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Ethyl acetate approach Options
 
Loveall
#81 Posted : 3/18/2021 12:30:18 PM

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shroombee, here is what I think (I could be wrong):

1) Many variables affect xtalization. Some are water, mescaline concentration, plant matter, temperature. We tried to control these (chemichal dry to remove water, microwave to remove the green in ethyl acetate, etc) but I don't think we need to do that anymore thanks to one reliable variable that is very easy to adjust: citric acid excess.

2) Looks like we have citric acid excess working for both of us. This is a KEY result I believe. For example, plant matter in ethyl acetate can be variable because of different cactus strains or even time as a lime base. As doubledog taught me, plant matter tends to hold mescaline in solution and stop xtalization. It is as if the plant wants to hold on to mescaline as much as possible (inside the plant that would help move mescaline around).

3) The ammount of citric acid is the key to keep this tek simple and working in a variable plant environment. This is why the ammount of citric acid has been increasing in the tek. We ave been finding that it works in more situations.

4) When sent for analysis, the clouds that we do get to crash leaving behind a clear solution are very clean mescaline citrate. I'm going to do this one more time with the "final" tek to verify.

5) Yields are good. I doubt that a significant ammount of mescaline stays in an acidic ethyl acetate solution. But yes, we should verify with A/B.

6) We cannot prescribe a fixed ammount to citric acid when salting. What if your cactus is 2% yielding? At 250mg of citric acid your pH would still be basic with no excess citric acid. On the other hand, someone with a 0.5% yielding cactus would have "acidic" ethyl acetate after adding that same ammount of 250mg and could see xtals already. Add to that, that the different cacti may have different plant stuff in ethyl acetate (e.g., the 2% cactus could also have a higher concentration of stuff that interferes with xtalization), and the ammount of citric acid needed to start xtalization can vary a lot.

7) Adding enough citric acid has been causing xtalization. So far every time for both of us. I have had clouds that did not precipitate until I added more citric acid, same as you. Once it starts to crash, you can get bigger xtals if it goes slow. If you have a lot of extra citric acid and shake it (or use a magnetic stirrer) it can go very fast and the xtals will be smaller. This is normal and expected and how I see mescaline citrate behave. There is also a borderline case where the clouds kind of settle but don't really and become a white wisp at the bottom. Sometimes part of this wisp sticks to the glass bottom. It can all be confusing and frustrating UNTIL more citric acid is added, then at some point, everything crashes beautifully.

8 ) Water may be good to have (which we organically have from the extract) to avoid the surprising effect where anhydrous citric acid does not go into solution. Also the mescaline citrate that crashes may be a hydrate. That's fine, all we do here is not chemically dry the solution.

Let's try to confirm this. If you go back to any cloudy solutions that you still have and add more citric acid, do they crash? If yes, I think we have a confirmed simple TEK.

The pH strip needs to be red throughout. The one on the right of post 71 was orange on the bottom. That was not enough citric acid I think. At the end of the day even the pH strip is not the final authority. If there is a lot of plant matter interfering with xtalization it may need to be redder than someone else's extraction. The key is: keep adding citric acid until the cloudiness is forced to crash. I'm temped to just say "add half a teaspoon" - that should force xtalization in most (all?) situations.

Are you familiar with Le Chatelier's principle? I think we are seeing an example here. The excess citric acid is overcoming all the other messy plant variables and crashing the clouds for us ๐Ÿ‘

You asked what I meant by "solution" and "salt". What I meant is that mescaline citrate (salt) does not dissolve (go into solution) during fresh (from can, little water) ethyl acetate washes. This is a good sign, but it does not prove that mescaline citrate won't dissolve into ethyl acetate + water. Actually I think the salt (mescaline citrate) may go into solution (dissolve), but if you add citric acid it will crash again.
๐Ÿ’š๐ŸŒต๐Ÿ’š Mescaline CIELO TEK ๐Ÿ’š๐ŸŒต๐Ÿ’š
๐Ÿ’š๐Ÿƒ๐Ÿ’š Salvinorin Chilled Acetone with IPA and Naphtha re-X TEK๐Ÿ’š๐Ÿƒ๐Ÿ’š
 

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doubledog
#82 Posted : 3/18/2021 1:16:26 PM

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I really like this thread, guys Smile

Loveall wrote:

For example, plant matter in ethyl acetate can be variable because of different cactus strains or even time as a lime base. As doubledog taught me, plant matter tends to hold mescaline in solution and stop xtalization.


