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Ethyl acetate approach Options
 
orchidist
#1181 Posted : 3/29/2022 10:50:58 PM

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Thought this was funny: I tasted the succinate. Like the acid on its own, it has a noticeable umami note to it. I think I've discovered the forbidden Aji-no-moto Laughing
 

STS is a community for people interested in growing, preserving and researching botanical species, particularly those with remarkable therapeutic and/or psychoactive properties.
 
orchidist
#1182 Posted : 3/30/2022 3:39:55 AM

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Citrate yields have been updated here
 
Loveall
#1183 Posted : 3/30/2022 10:09:51 AM

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orchidist wrote:
Citrate yields have been updated here


Thanks.

So less water in the paste helped with goo in your case? That's interesting.

Another thing to note is that your cactus is yielding on the lower side (0.3%).

Perhaps lower yielding cacti xtalization is more sensitive to citrate. While Cheelin and I both xtalized additional pulls 6-10 with very low yields, by then other plant matter pulled was low also (we were checking for extraction completenes in pulls 1-5.

If anyone gets citrate goo, them gets xtals with fumaric, succinic, or other anions, please report it here with yields. Wondering if a consistent theme can emerge here.

PS: I believe succinic acid solubility in EA is ~25mg/g based on the plot below (eyeballing X=0.002 in pure EA)
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Solubility-of-succinic-acid-SA-in-ethanol-ethyl-acetate-mixtures-at-29815-K-The-line.png (52kb) downloaded 203 time(s).
 
Loveall
#1184 Posted : 3/30/2022 10:58:13 AM

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orchidist wrote:
I posted about this in the salts to freebase calculator thread earlier, wanted to cross post it here because I think it'll be useful to many who try the TEK, and since it's browser based, doesn't require any spreadsheet software.

I've just added the ability to automatically produce yield % (standardized on the freebase to maintain equivalence between TEKS using different acids) and added some documentation.

Link to the repo is here

Planning to add an interactive CIELO ingredient calculator too.



Can you add an n-hydrate option?
 
orchidist
#1185 Posted : 3/30/2022 1:21:36 PM

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Loveall wrote:

Can you add an n-hydrate option?


That's a great idea. I'll work on that!
 
orchidist
#1186 Posted : 3/30/2022 2:02:07 PM

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Loveall wrote:

So less water in the paste helped with goo in your case? That's interesting.

Another thing to note is that your cactus is yielding on the lower side (0.3%).

Perhaps lower yielding cacti xtalization is more sensitive to citrate. While Cheelin and I both xtalized additional pulls 6-10 with very low yields, by then other plant matter pulled was low also (we were checking for extraction completenes in pulls 1-5.


Yes, I'm working with a new batch of this powder, so I'm not sure if comparing to my original 0.45% yield is a direct one, time will tell, this might be the best it can do. At the lowest end of moisture with the original powder (2.7:1), I got no extraction at all, so I might not have hit the sweet spot yet.

Definitely notable that I didn't have this problem with the higher yielding cactus (0.66% freebase), the one that turned to rubber at 3:1. The citrate crystallized out of it without using a powerful drying agent like K2CO3.

I'm inclined to believe that water dissolving in the EA is the dominant factor here (along with ambient conditions), and some hydrophilic component (perhaps polysaccharides, which could also explain the textural difference) holds that water back in the paste during extraction. I did an A/B extraction a while back to try to clean up the oil, but I got oil back. That should've excluded the vast majority of other plant material. I wasn't using a proper drying agent for that extraction, only Na2CO3.
 
Loveall
#1187 Posted : 3/30/2022 2:36:18 PM

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orchidist wrote:
Loveall wrote:

So less water in the paste helped with goo in your case? That's interesting.

Another thing to note is that your cactus is yielding on the lower side (0.3%).

Perhaps lower yielding cacti xtalization is more sensitive to citrate. While Cheelin and I both xtalized additional pulls 6-10 with very low yields, by then other plant matter pulled was low also (we were checking for extraction completenes in pulls 1-5.


