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Ethyl acetate approach [CIELO] Options
 
orchidist
#1201 Posted : 4/6/2022 3:03:51 AM

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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.
 

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orchidist
#1202 Posted : 4/6/2022 3:25:35 AM

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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
#1203 Posted : 4/6/2022 4:02:24 AM

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orchidist wrote:
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). Smile
 
orchidist
#1204 Posted : 4/6/2022 4:05:07 AM

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shroombee wrote:

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). Smile


Yes, yes, good catch! I did exactly that in earlier posts, forgot to here. I'll edit it
 
cyantific
#1205 Posted : 4/6/2022 6:15:19 AM

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Using this method with citric acid for example, is the end product considered full spectrum like you would get from tea/tar... or does this process yield mostly M leaving the other alkaloids behind?
 
_Trip_
#1206 Posted : 4/6/2022 6:18:50 AM

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cyantific wrote:
Using this method with citric acid for example, is the end product considered full spectrum like you would get from tea/tar... or does this process yield mostly M leaving the other alkaloids behind?


If you mean the cielo method, LC-MS results showed near pure mescaline. It is not full spectrum, the EA and citrate appears to be very selective to mescaline and forms M citrate crystals.
Disclaimer: All my posts are of total fiction.



 
cyantific
#1207 Posted : 4/6/2022 8:47:11 AM

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_Trip_ wrote:
It is not full spectrum, the EA and citrate appears to be very selective to mescaline and forms M citrate crystals.

Is there any reason to suspect that changing to acid would affect the purity, for example salting with fumarate acid?

Wondering if anyone has experimented with Oxaloacetate acid?

Oxaloacetate acid is a crystalline organic compound and intermediate of the citric acid cycle, where it reacts with acetyl-CoA to form citrate, catalyzed by citrate synthase.


 
_Trip_
#1208 Posted : 4/6/2022 9:36:08 AM

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Post #926 of this thread shows Loveall's experimentation with other acids and the corresponding mescaline salt forms they correspond with. I believe the math indicates other salt forms were quite selective too.

I don't believe anyone has experimented with Oxaloacetate acid. The Cielo wiki has information on what has and hasn't been tested as well as post #926.
Disclaimer: All my posts are of total fiction.



 
Loveall
#1209 Posted : 4/6/2022 10:04:34 AM

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_Trip_ wrote:
cyantific wrote:
Using this method with citric acid for example, is the end product considered full spectrum like you would get from tea/tar... or does this process yield mostly M leaving the other alkaloids behind?


If you mean the cielo method, LC-MS results showed near pure mescaline. It is not full spectrum, the EA and citrate appears to be very selective to mescaline and forms M citrate crystals.


Yes. A second possibility is that the cactus used for the LC-MC mostly contained mescaline and only small amounts of other alkaloids that would come through this process. DMPEA and anhalinine may come through in this process I think (if present). Other known alkaloids such ash 3-Methoxytyramine, 4-hydroxy-3-methoxyphenethylamine, 4-hydroxy-3,5-dimethoxyphenethylamine, anhalonidine, hordenine, and tyramine are probably not pulled by this TEK because of the hydroxy group being +1 after basing.
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Loveall
#1210 Posted : 4/6/2022 10:27:20 AM

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orchidist wrote:
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.


Interesting results, thanks.

When using other drying agents we never saw a yield boost, but we don't have any K2CO3 data, so looking forward to more data on that.

If you can repeat the 3:1 ratio goo again that may be valuable. It would check the possibility that lack of practice can be a driver for goo on some starting cacti. You can dry a sample of the extract and if that becomes goo, while the sample dried with K2CO3 xtalizes, them you will have clinched the reason as excess water and have a solution at the same time I believe.

Previously as you may know, we saw stable yields across a wide range of water values ~2.7:1 to ~3.3:1, then a dropoff when the paste is too dry (an experimental a mystery to me). With too much water large emulsions form that begin to affect yield. We did not come across goo during these tests on the cacti matter we had.
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orchidist
#1211 Posted : 4/6/2022 4:02:00 PM

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Loveall wrote:

When using other drying agents we never saw a yield boost, but we don't have any K2CO3 data, so looking forward to more data on that.


Yeah, I would be kinda surprised to get a boost, but with CaCl2 potentially absorbing some product, and Na2CO3 not completely drying the solvent, the benefit of drying might have been obscured.

Loveall wrote:

If you can repeat the 3:1 ratio goo again that may be valuable. It would check the possibility that lack of practice can be a driver for goo on some starting cacti. You can dry a sample of the extract and if that becomes goo, while the sample dried with K2CO3 xtalizes, them you will have clinched the reason as excess water and have a solution at the same time I believe.

