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Ethyl acetate approach Options
 
Loveall
#261 Posted : 6/5/2021 5:04:12 PM

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As a test I did two room temp pulls from spent chilled CIELO catus.

Nothing significant came through after salting. Maybe 10mg? Also, the few xtals that form are a lot smaller and cling to the wall, as is usual for me with room temp pulls.

Conclusion is that the chilled pulls are doing their job and picking up almost all the available mescaline.

Next, I'm going to try reusing the ethyl acetate from the chilled pulls. It had less plant stuff, so I should be more reusable (?). I'm washing it with sodium carbonate water to neutralize it for reuse.
πŸ’šπŸŒ΅πŸ’š Mescaline CIELO TEK πŸ’šπŸŒ΅πŸ’š
πŸ’šπŸƒπŸ’š Salvinorin Chilled Acetone with IPA and Naphtha re-XπŸ’šπŸƒπŸ’š
 

Trippy glass for trippy people.
 
Loveall
#262 Posted : 6/6/2021 9:51:59 PM

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Update for ethyl acetate reuse:

It worked when testing with chilled solvent. Extract became darker and needles were smaller. Yields not affected. At least 1x reuse is ok πŸ™‚πŸ’š. I imagine it can be reused a few more times.

I did filter the reused chilled solvent to remove some ice xtals that formed (water from the wash I presume). Tek has been updated to include a reuse section with the details. Cheers.


πŸ’šπŸŒ΅πŸ’š Mescaline CIELO TEK πŸ’šπŸŒ΅πŸ’š
πŸ’šπŸƒπŸ’š Salvinorin Chilled Acetone with IPA and Naphtha re-XπŸ’šπŸƒπŸ’š
 
Loveall
#263 Posted : 6/7/2021 11:13:11 AM

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Update on the paste reaction time: 10 minutes yielded the same as 24h. Together with shroombee's result (24h yielded the same as 72h), we can conclude that 10 minutes is enough time to freebase the powdered cactus' mescaline.

Note that the chilled ethyl acetate pulls are quick (60s each).

Starting with cactus powder and chilled ethyl acetate in the freezer, getting to the crystallization step takes an a hour or less without rushing. Long needles can be collected the next day (or even late in the same day) after passive slow crystallization.

Enjoy πŸ™‚πŸŒ΅

πŸ’šπŸŒ΅πŸ’š Mescaline CIELO TEK πŸ’šπŸŒ΅πŸ’š
πŸ’šπŸƒπŸ’š Salvinorin Chilled Acetone with IPA and Naphtha re-XπŸ’šπŸƒπŸ’š
 
grollum
#264 Posted : 6/8/2021 7:54:57 PM

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Loveall wrote:
Update on the paste reaction time: 10 minutes yielded the same as 24h. Together with shroombee's result (24h yielded the same as 72h), we can conclude that 10 minutes is enough time to freebase the powdered cactus' mescaline.

Note that the chilled ethyl acetate pulls are quick (60s each).

Starting with cactus powder and chilled ethyl acetate in the freezer, getting to the crystallization step takes an a hour or less without rushing. Long needles can be collected the next day (or even late in the same day) after passive slow crystallization.

Enjoy πŸ™‚πŸŒ΅



That would really be a quick run. Awesome. Thanks for all the new discoveries you made!
The reuse section is awesome as well! How much sodium carbonate and water per gram of solvent would you suggest?
 
Loveall
#265 Posted : 6/8/2021 8:27:40 PM

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grollum wrote:
How much sodium carbonate and water per gram of solvent would you suggest?


Thanks, it's all a team effort πŸ™

Want to saturate the water, 35g per 100ml of water should work. I just add sodium carbonate by eye and then a little bit of water until I see a separate water layer with undissolved sodium carbonate. Some water seems to separate out by just adding NaCO2, but to really neutralize the solvent some extra water seems necessary. I could be wrong and a simplification may be possible here (add only washing soda, give time to neutralize, and decant?). CO2 bubbles are also an indication of neutralization, maybe that can be used instead of pH paper to simplify further.
πŸ’šπŸŒ΅πŸ’š Mescaline CIELO TEK πŸ’šπŸŒ΅πŸ’š
πŸ’šπŸƒπŸ’š Salvinorin Chilled Acetone with IPA and Naphtha re-XπŸ’šπŸƒπŸ’š
 
Loveall
#266 Posted : 6/9/2021 1:08:34 PM

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After some tinkering and repeats, I have updated our TEK one more time. Focus was on simplifying the steps and making the process more robust to allow for some user error.