It seems that ethyl acetate is not extracting lot of plant matter. This could be expected, it is less polar than ethanol, IPA or acetone.


Loveall wrote:

Yields are good. I doubt that a significant ammount of mescaline stays in an acidic ethyl acetate solution. But yes, we should verify with A/B.


What about just salting out like you would do with limo or toluene? I mean to wash with some water and evaporate the water?
 
Loveall
#83 Posted : 3/18/2021 1:44:47 PM

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doubledog wrote:
What about just salting out like you would do with limo or toluene? I mean to wash with some water and evaporate the water?


We can try that, it's a good idea. There should be excess citric acid coming through after evaporation. If everything dissolves into a small ammount of fresh (dry) ethyl acetate that means that it was all citric acid monohydrate and all the product crashed during the tek (I believe).

Also, I have update the experimental tek. I think we can ignore the pH strip if we simply add excess of citric acid (a lot). Also, if the pull is allowed to sit overnight it is very easy to decant, so I updated that. Threw in more citric acid too (it is kind of comical how it has been I creasing over time ๐Ÿ˜…). Essentially trying to make the tek as simple and robust as possible (we did call it "Leisurely" ).

Going to do a run with the tek as-is today and measure yields. May send for analysis if everything looks good and simply works (there have been several changes/simplifications since the first analysis).
๐Ÿ’š๐ŸŒต๐Ÿ’š Mescaline CIELO TEK ๐Ÿ’š๐ŸŒต๐Ÿ’š
๐Ÿ’š๐Ÿƒ๐Ÿ’š Salvinorin Chilled Acetone with IPA and Naphtha re-X TEK๐Ÿ’š๐Ÿƒ๐Ÿ’š
 
shroombee
#84 Posted : 3/18/2021 6:18:21 PM

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Loveall wrote:
1) Many variables affect xtalization. Some are water, mescaline concentration, plant matter, temperature. We tried to control these (chemichal dry to remove water, microwave to remove the green in ethyl acetate, etc) but I don't think we need to do that anymore thanks to one reliable variable that is very easy to adjust: citric acid excess.

Sounds convincing. In the lime/limo tek, we don't use citric acid at all because it doesn't evaporate and thus ends up in the final product. So HCl, sulphuric, etc are easier to use. If we can confirm this excess citric acid stays in the extract (or is easily washed away), then it sounds like a good way to keep things simple and reliable (one of my guiding principles).

Quote:
4) When sent for analysis, the clouds that we do get to crash leaving behind a clear solution are very clean mescaline citrate. I'm going to do this one more time with the "final" tek to verify.

I will also send a sample or two for analysis.

Quote:
Let's try to confirm this. If you go back to any cloudy solutions that you still have and add more citric acid, do they crash? If yes, I think we have a confirmed simple TEK.

I have several jars that I pulled out of the frig/freezer last night to let them reach room temperature. They don't all have clouds but I will try to crash them all.

Quote:
I'm temped to just say "add half a teaspoon" - that should force xtalization in most situations.

Perhaps we are arriving at a practical upper limit to give some guidance. A limit of citric acid in which we have confidence the excess will stay in the extract (or reliably washed away).

Quote:
Are you familiar with Le Chatelier's principal? I think we are seeing an example here. The excess citric acid is overcoming all the other messy plant variables for us and crashing the clouds for us

I will read up.

Quote:
You asked what I meant by "solution" and "salt". What I meant is that mescaline citrate (salt) does not dissolve (go into solution) during fresh (from can, little water) ethyl acetate washes.

Okay this is what I thought you meant.

Quote:
This is a good sign, but it does not prove that mescaline citrate won't dissolve into ethyl acetate + water. Actually I think the salt (mescaline citrate) may go into solution (dissolve), but if you add citric acid it will crash again.

So the idea would be to dissolve the end product (presumably contaminated with excess citric acid) in fresh ethyl acetate. Then crash out the mescaline with excess citric acid. Leaving us with mescaline citrate contaminated with citric acid. Huh? Confused

Quote:
Also, I have update the experimental tek. I think we can ignore the pH strip if we simply add excess of citric acid (a lot).

For those following the thread, the updated amount is 3.5 grams citric acid to 675 grams of extract (5.2 mg citric per gram of solvent). Sounds good. I'll go with that and after retrieving the crashed product I'll see if adding additional citric acid causes anymore clouds to form.

Loveall wrote:
doubledog wrote:
What about just salting out like you would do with limo or toluene? I mean to wash with some water and evaporate the water?

We can try that, it's a good idea.