Previously as you may know, we saw stable yields across a wide range of water values ~2.7:1 to ~3.3:1, then a dropoff when the paste is too dry (an experimental a mystery to me). With too much water large emulsions form that begin to affect yield. We did not come across goo during these tests on the cacti matter we had.


I can do that. And yeah, I didn't look very closely at the paste ratio at first, since I didn't have any emulsification. Always got a nice clear solvent at the end of my pulls. I did also get goo after A/B extraction, which should exclude most other plant compounds. Salting the solvent from that process also separated into a biphasic mixture and oiled out.

I'm still suspicious that cooler working conditions may contribute. I can't remember if I saw it in this thread or somewhere else, that water has an inverse solubility curve in EA. I haven't been able to find any sources that explore that though. I'd love to find one. Every result focuses on solubility of EA in water.

 
orchidist
#1212 Posted : 4/11/2022 4:30:35 AM

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Hey, just a quick update. Life's been busy, so I haven't been able to do any new runs or work on the calculator in the last week, but I did finally get to processing the succinate that failed to crystallize.

The volume of the solvent was about 200mL. I went about washing the solvent with ~30mL of saturated sodium carbonate to neutralize and allowed it to stir for 30 minutes on a stir plate. I transferred it to a separatory funnel and allowed it to separate, collected the solvent and dried it with K2CO3. pH paper registered slightly alkaline. The solvent clouded slightly during the drying step, I'm not exactly sure why that would be. Maybe some of the salt didn't react during the washing/neutralization step, and began precipitating? I decanted it and waited for anything to settle for a day. Nothing at all settled and the haze persisted, so, I decided to proceed with salting. The mixture became opaque and crystals in suspension were visible within a half hour. It took ~2 days for the solvent to completely clear. I gravity filtered the solvent through a 2.5 micron filter paper (possibly overkill, took a long time, but I wanted as much as I could collect), washed it a few times with fresh EA, and allowed it to dry. The result was a puck of fine, bright white powder that was easily collected off the filter paper.

Surprisingly, this workup gave me the same 0.48% (freebase) yield as the successful run with citric acid. It may be contaminated with a small amount of potassium and/or sodium succinate, though. I can't discern any difference in taste between this product and the one from the previous run that gave that beautiful crystal shrub, though, so I believe it's probably reasonably pure.

I decided not to try to get the remains of my fumarate run using this same method, since the amount I projected I'd recover from it was smaller than I care to put effort into. Hopefully it'll come out when I start to reuse solvent for future extractions.
 
Loveall
#1213 Posted : 4/11/2022 8:54:44 AM

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orchidist wrote:
Hey, just a quick update. Life's been busy, so I haven't been able to do any new runs or work on the calculator in the last week, but I did finally get to processing the succinate that failed to crystallize.

The volume of the solvent was about 200mL. I went about washing the solvent with ~30mL of saturated sodium carbonate to neutralize and allowed it to stir for 30 minutes on a stir plate. I transferred it to a separatory funnel and allowed it to separate, collected the solvent and dried it with K2CO3. pH paper registered slightly alkaline. The solvent clouded slightly during the drying step, I'm not exactly sure why that would be. Maybe some of the salt didn't react during the washing/neutralization step, and began precipitating? I decanted it and waited for anything to settle for a day. Nothing at all settled and the haze persisted, so, I decided to proceed with salting. The mixture became opaque and crystals in suspension were visible within a half hour. It took ~2 days for the solvent to completely clear. I gravity filtered the solvent through a 2.5 micron filter paper (possibly overkill, took a long time, but I wanted as much as I could collect), washed it a few times with fresh EA, and allowed it to dry. The result was a puck of fine, bright white powder that was easily collected off the filter paper.

Surprisingly, this workup gave me the same 0.48% (freebase) yield as the successful run with citric acid. It may be contaminated with a small amount of potassium and/or sodium succinate, though. I can't discern any difference in taste between this product and the one from the previous run that gave that beautiful crystal shrub, though, so I believe it's probably reasonably pure.

I decided not to try to get the remains of my fumarate run using this same method, since the amount I projected I'd recover from it was smaller than I care to put effort into. Hopefully it'll come out when I start to reuse solvent for future extractions.


After neutralizing and drying you salted with succinic again? So is the conclusion that succimnatr wont precipitate/crystalize from wet EA, but will Xtalize from chemichally dried EA?