Updates:

* Use ice water to make the paste and keep things colder
* No longer measure added solvent during the pulls, simply cover the paste with each pull and repeat until extract fills 80% of a quart jar (usually 6 pulls total).
* Crystalize in jar instead of shallow baking dish (crystals from chilled pulls don't cling to the jar walls)
* Catch and wash crystals in a filter (I prefer this to decanting and find it more straightforward for loose crystals). It takes only seconds to get the mat of crystals off the filter and they are easy to handle.

Bellow is the latest crop of crystals growing in ethyl acetate with the updates (ended as a healthy 1.1% yield of white dry crystals). Cheers.
Loveall attached the following image(s):
IMG_20210609_064813073.jpg (1,108kb) downloaded 187 time(s).
πŸ’šπŸŒ΅πŸ’š Mescaline CIELO TEK πŸ’šπŸŒ΅πŸ’š
πŸ’šπŸƒπŸ’š Salvinorin Chilled Acetone with IPA and Naphtha re-XπŸ’šπŸƒπŸ’š
 
Loveall
#267 Posted : 6/10/2021 2:25:27 PM

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Minor update: Did a room temp pull on the cacti spent by the Tek. Got a minimal amount of crystals. They were tiny the small amount only weighed 4mg.

So not worth it.

I am noticing more green using ice cold water. I think the chlorophyll is broken down less? Perhaps something to look into. Does not seem to affect crystal size.

Maybe im the future will let the paste sit for a while to hydrolyze chlorophyll and get less green. Then cool it down in the fridge and start the chilled extract. Hydrolyzed chlorophyll should be more polar and less soluble in ethyl acetate, which could make the solvent reusable more times...

Anyway, pretty happy with the TEK as is for now.

πŸ’šπŸŒ΅πŸ’š Mescaline CIELO TEK πŸ’šπŸŒ΅πŸ’š
πŸ’šπŸƒπŸ’š Salvinorin Chilled Acetone with IPA and Naphtha re-XπŸ’šπŸƒπŸ’š
 
Tony6Strings
#268 Posted : 6/10/2021 2:46:00 PM

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Loveall, I saw the writeup for this on the wiki. This is perfect and exactly what I was after, IE, mesc crystals without using xylene and without having to work with a large amount of NaOH basified material. That green ethyl acetate in the jar is freaking beautiful man. Cannot wait to give this a go.
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Loveall
#269 Posted : 6/11/2021 1:15:43 AM

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Thanks Tony6Strings, best of luck with your extraction.


I have another update. I tested washing soda to make the paste (instead of lime). It works too, but is different.

- Mixed 300g of water and 100g of sodium carbonate (~saturated solution).
- Mixed in 100g of cacti. At first it was very liquidity, then after a few minutes of mixing it congealed.
- Quick cold pulls were not able to grab all the mescaline. I would guess this was because the cactus is congealed into a compact blob making it harder to access the mescaline
- Soaking the blob in ethyl acetate for a few hours was effective at pulling mescaline πŸ™‚
- Benefit is that the blob is super easy to decant. Downside is that pulls take a long time and the extract is darker vs. the quick cold pulls with lime

Could be an option if anyone wants to avoid the french press and values super easy decanting. Solvent reuse may be more limited because a lot of the plant stuff is pulled with the long soak at room temp. The xtals are smaller and stickier which I don't care for. Maybe a long fridge soak would be better for the washing soda approach.

Anyhow, could be an interesting path to some. I prefer lime and the quick cold pulls on the "sandy" cactus paste - but at some point it's a personal choice. With lime the french press helps to hold the sand back, so if a french press is not available I image washing soda has a big plus. Also, one could defat to avoid the darker greens and grow longer needless in a cleaner room temperature extract (?).

