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Ethyl acetate approach [CIELO] Options
 
Cheelin
#701 Posted : 12/29/2021 1:07:48 AM

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Yep, I had a place-saver post that I deleted. I guess the app treats it differently depending on logged in/out.

I think it would be useful to note pH levels of reused solvent, combined pulls, and salted solution. We may find that this is relevant along with, or perhaps more so than, specified amounts of some ingredients.




Previously I tried to run some of the crappy product from early runs of this tek, by itself (no cactus powder), using a modified version of this tek. The result was a mess, and the yield was nearly unmeasurable. Significant work will be needed to develop an efficient and effective crap rehab tek of this sort.

I. So I decided to sacrifice a 45g run in an attempt to rehab 2.0g of brown, somewhat crystalline crap.

I used the std tek, but before mixing the paste I took a mortar & pestle to the 2.0g of crap and powdered it as well as I could, then in 2 cycles, I mixed 10mL boiling water each with the powdered crap in a shot glass to dissolve it. I then mixed the lime with water, and then the powdered cactus, as usual. I added the crap & water mix into all of this, then started my 8 min stir & 10 min rest. Using crystal clear, previously neutralized (pH 6-7 ish), reused std pull solvent (moderately green at this point), I did the 6 pulls, and let the filtered combined pulls settle for an hour (pH 8-9ish). Filtered again, then settled another hour. Then filtered again, then settled another hour, The slight cloudiness from the pulls never changed. I then filtered again, added 2.25g of citric acid, stirred (pH 4-5ish), and let crystallize passively. After 24 hours the top 1/3 of the solution was crystal clear. I filtered the whole jar, and returned the EA to the crystallization jar, to continue crystallizing. The jar cleared and was filtered at 48 and 72 hours,; then hot water washed into a glass baking dish, evaporated, and scraped.

The 45g of this cactus, when fully crystallized should produce ~0.5g. 24 hr total yield 0.8g, 48 hr incremental yield 0.08g, 72 hr incremental yield 0.003g, jar wash residue 0.042g, So, total yield = 0.925g, with expected cactus yield ~0.495g, the crap recovery was 0.430g. Since initial crap was 2.0g, percent recovery was 21.5%.


II. Did a run with 5g of same cactus powder and 1g crap (crap was from a different material, from same vendor, as the crap in I.), using standard wet mix paste.
Pickling Lime = 1.25g
Distilled Water = 15mL

Powdered crap w mortar & pestle, then mixed in shotglass w 2mL boiled water til dissolved, mixed again with another 2mL boiling water. Dumped this in bowl with lime, mixed til milky, added cactus powder, mixed 8 mins, rested 10 mins. Put in wide-mouth 1-pint jar, with wire screen from french press as cover. Did 6 pulls; started with 2 pulls using 10ml, neutralized (6-7 ish pH) std paste reused solvent. Too little solvent for the container sizes I have in my kitchen, so used 20mL/pull for pulls 3 through 6 (pH 8-ish). (Next time, will try dissolving crap with boiling water, then let it cool to room temp, before mixing paste; paste got snot-like for all pulls, reminding me of previous boiled water run where paste remained sticky through all 6 runs). Let combined pulls settle 1 hr, the tiniest amount of cloudiness did not settle out. Then passively salted with 0.5g citric acid (pH 5 ish). The 5g of cactus, should produce ~0.055g. 24hr total yield 0.136g, 48hr incremental yield 0.014g, 72hr incremental yield 0.0g, jar wash residue 0.046g. So, total yield = 0196, with expected cactus yield ~0.055g, the crap recovery was 0.141g. Since initial crap was 1.0g, percent recovery was 14.1%. Product looks and tastes like product from standard process.


III. Ran another version of II. (same cactus powder, same crap), this time the dissolved crap was cooled to ambient temp before mixing, and pulled 6 times with 20mLs/pull of Fresh solvent. The paste was still snotlike during the pulls, Fresh solvent pH = 5-6ish, combined pulls pH = 7ish, salted pH = 4-5ish. The 5g of cactus, should produce ~0.055g. 24hr total yield 0.144g, 48hr incremental yield 0.016g. 72hr incremental yield 0.003g, jar wash residue 0.030. So, total yield = 0193, with expected cactus yield ~0.055g, the crap recovery was 0.138g. Since initial crap was 1.0g, percent recovery was 13.8%. Product looks and tastes like product from standard process.


IV. Washed some crap with anhydrous acetone. Since I only needed a small amount, and dry acetone is pretty expensive, I picked up a quart of acetone at my local bigbox, ordered some epsom salts, and used the acetone drying approach discussed in https://www.dmt-nexus.me...aspx?g=posts&t=4571 . Once the acetone was “dry”, I mixed 1.354g of powdered crap in a full shotglass of acetone for ~5 minutes. After filtering and drying, the pinkish powder, which tasted nothing like any of the product from any of the other runs, yielded 0.248g or 18.3% of the original crap. I guess I could rewash this in acetone a couple more times, and/or water wash and evaporate in an attempt to improve the quality. But the yield is aleady so low, it’s not worth it to me to do the additional work.