Why is the FB yield a surprise vs citric acid? We expect citrate to (roughly) fully precipitate from wet EA based on previous TEK testing.
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orchidist
#1214 Posted : 4/11/2022 9:09:50 AM

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Yes, I salted again with succinic acid. I'm surprised that the extra workup didn't cause any appreciable loss of yield. Figured at least a small amount would be lost due to washing, and the unexpected clouding while drying was somewhat concerning too.

Also I forgot to mention, using the small amount of succinate crystals left behind after decanting, I washed them back to the bottom of the jar then added approximately 100ml of dry EA. After adding a few drops of water and allowing it to dissolve in the EA, the crystals also dissolved. So I'm pretty certain of its solubility in wet solvent, and my disparity in the first attempt with succincic was due to that, not the formation of the dimescaline salt.
 
orchidist
#1215 Posted : 4/11/2022 9:28:16 AM

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With succinate, you for sure run the risk of not crystallizing at all without drying. With fumarate, looks like it'll reduce yield. For both, I'd 100% recommend chemical drying. Unfortunately that seems to also greatly reduce the size of the crystals, at least when the salting is done by directly adding solid acid. Haven't tried using solutions of them to slowly neutralize yet.


Of all three citric acid does seem the easiest, still. The official TEK should stick with citric. Part of me still wants to reproduce those gorgeous mossy looking succinate crystals that I got the first time, but with good yields.
 
Loveall
#1216 Posted : 4/11/2022 11:36:51 AM

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Thanks for your contributions orchidist. Will keep the main TEK as is for now. For people having issues will recomend drying and using fumaric as a guardrail option.

Since the water wash was saturated with sodium carb it had a high ionic strength and minimal product loss is expected. Mindlusion has confirmed this with brine washes.

Xtal formation can be tricky. There could be a wetness region where no succinate precipitates, then a slightly dryer region where larger dimescaline precipitates, then a dry region where small xtal monomescaline precipitates. Also, the excess succinic concentration could affect precipitation (excess in solution forcing the salt to crash).
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orchidist
#1217 Posted : 4/11/2022 5:30:13 PM

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Thanks to you and everyone else too! This has been a very rewarding experience!

Loveall wrote:
Since the water wash was saturated with sodium carb it had a high ionic strength and minimal product loss is expected. Mindlusion has confirmed this with brine washes.


I missed that! Glad that's the case. Now we have some replication Smile

Loveall wrote:
For people having issues will recommend drying and using fumaric as a guardrail option.


At this point I would still recommend citric for goo resolution, since it produces large crystals in all cases. I have been using filters made for lab use to collect product, I think it's likely that some of the finer crystals will pass through a coffee filter. The fumarate especially was fine as flour.

I still think these two acids are worthy of a footnote in the TEK. If somebody wants brilliant white crystals, K2CO3/succinic/good filter paper appears to be an excellent way to go for that.


Loveall wrote:

Xtal formation can be tricky. There could be a wetness region where no succinate precipitates, then a slightly dryer region where larger dimescaline precipitates, then a dry region where small xtal monomescaline precipitates. Also, the excess succinic concentration could affect precipitation (excess in solution forcing the salt to crash).


Definitely testable! Though at this point, maybe an open question I'll leave to others to explore since I'd like to dry all my extracts from here on and spend time focusing on optimizing yields for the cactus I have. Still absolutely willing to do any testing that involves dry solvents

Had I held onto the solvent from the succinate that produced the result that suggested dimescaline, I could've tested it easily. If I did the same recovery procedure and got more product, that would have given us an answer. My gut thinks the slightly dryer region slows down formation/decreases the amount of nucleation sites (it took a lot longer for that jar to crystallize compared to the others and it clouded less) enough to allow for the formation of larger crystals. If that's the case, those nice crystals should be obtainable by slow addition of SA in solution. I will for sure be testing that in a future run.
 
orchidist
#1218 Posted : 4/18/2022 3:01:00 AM

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The salt conversion calculator now supports default values for hydration. Currently the only one I've set a default for is M sulfate dihydrate. If there are others, let me know, and I'll add those.
 
merkin
#1219 Posted : 5/11/2022 7:59:38 AM

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Hi guys. I'm back on the wagon again and into my first CIELO for many months. The major difference now is I'm finally getting to use my own plants. My previous extractions were with some old powder bought many years ago, yet still super productive. I have a few garage shelves stacked with wrapped pedros and bridgesii but started with bridgesii because some of them had shrunk and rotted (2), one dried quite considerably and 3 more looked like they looked the day I wrapped them! All almost exactly one year ago. Wasn't sure how long to rest and in hindsight should have checked more often. Anyway...