Yes, I'm working with a new batch of this powder, so I'm not sure if comparing to my original 0.45% yield is a direct one, time will tell, this might be the best it can do. At the lowest end of moisture with the original powder (2.7:1), I got no extraction at all, so I might not have hit the sweet spot yet.

Definitely notable that I didn't have this problem with the higher yielding cactus (0.66% freebase), the one that turned to rubber at 3:1. The citrate crystallized out of it without using a powerful drying agent like K2CO3.

I'm inclined to believe that water dissolving in the EA is the dominant factor here (along with ambient conditions), and some hydrophilic component (perhaps polysaccharides, which could also explain the textural difference) holds that water back in the paste during extraction. I did an A/B extraction a while back to try to clean up the oil, but I got oil back. That should've excluded the vast majority of other plant material. I wasn't using a proper drying agent for that extraction, only Na2CO3.


Perhaps we should reccommend fumaric or succinic over citric then. Seems more robust for a wider range of starting concentrations (of both water and mescaline) based on your results.
 
orchidist
#1188 Posted : 3/30/2022 2:57:26 PM

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I would be mostly comfortable with making that recommendation for fumaric acid. It seems to solve the goo problem pretty well. I'm hesitant to recommend succinic acid yet, as I haven't tested it with the 3:1 paste. Definitely want to continue looking into drying agents with all three, to make sure we're not seeing any loss of yield and to explore hydration of the product.

I didn't make any quantitative comparisons at the time, but in earlier experiments with extractions that would've oiled out with citric, using fumaric acid, Na2CO3 drying seemed to give bigger crystals. K2CO3 drying resulted in a very fine precipitate that would probably be hard to collect with a typical coffee filter. Perhaps the nice looking sheets observed without/incomplete drying are the hydrate, powder is anhydrous. Citrate crystals formed with K2CO3 drying remained as needles, and were easier to work with. I haven't tried this yet with succinic acid.

While Na2CO3 isn't listed as a drying agent anywhere, it does clump up when added to wet EA, so it probably does do a little something. K2CO3 deliquesces in wet EA, definitely more effective at pulling water.
 
Loveall
#1189 Posted : 3/30/2022 10:58:05 PM

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Which Succinic acid do you use orchidist?

Also, do you use it to grow orchids too 😅?
 
orchidist
#1190 Posted : 3/30/2022 11:04:12 PM

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I've actually never heard of succinic acid as a plant supplement, which is surprising, since I've spent years surrounded by orchid obsessives. Might give it a shot, perhaps try it on cacti, too Pleased

This is what I'm using


 
orchidist
#1191 Posted : 3/30/2022 11:14:58 PM

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Loveall, does this mean you'll be trying out succinate soon? 🙃
 
Loveall
#1192 Posted : 3/31/2022 12:18:17 AM

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orchidist wrote:
Loveall, does this mean you'll be trying out succinate soon? 🙃


I believe so, wanna add to my mescaline salt collection 😅
 
orchidist
#1193 Posted : 3/31/2022 3:28:17 AM

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Working on updating the calculator to add hydration, I have it calculating yield % with hydration of the source salt and it converts to equivalent anhydrous salts, but haven't implemented adjustments for hydration of the destination salt. I pushed what I have. It's on the hydrate-calculations branch of the repository, the old one is still available as the master branch until I'm happy with it, and replace it with this version.

If I consider the citrate to be the monohydrate, my yield goes from 0.36% down to 0.34% freebase, which then agrees more closely with anhydrous fumarate (0.33%), and anhydrous dimescaline succinate (0.31%). Certainly need more data points to call it though.
 
orchidist
#1194 Posted : 4/1/2022 6:53:23 PM

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Did another extraction yesterday. Mixed up 60g worth of paste, extracted it, and then split the extract into three jars approximately equally, recorded the mass of each for yield calculations later on. I upped the water ratio to 2.85:1 for this run. No drying agent used in these runs. Haven't collected any yields yet, still observing.