I've thought about salting out with acidic water, but the key thing about this tek is its simplicity in crashing directly from the extract. I love this tek for not making me wash my separatory funnel!

Loveall wrote:
There should be excess citric acid coming through after evaporation. If washed it with fresh (dry) ethyl acetate and everything dissolves that means that it was all citric acid monohydrate and all the product crashed during the tek (I believe).

As above, I'm confused here. If everything dissolves in a fresh ethyl acetate wash, how do we separate the mescaline from the excess citric acid?

BTW, with all the excess acid, are we crashing other alkloids? Like in the lime/limo tek we titrate to pH 6.6-7.0 to avoid pulling too much junk.

Loveall, the sample you sent for analysis was fairly pure mescaline. But wasn't that produced using a lesser amount of acid, not this much excess? So we potentially have contaminants from crashing other alkloids as well as excess citric acid.

doubledog wrote:
I really like this thread, guys Smile

I was wondering when you were going to drop in and help us. Smile
 
Loveall
#85 Posted : 3/18/2021 6:48:54 PM

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shroombee wrote:
As above, I'm confused here. If everything dissolves in a fresh ethyl acetate wash, how do we separate the mescaline from the excess citric acid?

BTW, with all the excess acid, are we crashing other alkloids?


About the confusion: this would be a test to see if some mescaline citrate did not crash. In detail:

- Do the tek
- The spent ethyl acetate (after removing the mescaline citrate crystals with a filter) should only have citric acid. But what if it also still has some mescaline citrate in solution? To check we do a water wash. The water will grab citric acid and (if present) mescaline citrate. Then we evaporate this water.
- The water will evaporate to citric acid crystals (and if present mescaline citrate, but we hope that is not present).
- Imagine we get 3g of unknown xtals after evaporation. If they dissolve in 15ml of fresh ethyl acetate, it is highly unlikely that there was mescaline citrate. That's the test. We expect no mescaline citrate and to never have to do this again.
- This poweder may be interesting. Along with citric acid other stuff may be present. If anything does not dissolve into the fresh ethyl acetate I would send that for analysis (could be a different alkaloid salt, etc).

About the excess acid crashing other alkaloids, that is a good question. I think that is not happening, because the cloudiness and precipitation only happens once. However, like I said before we need to analyze the product again since the first time this worked we were not liberally bombing the ethyl acetate with a generous excess of citric acid.

One thing I don't understand is why are you worried about citric acid itself crashing or not dissolving? You found info that the monohydrate was 5% soluble (50mg+ of citric acid dissolves in one gram of ethyl acetate), and we have some water in the extract, which I think will make even anhydrous citric acid behave like the monohydrate (I'm assuming this though and I think that is what you observed yourself, but I could be wrong). Even with the half teaspoon bomb, we would only be at ~0.5% citric acid. It should all go easily into the watery Ethyl-acetate solution, right? Citric acid is considered soluble in ethyl acetate, while we are seeing that mescaline citrate is much less soluble. This is an ideal situation, and indeed it looks like we can force mescaline citrate out of solution by adding citric acid. It is a manske/Le-Chartelier/Comon-ion effect.

I'm hopeful we have stumbled on a simple and robust way to get very clean mescaline citrate, but time and more tests will tell.
๐Ÿ’š๐ŸŒต๐Ÿ’š Mescaline CIELO TEK ๐Ÿ’š๐ŸŒต๐Ÿ’š
๐Ÿ’š๐Ÿƒ๐Ÿ’š Salvinorin Chilled Acetone with IPA and Naphtha re-X TEK๐Ÿ’š๐Ÿƒ๐Ÿ’š
 
shroombee
#86 Posted : 3/18/2021 11:11:51 PM

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Loveall wrote:
shroombee wrote:
As above, I'm confused here. If everything dissolves in a fresh ethyl acetate wash, how do we separate the mescaline from the excess citric acid?

BTW, with all the excess acid, are we crashing other alkloids?


About the confusion: this would be a test to see if some mescaline citrate did not crash.

What I was referring to here was a fresh ethyl acetate wash to clean the dried product, believing we needed the wash to remove excess citric. But after running some experiments this afternoon, I think we're fine.

With a few rounds of gradually adding citric and magnetic stirring, I dissolved 20 mg citric per gram of solvent into a previously salted pull. This was the yellow pull in which I got the powder xtals. I moved the cleared (no longer cloudy) solvent to a new jar to see if I could get it to crash again, and I ended up adding 20 mg/gram before stopping. It wouldn't crash and the citric stayed in solution.