Started with a 800mm bridgesii, quite dry already so I just sliced and dehydrated. Ground the entire thing (thorns previously removed for handling purposes), core and all. Gave ~220g, many small pieces of 'wood' made it into the 'flour' as my sieves aren't fine enough. Didn't think that would be a real issue and don't think it was. In the dough it was hardly noticeable. The other 3 lengths (~800mm each) I will remove the core first.

Extraction process went well I think. I followed Cheelin's nice breakdown steps quite thoroughly and am at about 36 hours into the 'crystallization' phase. Seems I'm looking at a fine powder result at the moment as more action on bottom (with some tiny crystal clusters tumbling around visible now an again).

Seeing the results per pics below, I was disappointed not to get needle-y crystal clusters so I started reading this thread from about page 40 last night and now I have some questions for y'all, also as some of this process is quite different with my 'fresh' product:

1. Colors: The green color was far more richly intense than I expected. Basically it's black unless backlit. This made looking for debris and water almost impossible. I filtered twice (first straight from the extraction and second after overnight fridge settle) but nothing seemed to pass the initial filter from the plunger (coffee plunger fits perfectly in a 1000ml tall beaker - I broke my original glass). Is this normal? I am used to a light brown but pretty clear liquid, from my previous 'old' powder, which was easy to see debris or water drops.

- The settling color is this intense purple-red gradually going into brown then green at the bottom if lit normally, but green if lit from behind? The purple-red grows downwards as time progresses. Never saw this before except that one crystal pic in the wiki so I assume all good?

- Saturation of color made it impossible to see if citric dissolved or honestly to even notice any clouding! I switched to a lab store AR grade which was more crystalline than the finer supermarket type I used before. It does not dissolve quickly so I may have stirred to much after dropping in (2.5g in ~820ml EA).

2. By looks of things I am headed for powder again (I always went with the 'bomb and stir' method before so I am OK with that). Maybe brought on by too much stirring after citric? I didn't stir THAT much though. Keen to get crystals at some point so I would like to get this right. I have ground the citric to powder in pestle for next run. Or predissolve?

3. Nemoo's suggestion of pre-dissolving the acid. How would this work? Dissolve all 2.5g citric (or however much) in how much EA before adding? The same thought had come to me when I saw nothing in the green blackness after adding citric and looking for signs of dissolving remnants or clouding. I worried that citric wasn't dissolving fast enough but maybe I am over thinking it?

4. This brings me to fumaric acid. Maybe I will get better chance at crystals like this. I stocked up on all acids to try them. Loveall's results are always inspiring and I'm keen on trying the succinic per orchidist. Fumaric always seemed to be a non-dissolving powder every time I have used it (without violent agitation)?

How much fumaric to use for 100g Cactus / ~820ml EA extract (originally ~946ml)?
I read 10mg (per g EA? or per g Cactus?) but not sure here
If I pre-dissolve fumaric - how many mg in how many ml EA would be good?

5. Drying extract solvent: with Potassium Carbonate. How does one actually do this? I read to keep it 30 mins at least, but have only ever 'dried' Acetone for spice fumarate with MgSO4. How would one "dry" the extract (~800ml+) with this method? Dump, stir and filter after 30+ min? How much K-Carb to add?

Looking forward to a good few sessions getting to know my own plants, well at least two of them (even though they've been cloned and growing all over the place). My Peruvians haven't grown enough yet to think about harvest, but I've got lots of pedro and a bit more bridgesii waiting...there's just something special about growing your own, like shrooms too, there's an implied affinity, well, psychologically anyway Pleased

Pretty glad I didn't get goo tho, or at least not much! Once was enough.

Cheers


*** EDIT :: approaching 48 hours ***

Spoke too soon about the crystals! OMG. This deceptively dark liquid hides a gazillion little starry clusters on the sides of the beaker. When larger they tumble in slow motion to the fluffy bottom below. The color of the red-purple is psychedelic, so is the green. Not the best pics I know - it's so hard to shoot pics holding phone and torch and juggling reflections on the glass. Looks like dirt but really it is a sparkling wonderland of crystal beauty and color. Unbelievable. A whole new experience and all from my garden! The Mesc Gods are smiling on me today saying thanks for 15+ years of dutiful propogation! Loveall, this is just beyond words. Move over Manske... Wow, Wow WOW.




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orchidist
#1220 Posted : 5/12/2022 4:45:35 PM

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Hey! Sorry I fell off off this. Spring is a busy time in the garden, have spent every moment of my free time out there. I do plan on revisiting the experiments.



merkin wrote:

3. Nemoo's suggestion of pre-dissolving the acid. How would this work? Dissolve all 2.5g citric (or however much) in how much EA before adding? The same thought had come to me when I saw nothing in the green blackness after adding citric and looking for signs of dissolving remnants or clouding. I worried that citric wasn't dissolving fast enough but maybe I am over thinking it?


