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TEK Ethyl acetate approach [CIELO]

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pH levels based on the color of the pH strip? I think that is hard to measure.

We can add that the pulls should be basic on pH paper, neutral after a wash (if that is needed), and acidic after salting (cause we want to use excess citric). I hesitate to put down a number because pH paper is subjective. Also, not sure it reacts the same way in EA for different pH paper material, it is made to match a standard in water I think.

Sounds like you successfully converted old goo to xtals, congrats! How much product do you think was in the 2g of goo (how much cactus went into it).

A small suggestion: For the intial cloudiness before salting, I would have let it sit in the fridge overnight, see if it settles.
 
I wasn’t saying we add pH testing to the wiki, at least not now. I was saying we should report it in our experiments. You have already shown, and i know it to be so, that there is a big and “measurable” difference between pH 8-ish, 6-ish, 4-ish, and 2-ish. I see no reason why these levels can’t be reliably and directly determined with pH “paper” (mine are actually plastic; Millipore 1.09535.0001 MColorpHast pH 0-14 Universal indicator) for any liquid, not just water.

I have no recollection of how much dry material I used, and no clue as to it’s approximate M%. At the time, I was just roughly running the tek to see what it produced, and whether the logs I had sourced, from a verbose and commonly agreed to be unreliable source, had any M in them. If I can recover an extra half gram of needles from this crap and not significantly reduce the quality of the entire load, I will consider it a worthy effort, and a useful method to deal with a few learning curve runs.

If people cannot produce white needles after a few runs of this tek, they have no business doing extractions with organic solvents, and should stick to boiling the plant or eating it raw. I can’t really justify wasting my time trying to salvage a few crappy runs any other way. I don’t expect to produce crap from this great tek ever again.

Yes, settling it in a fridge over night, or running through a lab filtration system (which I have), would have improved the chances of getting the cloudiness out. But, when I considered it, I decided to see what would happen if I just took the lazy approach.

I am not saying, dissolving the crap and throwing it in with a regular run is the best approach, just that it’s better than the other alternative that you mentioned, and is safer than eating product that obviously does not look or taste like the proper end result of this tek.

I have several more g of crap, i’m going to see what I recover from them in a couple smaller runs of the same material. Will report results in the other post above.
 
Cheelin I think it is a good idea. If you get goo on your first extraction ever, just add the goo to your second extraction and hope it works out the next time just by getting better at the extraction technique.
 
Hey Loveall just checked out the updated Tek,

One question (I must of missed something), the tek says:

"if the paste is too dry it will block ethyl acetate penetration and lower yields"

Just wanted to ask what was the percentage it lowered by? And how was this established?

I admit I haven't conducted any controlled test but i have never had issues with lower yields from drier material, my extractions seem to be fairly consistent.

I just want to make sure I haven't been cheating my self out of extra crystals.:surprised
 
_Trip_ said:
Hey Loveall just checked out the updated Tek,

One question (I must of missed something), the tek says:

"if the paste is too dry it will block ethyl acetate penetration and lower yields"

Just wanted to ask what was the percentage it lowered by? And how was this established?

I admit I haven't conducted any controlled test but i have never had issues with lower yields from drier material, my extractions seem to be fairly consistent.

I just want to make sure I haven't been cheating my self out of extra crystals.:surprised
Click to expand...

Was done with a "min water" test where water was added slowly until the paste transitioned from clumpy to smooth (~222ml instead of the usual 300ml). Results reported here. Needed more pulls to get the mescaline out.

It's always good to do an extra set of pulls into a second jar at least one time. Make sure the technique on the first set of pulls is good and nothing substantial (<10%) comes through with the extra effort.

I'm adding a reference in the TEK to the min paste result.
 
HLP, yep, i look as it as salvage, if I can recover anything extra from the crappy product, and it doesn’t hurt the quality of the overall run, I’m good. I have a 5g powder run with some crap crystallizing right now, might be the best way to go, other than trying to clean & recrystallize with other solvents.
 
Thanks, the standard + dissolved crap runs are not done yet, but I expect them to show 15-20% recovery of starting wt (on top of yield from cactus powder), with roughly same apparent quality as a standard run. Not much yield, but worth the effort; and we will now have a stake in the ground for use in comparing other recovery methods.