The 20 mg/gram is far above the 5.2 mg/gram of solvent that the tek is currently recommending. The trick to get it to dissolve in a timely manner is to use the magnetic stirrer. Otherwise wait quite a while. Recall my experiment watching a single grain of citric acid that would not dissolve in ethyl acetate after 10 minutes. The simple solution is just stir thoroughly. Smile

Quote:
In detail:

- Do the tek
- The spent ethyl acetate (after removing the mescaline citrate crystals with a filter) should only have citric acid. But what if it also still has some mescaline citrate in solution? To check we do a water wash. The water will grab citric acid and (if present) mescaline citrate. Then we evaporate this water.
- The water will evaporate to citric acid crystals (and if present mescaline citrate, but we hope that is not present).
- Imagine we get 3g of unknown xtals after evaporation. If they dissolve in 15ml of fresh ethyl acetate, it is highly unlikely that there was mescaline citrate. That's the test. We expect no mescaline citrate and to never have to do this again.
- This poweder may be interesting. Along with citric acid other stuff may be present. If anything does not dissolve into the fresh ethyl acetate I would send that for analysis (could be a different alkaloid salt, etc).

Sounds like a good verification test. I think you mean 3g unknown xtals dissolved in 150g of fresh ethyl acetate (20 mg/g)? 3g in 15g of ethyl acetate is 200 mg/g and the solubility of citric acid monohydrate is 52.8 mg/g.

Quote:
About the excess acid crashing other alkaloids, that is a good question. I think that is not happening, because the cloudiness and precipitation only happens once.

Even with a single precipitation event, is it possible to precipitate mescaline citrate as well as other alkaloids simultaneously if we add a ton of excess citric in one bombing? Similar to how using overly acidic water when salting in the lime/limo tek, we end up with a dirty product that needs to be cleaned with acetone and IPA washes.

Quote:
One thing I don't understand is why are you worried about citric acid itself crashing or not dissolving?

No more worries. Thanks. Smile Add excess and stir thoroughly to ensure the citric fully dissolves.
 
Loveall
#87 Posted : 3/19/2021 12:49:18 AM

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Shroombee,

Yeah, I made a mistake - if 3g of residue is left during the water/pull evap test then we would need 60g. What does not dissolve (if anything) could be very interesting. There may be other alkaloids that are hard to crystalize originally (their effects may be undesirable though).

Going my back to the salting step: I agree that more than one thing could crash at once in principle, but when we sent what crashed for analysis only mescaline was detected. Since nothing crashes after that (I'm getting the same results you are), I don't see a risk of unwanted stuff coming through if/when over acidifying. I did an extra test out of paranoia and over acidified the spent ethyl acetate from the pull that was sent for analysis. No new clouds form and nothing else crashes. This is a fortunate result that I think makes the tek robust and simple: 5mg/g of citric acid should crash the most stubborn of cloudiness and there is no indication of a risk of forcing unwanted stuff to crash (which is not the case for other TEKs as you point out).

I did the tek again, and got 1.1% yield (again). This is a great result for me compared to other teks that I have experience with, and I have very little concern that there is a significant ammount of mescaline that did not become product. From what I can see, once we debugged the difficulty crashing the cloudiness (that is, add more citric acid - thank you so much for helping with that), the process works reliably and there is little need to worry about other variables. Also, I'm finding that the time in lime and/or the time in the pull are second order effects. 1.0% yield is achievable rushing through these steps (minutes for each), patience gets you the last 0.1% to reach 1.1% (at least for the cactus I'm working with). I am finding I like the first pull to stay in the solvent overnight so the paste congeals and makes decanting trivial (cause I'm lazy and don't want to filter the first pull).

How did it go isolating what you got to crash? Did you get fluffy xtals ๐Ÿคž? If you can confirm the TEK I think it is ready to move to the main wiki.
๐Ÿ’š๐ŸŒต๐Ÿ’š Mescaline CIELO TEK ๐Ÿ’š๐ŸŒต๐Ÿ’š
๐Ÿ’š๐Ÿƒ๐Ÿ’š Salvinorin Chilled Acetone with IPA and Naphtha re-X TEK๐Ÿ’š๐Ÿƒ๐Ÿ’š
 
shroombee
#88 Posted : 3/19/2021 6:25:18 AM

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Here are some results from my experiments today.