You'd create a saturated solution of acid in ethyl acetate. Just keep adding it until no more dissolves and decant what didn't dissolve. We were exploring gradual addition as a means to prevent the product from oiling out, but it seems like you're not having that issue. I don't think it'll be worth your time to do.

merkin wrote:

4. This brings me to fumaric acid. Maybe I will get better chance at crystals like this. I stocked up on all acids to try them. Loveall's results are always inspiring and I'm keen on trying the succinic per orchidist. Fumaric always seemed to be a non-dissolving powder every time I have used it (without violent agitation)?


For the fumaric acid, I'd strongly recommend using a drying agent. FA resists oiling out, but with no drying at all, yields will suffer. My experiments so far suggest that a drying agent as strong as potassium carbonate may not be necessary to get good yields with FA. When the solvent is too dry, the salt comes out as a fine precipitate. I've found that sodium carbonate pulls out enough water to get yields comparable to CA, nice looking crystals, and very rapid precipitation.

I've found succinic to be extremely touchy, my results varied a lot between runs and I only got beautiful crystals once, by accident, and the yields were questionable...I'm not sure if it's related to the succinate's solubility, the possibility of forming either di or monomescaline succinate, or what. I've gotten a few results where the mass of my yield suggests the formation of the dimescaline salt, and others that are higher than expected for dimescaline, but less than expected if it were precipitating as monomescaline.

I still intend to investigate succinic acid more, because it's fun, but I can't recommend it if your goal is maximum yield, reliability, and predictable dosing...since we don't really know the identity of the product yet.

merkin wrote:

How much fumaric to use for 100g Cactus / ~820ml EA extract (originally ~946ml)?
I read 10mg (per g EA? or per g Cactus?) but not sure here
If I pre-dissolve fumaric - how many mg in how many ml EA would be good?


I've been using FA in much lower quantities than CA, I don't have my notes in front of me right now, but I think for a very safe lower bound, assume 2% of the dry mass of the cactus is freebase mescaline, then from there calculate the mass of whatever acid you're using that would be required to neutralize it.

That calculation would be:

neutralizing_quantity = mass_cactus * 2/100 * molar_mass_acid / molar_mass_mescaline

For 100g of cactus and Fumaric acid, that's ~2.2g of FA.

To estimate the mass of acid per gram of solvent, I did the following calculation using 0.9 g/mL as the density of the solvent:

target_concentration = neutralizing_quantity / (input_ea_volume_ml * 0.9 g/mL * percent_solvent_recovery)

For me, I've recovered on average 87% of the solvent I put into the extraction. So for fumaric acid, that is about ~3mg/g of solvent, well within the limits of FA's solubility in EA.

merkin wrote:

5. Drying extract solvent: with Potassium Carbonate. How does one actually do this? I read to keep it 30 mins at least, but have only ever 'dried' Acetone for spice fumarate with MgSO4. How would one "dry" the extract (~800ml+) with this method? Dump, stir and filter after 30+ min? How much K-Carb to add?


I have been working on volumes around 500mL and used probably 1-2 teaspoons worth of potassium carbonate. The amount isn't super critical, you'll know when it's done by observation. After about half an hour, what you'll likely find is that the powder has dissolved into a puddle that's easily removed with a pipette. If it hasn't dissolved, it turns into a paste like consistency and is easily decanted off.

It's actually looking like even that quantity of carbonate isn't enough to remove all the water in the solvent. I had one jar where I added more and more, and it kept pulling more water out. But at the rate I suggested, it is enough to solve issues with oiling out.

If using sodium carb, it won't dissolve like potassium carb does. Just add it in portions until the quantity you just added doesn't clump, let it sit a while, then decant.

merkin wrote:

*** EDIT :: approaching 48 hours ***

Spoke too soon about the crystals! OMG. This deceptively dark liquid hides a gazillion little starry clusters on the sides of the beaker. When larger they tumble in slow motion to the fluffy bottom below. The color of the red-purple is psychedelic, so is the green. Not the best pics I know - it's so hard to shoot pics holding phone and torch and juggling reflections on the glass. Looks like dirt but really it is a sparkling wonderland of crystal beauty and color. Unbelievable. A whole new experience and all from my garden! The Mesc Gods are smiling on me today saying thanks for 15+ years of dutiful propogation! Loveall, this is just beyond words. Move over Manske... Wow, Wow WOW.


Congrats! It's such a nice feeling to see those crystals! For me, drying the solvent had the extra benefit of making crystals form much more quickly. Definitely play around with that and see where it gets you Smile
 
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