings have yielded 2-4% from 4 of 6 runs, of white/yellow/brown, each with a noticeable sticky texture, and definitely a more acidic “taste” than the also bitter “taste”; even after powdering, fresh EA washing, and redisolving/evaporating in warm water. I am currently bioassaying for threshold level on the first run, so i can’t speak to the potency of the runs yet.

I have a background in chem lab techniques, and believe I am now up the learning curve as far as the process steps are concerned. I have used the standard process, as well as the microwave pastemaking, solvent/paste chilling, and magnetic stirrer process options.

I have 3 new source materials that i will be running soon, using the materials that Loveall specified, and the pickling lime that Shroombee linked. I will have sufficient material to make several small runs, which i plan to do using the microwave-cold chill process along with side-by-side use of Loveall’s passive salting/crystallization process and Shroombee’ s stir and dump process. Hopefully i will be able to produce sufficient beautiful white needles that collect in the initial filtering. If not, perhaps those with better results will help me debug my process.

Again, thanks to all who have contributed to this simple, quick, relatively safe extraction process!
 
Cool. Color of the xtals can indeed vary. The taste is bitter, but not overly so (e.g. compared to a resin which is much more bitter). One reason for high yields by mass is the heavier salt form as you may know already.

Thanks for the update 🙂
 
Hi there and thanks for developing this tek. I have a question for you..
Can I use a traditional oven with thermostat to achieve same results than using a microwave one?
If yes, how can I do that, I mean what are the steps to follow?..temps, time etc..
Thanks in advance.
 
Nachooo said:
Hi there and thanks for developing this tek. I have a question for you..
Can I use a traditional oven with thermostat to achieve same results than using a microwave one?
If yes, how can I do that, I mean what are the steps to follow?..temps, time etc..
Thanks in advance.
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I don't know. In theory the microwave helps break down chlorophyll so xtalization is better and ethyl acetate can be reused many times. The TEK has a link to literature going into more details. It's all speculative because we don't measure things directly, but the green chlorophyll color does go away.

If you try the oven and the paste color changes from green to tan that would be promising.
 
Thanks for the quick response, also I understand that if the cactus powder is old and mostly yellow or light brown, the microwave step has no sense...
 
Maybe if green powder is used,spreading it and exposing it to pure UVA/B light will degrade the chlorophyll...dont know about the other actives though..
 
Nachooo said:
Maybe if green powder is used,spreading it and exposing it to pure UVA/B light will degrade the chlorophyll...dont know about the other actives though..
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I wouldn't worry too much about it. I still got good results with green powder from the outer skin without a microwave. Xtals were smaller and the solvent color made me wonder how many times I could reuse it. Neither a big deal for me.
 
To extend the life of your solvent, you might try the chilled pull option. My chilled pull was clear light-yellow, vs green when run at ambient temp, with or withoutt microwave.

I may do a side-by-side to see if yield is affected.

If you can spare 25g, develop your oven idea and test it.
 
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