These are from the same Run #3 (50 grams powdered, 22 hours basing, 6 x 10 minute pulls). All pulls combined and then split equally into four jars:

(A) Yellow solvent jar from a few posts back. Salted with 2 mg/gram citric. Overnight in the freezer. Nothing crashed. Removed floating ICE. Crashed by adding 1 mg/gram of citric;
(B) Salted with 5 mg/g citric. Crashed immediately;
(C) Salted with 3 mg/g malic. Did not crash. Put it in the frig for 90 minutes to see if that would help. Nothing. Then added 2 mg/g malic and it started crashing. The amount precipitating is small though (a lot smaller than jar (B);
(D) Salted with 20 mg/g citric. Crashed immediately. BUT the amount precipitating appears to be noticeably less than (B);

Given how well citric works and how excess appears to stay in the ethyl acetate, I don't see a reason to experiment with malic since (C) appears to be a dud. Thumbs down

Curious observation for the day: why am I getting more from (B) than (D)? They are the exact same extract. (B) salted with 5 mg/gram and (D) salted with 20 mg/gram. I have these jars in the frig and will decant and get yield numbers tomorrow. So it's possible the yield is closer than I believe and the visual difference is misleading. I have a theory for the difference, but for now I'll wait until tomorrow so we have hard numbers first.

Other good news is that I got nearly all the jars from the previous runs to crash by adding more citric! Thumbs up All jars were cloudy upon first bombing with citric, then they cleared with no xtals. Bringing them up to at least 5 mg/gram citric today made them crash. Not nearly as much yield as (B) though.

So crashing all in one bombing seems to be key. What could be the reason for that? Perhaps if not enough acid is added, the mescaline citrate cloud eventually dissolves into the ethyl acetate or the water. Whereas an excess of acid forces it out before it can dissolve? And once it's been dissolved the second bombing with acid doesn't force it out. Just guessing here. I wonder whether drying the ethyl acetate will release the mescaline citrate? Maybe try a molecular sieve?

Or I can do water pulls to see whether I can retrieve this lost product.

Quote:
I did the tek again, and got 1.1% yield (again). This is a great result for me compared to other teks that I have experience with, and I have very little concern that there is a significant ammount of mescaline that did not become product.

Have you adjusted yield comparisons for the different product molecular weights (mescaline HCl versus mescaline citrate for example)?

Quote:
I'm finding that the time in lime and/or the time in the pull are second order effects. 1.0% yield is achievable rushing through these steps (minutes for each), patience gets you the last 0.1% to reach 1.1% (at least for the cactus I'm working with).

You previously observed a 20% increase in yield by basing for at least one hour versus basing for a few minutes before adding solvent. Is that still a valid observation? And I observed needing an extra pull to get to "no freebase present" when basing 24 hours versus basing for a few minutes. I don't yet have yield numbers to confirm that as a general recommendation.

Quote:
How did it go isolating what you got to crash? Did you get fluffy xtals?

I have the precipitate sitting in the coffee filter but haven't scraped it out yet.

Quote:
If you can confirm the TEK I think it is ready to move to the main wiki.

We are very close! The (B) versus (D) jar difference is curious. As I said, I have a theory but will wait until getting yield numbers tomorrow. And would we want to do any verification processes first, such as your suggestions of A/B, water pulls, and sending out for analysis.
 
Loveall
#89 Posted : 3/19/2021 10:30:28 AM

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I suspect the differences in apparent yield is due to how the xtals formed and how fluffy they are. I've had this situation before, where it looked like I got less, but when measured on a scale yields were fine. The xtals can be very fluffy depending on how they crash (initial citric concentration, slow or fast citric dissolution, etc), so it is difficult to estimate the yield visually. Also, are you getting a xtals on the walls? This can add up too.

20% less yield (0.9%) was super rushed. I got 1% going pretty fast another time. Slow and patient was 1.1% (repeated). We can update the range to say 10-20% boost with patience, but that may vary with technique and if someone is skilled they could go faster with minimal losses.

I usually get the mescaline sulfate dihydrate from other teks. Molecular weight is the same (~280g for 1 mol of mesclaine) assuming mescaline citrate is anhydrous. It would be a little less potent if we are getting a mescaline citrate hydrate (but only ~2% per molecule of water). Both the sulfate and the citrate are 10% weaker by weight compared to MescalineHCl.

Agree that we are very close to having an independently verified TEK. Let's see what yields you get and if they look fine/consistent we can publish. Both us repeatedly getting good crashing at 5mg/g is great news ๐Ÿ‘
๐Ÿ’š๐ŸŒต๐Ÿ’š Mescaline CIELO TEK ๐Ÿ’š๐ŸŒต๐Ÿ’š
๐Ÿ’š๐Ÿƒ๐Ÿ’š Salvinorin Chilled Acetone with IPA and Naphtha re-X TEK๐Ÿ’š๐Ÿƒ๐Ÿ’š
 
Metta-Morpheus
#90 Posted : 3/19/2021 10:26:25 PM

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I plan on running this tek tomorrow. So I will refer all questions to this thread as/if they arise.

