TEK Ethyl acetate approach [CIELO]

[Loveall]

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]

Can you add an n-hydrate option?

That's a great idea. I'll work on that!

 

[orchidist]

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]

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]

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]

Which Succinic acid do you use orchidist?

Also, do you use it to grow orchids too ?

 

[orchidist]

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

This is what I'm using

 

[orchidist]

Loveall, does this mean you'll be trying out succinate soon?

 

[Loveall]

Loveall, does this mean you'll be trying out succinate soon?

I believe so, wanna add to my mescaline salt collection

 

[orchidist]

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]

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]

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

 

[Loveall]

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]

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]

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]

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]

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
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.

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.

 

[orchidist]

Sorry for the delays on updates, it's been busy recently.

For my 2.85:1 paste ratio, without solvent drying:

Citrate crystallized at 0.48% freebase yield, a big improvement from the last run of 2.75:1, which was 0.33% freebase, and also an improvement on the 3:1 ratio.

Succinate did not crystallize at all. I've neutralized the succinate, dried it with K2CO3 and re-salted, but I've yet to collect the product. It's a fine powder, nothing like the pretty crystals I got before. Whatever the yield is from there, I don't think it's worth reporting on right now anyway, I'd consider this a big fail for succinic acid.

I collected the fumarate that crystallized, for a yield of 0.43% freebase.

If hydrates aren't involved, for this scale (~20g) the difference amounts to about 10mg of freebase mescaline lost

It seems that the fumarate and especially succinate have non-negligible solubility in wet EA. I don't particularly like working with the powder that forms when using either of these in dry EA. Switching from salting with solid crystals to dropwise addition of acid in solution may be the way to go to get nice crystals of these in dry solvent, but that's more work, not in the lazy spirit of CIELO. Using sodium carbonate as a weak drying agent when using these acids could be enough to close the yield gap without sacrificing nice crystals, though, so I'll look into it.

So my general assessment remains the same, goo comes from excessively wet paste, and is perhaps more likely to occur with certain cactus that more freely give up that water, for beginners, and for those using less accurate means of measuring out their paste ingredients. K2CO3 pretty much eliminated goo for me, and with citric acid, it still makes easy to filter crystals even when the solvent is dried, and is easy enough to use that it should probably be recommended for beginners and when optimizing the ratio for unfamiliar plant material.

I haven't done any experiments to check how it affects citrate yield, that'll be coming soon. Might be able to squeeze out a bit more of the M with drying.

 

[orchidist]

Calculator with hydration features now here. Let me know if there are any issues. If there are I'll correct them before making it the master version.

 

[shroombee]

Citrate crystallized at 0.48% yield, a big improvement from the last run of 2.75:1, which was 0.33%, and also an improvement on the 3:1 ratio.

Succinate did not crystallize at all. I've neutralized the succinate, dried it with K2CO3 and re-salted, but I've yet to collect the product. It's a fine powder, nothing like the pretty crystals I got before. Whatever the yield is from there, I don't think it's worth reporting on right now anyway, I'd consider this a big fail for succinic acid.

I collected the fumarate that crystallized, for a yield of 0.43%.

These yields are freebase weight correct? If so, it's probably a good idea to always state "freebase" when you're quoting your yields, as most of us quote the salt weight. Especially since none of our teks produce freebase mescaline (which I believe is an oil).