Btw, great job on the wiki. Keep up the good work!
 
Thanks Cheelin.

I did a second set of pulls on the standard TEK using 100g of powder. Results:

- First quart jar (standard): 1.34g of monomescaline citrate
- Second quart jar: 0.11g of monomescaline citrate

That's a +8% boost. Not worth my time and effort I think, even though the combine yield is a record 1.45% (0.9% mescaline HC equivalent). I'm happy at 1.34% without having to double the pulling for that last bit of mescaline.

What this tells me is that the first set of pulls are effective and sufficient to first order (<10% loss if stopping after the first set of pulls).

I no longer rinse the jar walls with water. I've just started to resuse them. The minimal xtals that stay in them act as seed xtals for the next batch. This is lazy Tek approved since there is less jar cleaning (simply reuse).

I recommend that everyone do this check at least once to verify their pulls are efficiency. Getting >10% in the second jar means the initial paste or pulls technique needs to be improved (wetter/looser paste, more paste mixing, more ethyl acetate mixing, more ethyl acetate draining between pulls, etc).
 
Good info Loveall. Yep, for me, 10% is not worth the time or solvent to do additional pulls, I also agree on doing the check “at least once”. I’d say, generally, do it the first time you run a different material; then you can calculate your % yield, and compare future runs of same material to identify outliers.

Good idea about just letting the jar wall crystals build up, then eventually washing them when the yield justifies the time & effort. For test runs, where I want the results to be more precise, i’ll still wash & evap.

You seem to have the lazy gene, too.
 
Agreed Cheelin.

In other lazyness efforts, I tried reusing ethyl acetate without a carbonate water wash. Straight after xtalization (2.5g in quart jar) into the new factus paste.

pH paper went from acidic to basic, so it seems the lime in the paste did it's job neutralizing the solvent, allowing mescaline to move into then extract. However, the extract is super cloudy (see image). I imagine this is simply calcium citrate in suspension, possibly not absorbed by the paste since the water solubility of that salt is poor.

I'll give the calcium citrate time to settle and then decant/filter. Citric acid mescaline xtalization will follow, see if the mescaline came through (it should 🤞).
 

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Good stuff. I’m working out my strategery for testing reused solvent, this will be part of it. I suspect that results with unwashed used solvent will depend on how much citrate was used for salting.



Happy New Year, All!
 
Cheelin said:
Good stuff. I’m working out my strategery for testing reused solvent, this will be part of it. I suspect that results with unwashed used solvent will depend on how much citrate was used for salting.



Happy New Year, All!
Click to expand...
Yep, salt with too much excess citric and the lime in the paste could be overwhelmed. I would expect even more cloudiness upon reuse also.

Happy new year 🙂
 
Welcome to a fresh start, aka 2022!

Had started a post here about testing reused solvent, but discovered that i needed to specify washing method better than it is currently described in the tek. So, because of the delay, i’m moving the info to more current post.
 
Loveall, when you mix the used/unwashed EA with the 69ron paste, wouldn't this potentially cause some proportion of the freebase mescaline to salt out of solution?

Do you think that the citric acid in the used EA will be chemically attracted to the lime and get neutralized before it has a chance to interact with the freebase mescaline?

Lastly, how much excess lime is in the 69ron paste? Are we using way more than we need, sufficiently so to neutralize all the citric acid in used/unwashed EA?

Cheelin, sorry man I wanted to also compare the fresh EA vs used EA vs cold used EA as well. But EA is somewhat inconvenient for me to obtain because I have to buy it over the internet and I have made so many purchases already that I've decided to hold off for time time being.

So my next experiment will just be to simply reuse the same room temperature EA 10x or until I see a significant drop in yields.
 
So HLP, not sure what you mean.

The first experiment will be fresh EA vs washed EA that is then chilled to freeze the water wash vs untreated used EA.