And again, thanks for your work friends!
โ€œYou think thatโ€™s air youโ€™re breathing?โ€ -Morpheus
โ€œWhoa fellas, Iโ€™m feeling kinda bowling ball-ish.โ€ -Leopold Butters Stoch
Itโ€™s got what plants crave. -Brawndo

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shroombee
#91 Posted : 3/19/2021 11:32:05 PM

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Metta-Morpheus wrote:
I plan on running this tek tomorrow. So I will refer all questions to this thread as/if they arise.

Let us know how it goes. Thumbs up There are some minor process refinements I want to share, as well as running some experiments that might result in additional yield or time savings. Nothing ground breaking though.

Quote:
And again, thanks for your work friends!

Thanks to Loveall for pioneering this tek! I'm pretty sure this tek has replaced lime/limonene in my mescaline extraction book. Smile
 
Loveall
#92 Posted : 3/20/2021 12:21:04 AM

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Best of luck Metta-Morpheus. I hope you get clouds in the solvent and that they crash nicely for you to a pure product with high yield ๐Ÿคž. Looking forward to your results - whatever they are.

Current experimental TEK

One thing I'm not sure about is the pulls. Not sure if 4 quick pulls before the paste congeals is better than waiting for ~one pull/day and letting the paste congeal together before the first pull. The latter is very easy to decant without a filter. I'm running more of that now (yields seem decent but the product is slightly tan). The former has given ~1% yields repeatedly and may be whiter at the end.

And a big thanks to shroombee for helping figure out how to make the process robust (or so we believe at this time).
๐Ÿ’š๐ŸŒต๐Ÿ’š Mescaline CIELO TEK ๐Ÿ’š๐ŸŒต๐Ÿ’š
๐Ÿ’š๐Ÿƒ๐Ÿ’š Salvinorin Chilled Acetone with IPA and Naphtha re-X TEK๐Ÿ’š๐Ÿƒ๐Ÿ’š
 
shroombee
#93 Posted : 3/20/2021 5:27:13 AM

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Loveall wrote:
I suspect the differences in apparent yield is due to how the xtals formed and how fluffy they are. I've had this situation before, where it looked like I got less, but when measured on a scale yields were fine. The xtals can be very fluffy depending on how they crash (initial citric concentration, slow or fast citric dissolution, etc), so it is difficult to estimate the yield visually. Also, are you getting a xtals on the walls? This can add up too.

Loveall, this is spot on. The composition of the product can make it look like yield is higher or lower as it is floating in the solvent.

Now for today's curiosity. Confused

Both samples represent 12.5 grams of powdered cactus (50 grams pulled, combined pulls split into 4 equal samples).
Sample (B) salted with 5 mg/gram;
Sample (D) salted with 20 mg/gram;

I weighed the coffee filters before using them to strain the xtals, then weighed the coffee filters after the xtals dried. After weighing the dried filters, I scraped the product and weighed it. I also used hot water to retrieve any xtals that were stuck to the jars. The water was evaporated in a dehydrator at 95 degrees.

Results for (B)
Difference in weight of coffee filter before/after filtering solvent: 117 mg;
Dry product scraped from coffee filter: 91 mg;
Unknown product still remaining in coffee filter: 26 mg (117 mg - 91 mg);
Evaporated xtals: 92 mg;

Total recovered yield: 183 mg (91 mg + 92 mg)
Percentage recovered yield: 1.46% (183 mg / 12.5 grams)

Results for (D)
Difference in weight of coffee filter before/after filtering solvent: 296 mg;
Dry product scraped from coffee filter: 176 mg;
Unknown product still remaining in coffee filter: 120 mg (296 mg - 176 mg);
Evaporated xtals: 0 mg (a clear, dry film, giving some resistance to the razor blade, not oily or sticky, bitter tasting - minimal weight);

Total recovered yield: 176 mg (176 mg + 0 mg);
Percentage recovered yield: 1.41% (176 mg / 12.5 grams);

First, I doubt this Peruvian Torch cactus contains 1.4-1.5% mescaline. Yields are maybe half that using lime/limo tek on this same batch. Although my lime/limo extractions seem to have a lot of variation and I've never perfected the tek. In the event this really is a higher yielding cactus and I happened to find a good extraction combination, the extraction process was: base the cactus, cover container to prevent over-drying (not sure this made a difference because the plastic wrap didn't stay on too tightly), wait 22 hours, then 6 x 10 minute pulls working quickly between pulls (bare minimum manipulation of the cactus during pulls, just enough to get the cactus under the solvent - let the solvent do the work).

