TEK Ethyl acetate approach [CIELO]

[merkin]

Congratulations - that's a great yield!

Thanks Pretty impressed with that old powder!

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.

I tend to think you’re right shroombee. Loveall I hope you’re not giving any of my initial issues too much weight here? In hindsight I would say the lack of yield and difficulties crystallising were all my own ineptitude. Especially the cloudy limey solvent. Things turned around for me when I copied shroombees limewater paste prep method and worked slowly and more carefully with the room temp solvent. I think that was the main reason I was having problems. Trust your instinct here rather. The improvement I got was so huge it was like a whole different tek.

 

[Loveall]

Here are the details of what I observed with the diffusion method and chlorophyll:

- When chlorophyll is minimally/not present sub mg/g formed crystals. With chlorophyll started seeing them at ~2mg/g +
- With deep chlorophyll color I've never been able to grow long crystals. Their size is inverse to the intensity of the green color. Longest crystals grow with light chlorophyll color (chilled pulls) or tan color (microwave chlorophyll saponification).

It could be something else other than chlorophyll and correlated with it. For example, whole plant was also more difficult to xtalize but was not greener.

As long as everyone's clouds crash, I don't care. Reason to push for less chlorophyll and less plant matter was to help anyone with starting material that could have more crystallization interfering stuff.

Secondary factor is solvent readability.

 

[MtHighlands]

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!

Merkin, what kind of cactus did you start with?

 

[shroombee]

Here are the details of what I observed with the diffusion method and chlorophyll:

- When chlorophyll is minimally/not present sub mg/g formed crystals. With chlorophyll started seeing them at ~2mg/g +
- With deep chlorophyll color I've never been able to grow long crystals. Their size is inverse to the intensity of the green color. Longest crystals grow with light chlorophyll color (chilled pulls) or tan color (microwave chlorophyll saponification).

It could be something else other than chlorophyll and correlated with it. For example, whole plant was also more difficult to xtalize but was not greener.

Okay this is good to know. For slow diffusion to grow large xtals, do you recommend less citric? Or can I start with 5 mg/g?

BTW, for everyone else running this tek, the 3 minute room temperature pull process is basically our previously published tek before starting cold solvent experiments. So what's happened over the past week is we realize that keeping it simple with room temperature pulls might be more reliable for most people. And the milky water basing process was inspired by Loveall telling me to "make milky water". Although these processes may casually be referred to as "shroombee's method", these are more accurately called the team's method and the success we're having is definitely a group effort.

We continue to learn and refine as we get feedback. It's great to see that folks are having success! :thumb_up:

 

[merkin]

Wow!
Merkin, what kind of cactus did you start with?

Hi, I have no idea really. It was bought off internet in 2011 directly from Peru and labelled “Icaro” but listed as “San Pedro” dried powdered. It is now a brown powder, was greener at first due to age deterioration, which fortunately seems to have had no effect on mesc content. When this is finished I will use some of my own. Have about 6m of bridgesii and Pedro that were broken by a falling tree quietly sitting wrapped in newspaper waiting their turn. Not sure what their yield would be. But this tek is so great because you can repeat it often and make up in iterations what may be lacking in yield. I extracted about 9g “Sanchez” HCl when I got it but that method was so laborious I gave up and left the rest of the powder in the garage, only to bring it out two weeks ago when I read this thread and got totally inspired!

 

[Loveall]

Okay this is good to know. For slow diffusion to grow large xtals, do you recommend less citric? Or can I start with 5 mg/g?

For slow diffusion to make large crystals from chilled extract with my particular cactus material I drop in ~2mg/g of citric acid. If I use less, then adding more citric crashes a tiny bit more crystals. If I use more the xtals don't seem to grow as big. I'm not very certain as these are rough observations, but they have repeated a couple times.