Edit: The whole point of the test was to hydrolyze chlorophyll and see if a less green extract would result. That did not happen.
πŸ’šπŸŒ΅πŸ’š Mescaline CIELO TEK πŸ’šπŸŒ΅πŸ’š
πŸ’šπŸƒπŸ’š Salvinorin Chilled Acetone with IPA and Naphtha re-XπŸ’šπŸƒπŸ’š
 
Loveall
#270 Posted : 6/11/2021 10:26:58 AM

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One small improvement I want to pursue is less color in the extract. Want to see if that gives larger crystals and makes the solvent reusable more times. It would also be more robust if there are cacti species out there that send more stuff into the ethyl acetate that could interfere with crystallization.

One of the plant components that gets into ethyl acetate is chlorophyll. However, it can be hydrolyzed to more polar products that are more soluble in water to try keep it out of the solvent.

So here are a couple of ideas:

- Let the paste react longer to hydrolyze chlorophyll over time. Shroombee, did you ever notice a color change in the extract for different paste reaction times?
- Use 25g of NaOH instead of Ca(OH)2. This will hydrolyze chlorophyll over time (see attached paper). Then add 40g of CaCl2, this will buffer the pH to be more like Ca(OH)2 and more stable for ethyl acetate. Cool this paste in the fridge and extract with chilled solvent, this may have very few off colors (?).

Will be trying this in the future.
πŸ’šπŸŒ΅πŸ’š Mescaline CIELO TEK πŸ’šπŸŒ΅πŸ’š
πŸ’šπŸƒπŸ’š Salvinorin Chilled Acetone with IPA and Naphtha re-XπŸ’šπŸƒπŸ’š
 
shroombee
#271 Posted : 6/11/2021 8:33:29 PM

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Loveall wrote:
Shroombee, did you ever notice a color change in the extract for different paste reaction times?

Nothing obvious, but I wasn't paying close attention to notice subtle changes in the extract color. It's generally a beautiful emerald green.

How about a simple A/B comparison experiment:

A) Base a small amount of cactus for 72 hours;
B) 71 hours after starting (A), base another small batch of cactus for 1 hour (so it is finished basing at the same time as (A);

Do some pulls on (A) and (B), put the extracts into test tubes, and compare the colors. The pulls and comparisons should be done within a short window so we minimize any color changes that might occur over time.
 
downwardsfromzero
#272 Posted : 6/15/2021 3:35:59 PM

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Loveall wrote:
One small improvement I want to pursue is less color in the extract. Want to see if that gives larger crystals and makes the solvent reusable more times. It would also be more robust if there are cacti species out there that send more stuff into the ethyl acetate that could interfere with crystallization.

One of the plant components that gets into ethyl acetate is chlorophyll. However, it can be hydrolyzed to more polar products that are more soluble in water to try keep it out of the solvent.

So here are a couple of ideas:

- Let the paste react longer to hydrolyze chlorophyll over time. Shroombee, did you ever notice a color change in the extract for different paste reaction times?
- Use 25g of NaOH instead of Ca(OH)2. This will hydrolyze chlorophyll over time (see attached paper). Then add 40g of CaCl2, this will buffer the pH to be more like Ca(OH)2 and more stable for ethyl acetate. Cool this paste in the fridge and extract with chilled solvent, this may have very few off colors (?).

Will be trying this in the future.

Good idea. The NaOH/CaCl2 approach looks promising to me. I did a quick calculation or two and even 35g of CaCl2 would be an excess for 25g of NaOH, especially considering some will get used up freebasing the mescaline as well as reacting with saponifiable substances. Of course, most CaCl2 won't be fully anhydrous and much of the industrial grade stuff is partially hydrolysed so 40g is perhaps a sensible safety margin to ensure that all the NaOH gets converted and none remains to aggressively hydrolyse the EA. Maybe titrate a sample of the CaCl2 with NaOH first? [Thinking as I type here, clearly Smile]
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antichode
#273 Posted : 6/16/2021 7:54:25 AM

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Hey guys. I’ve been glued to this thread for months now. Really stoked with all the work you have done.

Have you guys scaled this up at all? I noticed with the classic calcium hydroxide teks that they were not super efficient once you got up above 300g or so.

I guess the larger you go the more mechanical challenges are ever present. Filtering and separating the reaction comes to mind
 
Loveall
#274 Posted : 6/16/2021 11:32:45 AM

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antichode wrote:
Hey guys. I’ve been glued to this thread for months now. Really stoked with all the work you have done.