Edit: I want to test whether we get more yield by doing fast pulls before the cactus gets sticky, which happens about 30 minutes after first contact with ethyl acetate.

Second, what the heck is the 296 mg extracted in (D)? That is theoretically a 2.4% yield. Nearly half of that product is still in the coffee filter, probably integrated with the fibers. I'm going to soak the filter in hot water to try to free up whatever is in there. And is this unknown product related to bombing with excess citric acid at 20 mg/gram?

Edit: Another possibly relevant difference between (B) and (D) is (B) was mag stirred for 3-5 minutes at moderate speed after adding the citric acid. (D) was stirred for 10 minutes at higher speed to ensure the citric acid was fully dissolved. In both cases, clouds crashing into xtals happened within a minute or two while the solution was being stirred.

I might experiment with making a 50 mg/gram saturated solution beforehand and add that to the pull so I don't have to mix so thoroughly -OR- go the other way and let the grains dissolve slowly. The idea is to see how this affects xtal formation and ease of later processing.

Also, given how quickly the crashing occurs, I believe it may be possible to filter the xtals within 5-10 minutes after adding the acid. Maybe a good experiment is to salt two jars from the same pull(s) and filter one at 10 minutes and the other several hours later. Any yield difference?

Quote:
And a big thanks to shroombee for helping figure out how to make the process robust (or so we believe at this time).

Thanks for having me along!
 
shroombee
#94 Posted : 3/20/2021 7:21:11 AM

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Loveall wrote:
One thing I'm not sure about is the pulls. Not sure if 4 quick pulls before the paste congeals is better than waiting for ~one pull/day and letting the paste congeal together before the first pull. The latter is very easy to decant without a filter.

Agreed it is very easy to decant the solvent once the cactus gets sticky. Since it appears we don't need to stir or mix the solvent into the cactus to get good yields, I might try the "fast pulls" experiment in a french press. That should make it easy to decant the solvent from the crumbly cactus.
 
Loveall
#95 Posted : 3/20/2021 10:25:48 AM

โค๏ธโ€๐Ÿ”ฅ

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Shroombee, here is my interpretation of your result:

1) Based in the MS analysis, we do expect the xtals from this TEK to be very clean mescaline citrate. I think your ~1.4% yield could be real. The higher the yield the more citric acid is needed to start building excess acid to crash the clouds (since more gets converted to the citrate salt). That may be why you had issues when we were just barely neutralizing the extract with citric. I've recently gotten 1.2% and have never seen that high with the limo or xylene TEKs (especially when cleaning the product towards whiteness). While the yield is high, it is not unheard of if starting with good cacti. How do the xtals look/feel/taste? Dry them slowly from water (takes a few days) and take pictures - they should become long needles - we can take a look here. I'll send pics of mine. Also, you can send them for anlysis and/or do a bioassay.

2) I would not worry about what remains inside the filter. It's probably citric acid and other soluble plant matter. Did you get a green ring as the green is wicked away? If part of the filter weight is dried citric acid, makes sense that the 20mg/g filter weighed about 4 times more more after drying than the 5mg/g one. We may have a ring of ctitric acid wicked away by the filter.

3) Looks like you discovered a way to avoid xtals sticking to the walls: use more citric acid. That is a great find, if all the xtals go into the filter to begin with, the TEK would be even less work in the final recovery step ๐Ÿ‘. It is funny to me how the 100g dry cacti TEK has gone from 250mg of citric, to 500mg, to 1g, to 2g, to 3.5g, and now may end up at 15g ๐Ÿ˜ฎ๐Ÿ˜…

I think you got an amazing result (pending confirmation). Let's confirm and if all is good, break out the congratulatory oolong tea (we don't do cigars here since we are about health and don't approve of using carcinogens ๐Ÿ™‚).
๐Ÿ’š๐ŸŒต๐Ÿ’š Mescaline CIELO TEK ๐Ÿ’š๐ŸŒต๐Ÿ’š
๐Ÿ’š๐Ÿƒ๐Ÿ’š Salvinorin Chilled Acetone with IPA and Naphtha re-X TEK๐Ÿ’š๐Ÿƒ๐Ÿ’š
 