Side note: One thing we mentioned a while ago was to try other organic acids. I do want to try at least one more: Malic acid. Room temperature solubility in ethyl acetate is ~40mg/g I believe (see attached paper) so the same process could work substituting citric acid for malic acid. Citric acid works great, but the curiosity here is to try to get what some believe to be a more natural salt form (?). Mescaline Malate would be same strength by mass as citrate or sulfate dihydrate, and 90% as strong as HCl.

 

[shroombee]

Side note: One thing we mentioned a while ago was to try other organic acids. I do want to try at least one more: Malic acid. Room temperature solubility in ethyl acetate is ~40mg/g I believe (see attached paper) so the same process could work substituting citric acid for malic acid. Citric acid works great, but the curiosity here is to try to get what some believe to be a more natural salt form (?). Mescaline Malate would be same strength by mass as citrate or sulfate dihydrate, and 90% as strong as HCl.

I tried malic acid and reported on it here. It was a dud. And I did try to add a lot more malic acid over time, put it in the frig, etc. Perhaps you'll have better luck.

 

[Loveall]

Side note: One thing we mentioned a while ago was to try other organic acids. I do want to try at least one more: Malic acid. Room temperature solubility in ethyl acetate is ~40mg/g I believe (see attached paper) so the same process could work substituting citric acid for malic acid. Citric acid works great, but the curiosity here is to try to get what some believe to be a more natural salt form (?). Mescaline Malate would be same strength by mass as citrate or sulfate dihydrate, and 90% as strong as HCl.

I tried malic acid and reported on it here. It was a dud. And I did try to add a lot more malic acid over time, put it in the frig, etc. Perhaps you'll have better luck.

Yes, I remember reading that now and the productive follow up discussion. I had forgotten about the malic acid info after all this time since we went on to focus on citric acid - thanks for the reminder. I'll skip malic then. I have other stuff to try. I'll give fumaric a shot, since many nexians may have that in the pantry already. TEK has been updated (development section).

 

[someblackguy]

In someblackguy's original work, the lime paste was dried completely and actives where indeed extracted with ethyl acetate based on his bioassay. Ethyl acetate was evaporated (not salted) leaving an oil behind. So drying the paste should work (?). His result was a green extract, so maybe microwaving to partially dry + extracting at 0F is more robust because the extract is near colorless.

Reviewing someblackguy's thread, he doesn't say how long he pulled with ethyl acetate. I'm guessing it was a lot longer than the pull times we're currently working with.

Short pulls from dried paste might be more colorless?

I believe the paste was pulled for 12 hours—which is overkill. At the time I believed that longer pulls might make up for fewer (not the case) and I tended to leave things sitting overnight.

(Gotta say—this thread is a damn interesting read. Great work/write up.)

 

[Loveall]

Thanks someblackguy. Not sure if you saw, but in the TEK, a particular emoji is used in your honor...

 

[MtHighlands]

Hi guys. A few questions as I prepare for another run.

- Any downsides to the Microwave method discovered so far? Any risk of microwaving too much?

- Since there was a focus on chilled pulls before, do you think there would be an advantage to allowing the paste to cool in the fridge after
Microwave?

- The Tek suggested using just enough EA to cover the paste. Shroombee was using around 1Q or so for a 50g of cactus. Seems like quite lot of EA compared to just covering. Thoughts?

 

[shroombee]

The Tek suggested using just enough EA to cover the paste. Shroombee was using around 1Q or so for a 50g of cactus. Seems like quite lot of EA compared to just covering. Thoughts?

I’m using about 650 grams ethyl acetate per 50 grams cactus. 650 grams EA is about 722 ml (about 3/4 of a quart). A quart is 946 ml. I’ll probably try using less solvent in the future. I’ve also been saving the used solvent, so I should try washing and reusing.

 

[Loveall]

The TEK says to cover the paste, pull, and repeat until you fill up a quart jar. Expect 5 to 6 repeats. From all that you can also infer that it is ~ 150 to 180ml each pull.