Have you guys scaled this up at all? I noticed with the classic calcium hydroxide teks that they were not super efficient once you got up above 300g or so.

I guess the larger you go the more mechanical challenges are ever present. Filtering and separating the reaction comes to mind


Thanks. I wouldn't expect any filtering issues, everything is easy to filter. Separating the paste and ethyl acetate would be harder if the french press is not large enough. Making the paste would require some elbow grease. Perhaps doing two batches would work well, the process is simple/fast anyway.
πŸ’šπŸŒ΅πŸ’š Mescaline CIELO TEK πŸ’šπŸŒ΅πŸ’š
πŸ’šπŸƒπŸ’š Salvinorin Chilled Acetone with IPA and Naphtha re-XπŸ’šπŸƒπŸ’š
 
Woolmer
#275 Posted : 6/16/2021 11:39:30 AM

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I'm amazed at how simple yet well yielding this tek is Loveall! Thank you Smile. All the other teks were always a bit difficult and often resulted in a more crude yield.

One question I have, I presume the dried cactus that you were using is only the green flesh? Has this been done with the addition of the white flesh underneath (dried of course) and does/would this affect extraction in terms of gunking things up and such?
 
Loveall
#276 Posted : 6/16/2021 11:49:38 AM

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Woolmer wrote:
I'm amazed at how simple yet well yielding this tek is Loveall! Thank you Smile. All the other teks were always a bit difficult and often resulted in a more crude yield.

One question I have, I presume the dried cactus that you were using is only the green flesh? Has this been done with the addition of the white flesh underneath (dried of course) and does/would this affect extraction in terms of gunking things up and such?


Yes, most tests were with the green part. The whole plant was tested too and it still worked, but more citric acid was needed and the xtals were not as clean (slight stickiness). However, that was before we found out that freezing ethyl acetate is better at keeping out plant stuff: using chilled acetate could be even more beneficial on the whole plant extraction.

Have you tried this extraction yet? Cheers.
πŸ’šπŸŒ΅πŸ’š Mescaline CIELO TEK πŸ’šπŸŒ΅πŸ’š
πŸ’šπŸƒπŸ’š Salvinorin Chilled Acetone with IPA and Naphtha re-XπŸ’šπŸƒπŸ’š
 
Loveall
#277 Posted : 6/16/2021 3:23:22 PM

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Update on the sodium carbonate paste that congealed: 0.6% yield along with a very slight tan color (usually this material yields 1% of white crystals with the standard TEK). It does not work as well as lime.

Update on NaOH followed by CaCl2 paste: This is very interesting so far πŸ™‚. Paste congealed with NaOH (25g), and the paste color changed to dark green (indication that chlorophyll reacted I'm guessing). After letting it react overnight, it was still congealed even after upping NaOH to 45g (nothing seem to change with the extra 20g of NaOH). Adding CaCl2 (80g) had a dramatic effect, paste became sandy 🀩. Extraction with chilled ethyl acetate resulted in a light yellow extract (see first picture comparing different extracts) πŸ‘. Added a small amount of citric acid (~1.5mg/g) since the solvent seems cleaner, crystallization should be easier (can always add more later if needed). Clouds currently forming (second picture), will report yield in a day or so. If it works, this process could be more robust to different cacti sources (since less plant stuff is pulled) and make reusing the solvent more straightforward 🀞.

PS: Oddly the picture came out a little green. However it looks yellow to the eye. It is the most colorless extract I've seen.
Loveall attached the following image(s):
Screenshot_20210616-110817-368.png (1,170kb) downloaded 21 time(s).
IMG_20210616_102026696.jpg (752kb) downloaded 21 time(s).
πŸ’šπŸŒ΅πŸ’š Mescaline CIELO TEK πŸ’šπŸŒ΅πŸ’š
πŸ’šπŸƒπŸ’š Salvinorin Chilled Acetone with IPA and Naphtha re-XπŸ’šπŸƒπŸ’š
 
Woolmer
#278 Posted : 6/16/2021 5:02:05 PM

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Loveall wrote:
Have you tried this extraction yet? Cheers.

I have not. No cacti right now to sacrifice but should be getting a few cuts in the next weeks. Definitely going to give this a go and will report back. One issue with cactus is that it was always so hard for me to figure out dosage, even with a crude extraction.

Closely following this thread for any updates!
 
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