The second experiment will use EA from each of the optional treatments vs fresh EA, and will be run over and over again in their respective treatments. So, in the case of the chilled paste & chilled EA treatment: the first run will use solvent that was from a run that the paste and fresh solvent were both chilled (as described in that experiment) before being pulled. This solvent will be washed & chilled to neutralize the acid, then chilled to pull chilled paste (1st reuse), this process will be repeated 2 more times using the same solvent and new, but chilled paste. Fresh EA with std paste, used EA with std paste, used EA with boiled water std paste, used EA with microwaved paste, and chilled used EA with microwaved & chilled paste will also be run.

Are you thinking of something different? If so, what? Are you saying, take used solvent from a std run, don’t wash it, but chill it to freeze any water in the solvent, decant off of any ice that forms, then run it?
 
No no, I just mean I would like to join you in your experiment, but as I am out of fresh EA and I don't want to order anymore online, I will only be able to do a subset of your experiment.

I will wash and freeze my EA and reuse over and over again and report the yield each time to identify when it becomes an issue. I will not be able to compare cold ea vs room temp ea reuse, or microwaved vs non-microwaved reuse, for example.

I think those are important though. I'm very eager to see your results. Cold EA and microwaved results in a very different color, which may or may not be important to reusing EA.

It would be really great if the standard tek could be simply reused for 10+ times without a decrease in yield.
 
highlightprotein said:
Loveall, when you mix the used/unwashed EA with the 69ron paste, wouldn't this potentially cause some proportion of the freebase mescaline to salt out of solution?

Do you think that the citric acid in the used EA will be chemically attracted to the lime and get neutralized before it has a chance to interact with the freebase mescaline?

Lastly, how much excess lime is in the 69ron paste? Are we using way more than we need, sufficiently so to neutralize all the citric acid in used/unwashed EA?
Click to expand...

The mescaline shouldn't salt out at equilibrium because reused citric is neutralized and the environment is alkaline at equilibrium.

There may be a brief moment when mescaline citrate could form before equilibrium, but that would eventually freebase as it interacts with the lime in the paste towards equilibrium. Regardless of the path, (direct citric acid to calcium citrate, or indirect citric acid and freebase, to mescaline citrate, to calcium citrate and freebase again), the citric acid is eventually neutralized as calcium citrate. The solvent pH was confirmed with paper strips, reused untreated EA went from acidic to alkaline as the mescaline moved into the solvent. In later pulls, when the mescaline is exhausted it just went from acidic to neutral.

69ron has 25g of lime (minus whatever is used to raise the pH, which should only be a few grams I imagine). I think that in theory that amount of excess can neutralize ~40g of citric acid, and I only had ~1.9g in my reused solvent (from the initial 2.5g minus ~ 600mg that formed a salt with freebase mescaline in the first extraction). So there is plenty of lime to neutralize EA. However, the more citric is used (e.g. 15g) the more messy it could be because of all the calcium citrate forming.

It's taking a loooong time for the calcium citrate to crash in the untreated reused EA. It is crashing and forming a while layer at the bottom of the extract, but at this rate it is going to take several days. I don't recommend this. I think a washing soda water wash to remove the excess citric acid in used EA is the way to go. I am going to avoid the calcium citrate in the future.
 
Oh, ok HLP, Got it. I may be the only person, at this point, with enough solvent from these various treatments to even get up to 4 uses out of all of them. Should be good enough to demonstrate what the effects are.

We’ll know pretty soon how good reuse of the solvent from standard paste works.
 
There may be a nice lazy way to reuse EA after all 🤞

Motivated by lazyness, I added washing soda powder straight to some used EA (no water). Nothing seemed to happen, but them I started seeing tiny bubbles. I shook and relieving pressure resulted in a hiss.

The neutralization is a lot slower than with a water layer, but it is happening. Eventually after a bunch of waiting and shaking the pH paper came out neutral and the hissing stopped. Shaking makes things go by faster.

The neutralized EA is a bit cloudy but not too bad. Gonna let it settle and see how it looks tomorrow.

If this works, we can skip the water separation. Simply decant off/filter the neutralized EA from the washing soda/sodium citrate solids.

I'll be testing this further and report back. Note that this process would also dry the EA, but I don't think that matters since the paste has a lot more water (overwhelming any potential effects from the EA carrying a bit of water I believe).
 
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