Note: I do not have an expected yield % for the material used in the original extractions that produced the crappy product being discussed in this post. It was material that I was concerned would have a low mescaline content. As a result, it is possible that the recovered yields from theses runs is a high percentage of what was in the original cactus. If this is the case, the crap recovery would under-represent the possible recovery % when using this method.


Main Points:
1. Reprocessing small amounts of crappy product by incorporating crap into a standard run yields approximately 14-21% recovery in excess of normal yield, without detrimental affect on quality.

2. Use of Fresh or 1-use solvent had no significant effect on yield or quality.

3. Standard runs as small as 5 grams of cactus powder can provide consistent yield and quality results.

2. Reprocessing a small amount of crappy product, by itself, will require further development.

3. Reprocessing small amounts crappy product using “dry” acetone will require further development.
 

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Loveall
#702 Posted : 12/29/2021 11:15:51 AM

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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.
💚🌵💚 Mescaline CIELO TEK 💚🌵💚
💚🌳💚DMT salt e-juice HIELO TEK💚🌳💚
💚🍃💚 Salvinorin Chilled Acetone with IPA and Naphtha re-X TEK💚🍃💚
 
Cheelin
#703 Posted : 12/29/2021 1:06:22 PM

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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.
 
highlightprotein
#704 Posted : 12/30/2021 3:14:16 AM
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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.
 
_Trip_
#705 Posted : 12/30/2021 4:36:27 AM

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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
Disclaimer: All my posts are of total fiction.



 
Loveall
#706 Posted : 12/30/2021 1:37:06 PM

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_Trip_ wrote:
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


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.
💚🌵💚 Mescaline CIELO TEK 💚🌵💚
💚🌳💚DMT salt e-juice HIELO TEK💚🌳💚
💚🍃💚 Salvinorin Chilled Acetone with IPA and Naphtha re-X TEK💚🍃💚
 
Cheelin
#707 Posted : 12/30/2021 3:10:13 PM

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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.
 
Loveall
#708 Posted : 12/30/2021 7:45:57 PM

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Cheelin, I have added your goo recovery result to the FAQ section of the TEK. If you want to change the info there to clarify or correct go ahead. Thanks.
💚🌵💚 Mescaline CIELO TEK 💚🌵💚
💚🌳💚DMT salt e-juice HIELO TEK💚🌳💚
💚🍃💚 Salvinorin Chilled Acetone with IPA and Naphtha re-X TEK💚🍃💚
 
Cheelin
#709 Posted : 12/30/2021 8:09:08 PM

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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!
 
Loveall
#710 Posted : 12/31/2021 4:05:52 PM

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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).
💚🌵💚 Mescaline CIELO TEK 💚🌵💚
💚🌳💚DMT salt e-juice HIELO TEK💚🌳💚
💚🍃💚 Salvinorin Chilled Acetone with IPA and Naphtha re-X TEK💚🍃💚
 
Cheelin
#711 Posted : 12/31/2021 4:53:46 PM

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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.
 
Loveall
#712 Posted : 12/31/2021 5:25:50 PM

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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 🤞).
Loveall attached the following image(s):
IMG_20211231_121629242.jpg (3,619kb) downloaded 162 time(s).
💚🌵💚 Mescaline CIELO TEK 💚🌵💚
💚🌳💚DMT salt e-juice HIELO TEK💚🌳💚
💚🍃💚 Salvinorin Chilled Acetone with IPA and Naphtha re-X TEK💚🍃💚
 
Cheelin
#713 Posted : 12/31/2021 5:33:15 PM

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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!
 
Loveall
#714 Posted : 12/31/2021 6:11:54 PM

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Cheelin wrote:
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!

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 🙂
💚🌵💚 Mescaline CIELO TEK 💚🌵💚
💚🌳💚DMT salt e-juice HIELO TEK💚🌳💚
💚🍃💚 Salvinorin Chilled Acetone with IPA and Naphtha re-X TEK💚🍃💚
 
Cheelin
#715 Posted : 1/1/2022 5:30:06 PM

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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.
 
highlightprotein
#716 Posted : 1/1/2022 10:54:44 PM
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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.
 
Cheelin
#717 Posted : 1/2/2022 12:11:06 AM

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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?
 
highlightprotein
#718 Posted : 1/2/2022 12:45:57 AM
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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.
 
Loveall
#719 Posted : 1/2/2022 12:59:59 AM

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highlightprotein wrote:
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?


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.
💚🌵💚 Mescaline CIELO TEK 💚🌵💚
💚🌳💚DMT salt e-juice HIELO TEK💚🌳💚
💚🍃💚 Salvinorin Chilled Acetone with IPA and Naphtha re-X TEK💚🍃💚
 
Cheelin
#720 Posted : 1/2/2022 1:11:47 AM

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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.

 
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