"Cover paste with ethyl acetate, mix well for 60s, allow to rest for 120s and decant into quart jar through a coffee filter. Do not squeeze with the french press, its purpose is to only hold back the paste from falling into the filter and squeezing can push unwanted material into the extract. Repeat until quart jar is full (~5-6x)."

Edit: There is a risk to over boil while microwaving after the first stir. Everything should be ok if keeping a close eye. However, if you don't care about reusing the solvent or care about xtal size, not microwaving is fine.

 

[shroombee]

Thanks someblackguy. Not sure if you saw, but in the TEK, a particular emoji is used in your honor...

Those emojis display correctly on my Mac. My Windows 7 machine displays random characters. I don't know whether Windows 10 displays them correctly?

 

[grollum]

"Cover paste with ethyl acetate, mix well for 60s, allow to rest for 120s and decant into quart jar through a coffee filter. Do not squeeze with the french press, its purpose is to only hold back the paste from falling into the filter and squeezing can push unwanted material into the extract. Repeat until quart jar is full (~5-6x)."

While reading this sentence I am thinking that it could be misunderstood.
For example when putting the paste like a lump of clay into a big round bowl and then fill with EA that could result in way to much EA. Maybe the text could suggest a more narrow jar and give advise to fill the jars floor so that it fills all the volume to the jar walls?

Maybe like this? :
"Make sure the paste is evenly stretched over the bottom of the jar without any bigger holes of air."

Do you know what I mean? Maybe I am overthinking...

 

[grollum]

Hi guys. A few questions as I prepare for another run.

- The Tek suggested using just enough EA to cover the paste. Shroombee was using around 1Q or so for a 50g of cactus. Seems like quite lot of EA compared to just covering. Thoughts?

It would be 50g powder + 150g water + 12.5g lime and it is used for several pulls.

I had almost exactly 1000ml EA for 100g cacti which was perfect for 5 pulls.

 

[someblackguy]

Thanks someblackguy. Not sure if you saw, but in the TEK, a particular emoji is used in your honor...

"Extract " :lol: ...in a nutshell :thumb_up:

Excellent tek. Thanks for the work (and the mention).

 

[MtHighlands]

Does this image look similar to what you have collected? Slight off-white to tan (some white) colors.

Collected 357mg from Attempt#1 jar. Washed with warm EA. That was from 65g Pach powder. So 0.55%

The weird thing is I didn’t get much but dust on attempt #2.

After collecting I bumped both jars up to 20mg/g citric acid, I’ll wait a little while to see if anything magical happens.

To summarize two different approaches:

Attempt1
- 65g Cactus powder
- low base time (3min)
- freezer chilled EA
- short 30s pulls
- small amount of EA (~350 g collected)
- crystallized for 5 days
- yield so far 357mg

Attempt2
- 65g Cactus powders (same mix from #1)
- long base time (15min)
- room temp ea
- longer pulls (30s stir, 2:30m rest)
- 700-800g EA collected and split into two jars
- no yield

 

[Loveall]

That looks right. You can dissolve in water and slowly evaporate, see if you get long small needles.

Second jar should have the goods too, may be a little harder to xtalize.

There is no chance you switched the jar labeling, right?

Yield seems high for PC. Your cactus picture sure looks PC-like, so I am curious about this.

 

[MtHighlands]

That looks right. You can dissolve in water and slowly evaporate, see if you get long small needles.

Second jar should have the goods too, may be a little harder to xtalize.

There is no chance you switched the jar labeling, right?

Yield seems high for PC. Your cactus picture sure looks PC-like, so I am curious about this.

No chance I confused the jars. Attempt1 was a single jar with 1/2 ea, Attempt2 was 2jars ~1/2Q ea. Both were split from a 130g of cactus powder.

It did take a while to crystallize so maybe the other one needs more time? Would a fridge help?

Any tips on how to crystallize after dissolving in water? I just dumped some in a pie plate but going to take a while to evap.

I was wondering for the water wash, would it be quicker to dissolve in Everclear, and evap?