Loveall
#96 Posted : 3/20/2021 1:27:55 PM

โค๏ธโ€๐Ÿ”ฅ

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Shroombee, see below for example images of slowly drying the xtals after dissolving them in a small amount of hot water. This is mescaline citrate according to MS results and multiple bioassays.
Loveall attached the following image(s):
IMG_20210320_092522124.jpg (3,305kb) downloaded 186 time(s).
IMG_20210320_092533068.jpg (3,250kb) downloaded 185 time(s).
๐Ÿ’š๐ŸŒต๐Ÿ’š Mescaline CIELO TEK ๐Ÿ’š๐ŸŒต๐Ÿ’š
๐Ÿ’š๐Ÿƒ๐Ÿ’š Salvinorin Chilled Acetone with IPA and Naphtha re-X TEK๐Ÿ’š๐Ÿƒ๐Ÿ’š
 
downwardsfromzero
#97 Posted : 3/20/2021 2:55:36 PM

Boundary Condition

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xtal pr0n payday Drool !!!

When I have secured some ethyl acetate I shall make my own attempt using a variant of this method.

Is there any reason against using fresh cactus?

An outline procedure would be as follows:

thinly slice fresh cactus, put in freezer overnight, thaw [possibly freeze-thaw cycle a couple of times], add requisite lime, adjust moisture level (if necessary using calcium oxide), pull with EtOAc, salt with citric.




โ€œThere is a way of manipulating matter and energy so as to produce what modern scientists call 'a field of force'. The field acts on the observer and puts him in a privileged position vis-à-vis the universe. From this position he has access to the realities which are ordinarily hidden from us by time and space, matter and energy. This is what we call the Great Work."
โ€• Jacques Bergier, quoting Fulcanelli
 
Loveall
#98 Posted : 3/20/2021 3:40:25 PM

โค๏ธโ€๐Ÿ”ฅ

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downwardsfromzero wrote:
xtal pr0n payday Drool !!!

When I have secured some ethyl acetate I shall make my own attempt using a variant of this method.

Is there any reason against using fresh cactus?

An outline procedure would be as follows:

thinly slice fresh cactus, put in freezer overnight, thaw [possibly freeze-thaw cycle a couple of times], add requisite lime, adjust moisture level (if necessary using calcium oxide), pull with EtOAc, salt with citric.


Looks good to me. I hope it works. I have some fresh cacti too I want to extract similar to this.

Here are the xtals from my previous post scraped up. 0.533% yield on the first pull (M1). Second pull is ongoing so we can measure p=1-M2/M1 (Elrik measured p ~ 0.4 for a Xylene tek, hoping we can improve on that here and push that up to maybe 0.5).
Loveall attached the following image(s):
IMG_20210320_112919648.jpg (2,243kb) downloaded 171 time(s).
๐Ÿ’š๐ŸŒต๐Ÿ’š Mescaline CIELO TEK ๐Ÿ’š๐ŸŒต๐Ÿ’š
๐Ÿ’š๐Ÿƒ๐Ÿ’š Salvinorin Chilled Acetone with IPA and Naphtha re-X TEK๐Ÿ’š๐Ÿƒ๐Ÿ’š
 
doubledog
#99 Posted : 3/20/2021 7:25:28 PM

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...and world consumption of ethyl acetate is rising...

What would be the way to recycle ethyl acetate after using in this tek?
Would be washing with water and drying with something like CaCl enough?
 
downwardsfromzero
#100 Posted : 3/20/2021 8:15:43 PM

Boundary Condition

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doubledog wrote:
...and world consumption of ethyl acetate is rising...
Indeed it is: https://communalnews.com...mand-in-food-packaging/

Quote:
What would be the way to recycle ethyl acetate after using in this tek?
Would be washing with water and drying with something like CaCl enough?
More or less, although if you're using it for basified pulls it would be good to include a sodium bicarbonate wash to minimise the acidity. You could otherwise use anhydrous sodium carbonate (soda ash) for the drying stage, which as we know can be produced quite easily from sodium bicarbonate.

I guess if you had the capacity for distillation you wouldn't be asking, but distillation would be a good option if there was any sound reason to free it from non-volatile contaminants.




โ€œThere is a way of manipulating matter and energy so as to produce what modern scientists call 'a field of force'. The field acts on the observer and puts him in a privileged position vis-à-vis the universe. From this position he has access to the realities which are ordinarily hidden from us by time and space, matter and energy. This is what we call the Great Work."
โ€• Jacques Bergier, quoting Fulcanelli
 
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