Fumarate started crystallizing first, but it looks like yields will be lower than the run with less water in the paste.
Citrate is crystallizing, it's still cloudy though, so still need to wait. The previous run was done by this time. It looks like a good yield, though. Looking forward to decanting this.
Succinate is cloudy, but not nearly as cloudy as the citrate, no crystallization yet.

Considering that I was working under much colder conditions for the previous run where I got those beautiful succinate crystals, I put the succinate and fumarate in the fridge to see if any more crystals crash out. No change for succinate (yet, hopefully), but fumarate did cloud up again, so I expect a boost.

It seems to me that drying the solvent is the major thing that's going to improve reliability (and/or yield) for any of the three acids.

Citrate crystallized well, and pretty quickly with easy to filter crystals when it was dried thoroughly with K2CO3.
Fumarate usually crystallizes very fast, it might perform better with Na2CO3 than K2CO3, as it yielded an extremely fine precipitate when dried aggressively. I'll have to try again and see if that was just a fluke.
Succinate looks like it will prefer drier conditions as well, but I haven't tested it alongside either drying agent yet.
 
orchidist
#1195 Posted : 4/2/2022 4:04:07 AM

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Alkaloid conversion/yield calculator has been updated to handle hydrates! Pretty happy with it!
orchidist attached the following image(s):
salt-converter.png (118kb) downloaded 103 time(s).
 
Loveall
#1196 Posted : 4/2/2022 2:55:39 PM

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Orchidist and Starbob: What is your assessment of goo after your work so far? Is it simply going away with practice and better technique?

Cheelin is reporting xtals from a 0.1% old cactus log. No goo. Simple tech. His data takes away the low yield goo signal.
 
orchidist
#1197 Posted : 4/2/2022 3:06:09 PM

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Yeah, my general sense of things is that it's water dissolved in the solvent that's the problem. I'd recommend K2CO3 as a guard rail for working with new cactus, and keeping citric acid for salting, potentially dropping the step once familiarity is developed.

I'm going to decant the citrate today to get a yield from my last experiment (no drying agent was used, but yield looks good), the others have so few crystals that I'm going to try to wash with saturated sodium carbonate to neutralize the acid, dry them, and salt again. I'm expecting to find that drying the solvent is mandatory for the other salts I'm trying, since it seems that they become soluble in wet EA.
 
Loveall
#1198 Posted : 4/2/2022 3:13:17 PM

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orchidist wrote:
Alkaloid conversion/yield calculator has been updated to handle hydrates! Pretty happy with it!


Thanks! Mescaline Sulfate is known to be a di-hydrate. Can that be coded as default?

I'm adding a link to this calculator in the WIKI
 
orchidist
#1199 Posted : 4/2/2022 3:42:43 PM

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Loveall wrote:
orchidist wrote:
Alkaloid conversion/yield calculator has been updated to handle hydrates! Pretty happy with it!


Thanks! Mescaline Sulfate is known to be a di-hydrate. Can that be coded as default?

I'm adding a link to this calculator in the WIKI


Will need to do a little more work to make defaults, but it won't be difficult
 
starbob
#1200 Posted : 4/2/2022 7:30:23 PM

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Loveall wrote:
Orchidist and Starbob: What is your assessment of goo after your work so far? Is it simply going away with practice and better technique?

I'm puzzled really, I don't know. I only had goo this once to speak of, and since I don't have a smoking-gun and given my inexperience I won't rule out I somehow goofed it...
I hope it goes away with practice Big grin
Technique-wise, I'm not trying for speed runs so I don't think it hurts to take another 2mins to slow down adding the acid as an additional EA solution. If goo is just some rare thing and this reduces some sliver of risk with little cost, I'll do it everytime.

Loveall wrote:
Cheelin is reporting xtals from a 0.1% old cactus log. No goo. Simple tech. His data takes away the low yield goo signal.

I haven't had a correlation with low yield either. I didn't have goo in any of my few previous attempts and they were all with <0.1% yield old log PC powder I made myself. And out of those, some I had made clear major mistakes; I didn't get goo.

 
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