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Ethyl acetate approach [CIELO] Options
 
Brennendes Wasser
#1341 Posted : 2/14/2023 9:49:26 PM

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Sadly NMR would not be able to tell the difference if it's either from the solvent or from the crystals.

But here is an easy way to find out:

1. Dry Ethyl Acetate COMPLETELY (wash with saturated NaCl solution -> let it rest with Mol Sieve [heated to dryness at > 100 °C for 5 h] or stirr in MgSO4)

2. Precipitate crystals, scrape and put them inside of a CaCl2-drying chamber (complexed water will not be removed, only last traces of Ethyl Acetate pollution)

3. Measure your NMR in the solvent of choice WITHOUT any analyte and track down the Intensity of the water peak (4,79 ppm in D2O, 3,3 ppm in DMSO)

4. Measure NMR of Mescalin Citrate from drying chamber and see if you still get a H2O peak

5. Compare intensity from Y-Axis of Water Peak (normally Y-Axis is something you never care about in NMR) with the one measured in 3.

Is there a water signal?
No = 6 % water was just from not perfectly dried EA
...
Yes:
Is there a water signal in your solvent?
No = water was complexed in Mescalin Citrate
...
yes:
What is the ratio of intensity of 3. and 4.?

in 3. it was much lower = water was from Mescalin Citrat
in 3. it is roughly the same intensity = water was from solvent and not from Mescalin Citrat

With those quick steps I guess it could be verified if Mescalin Citrate forms a Hydrate. But that would be quite likely, many products from pharmaceutical industries are given their melting point on Wikipedia as Freebase and often Chloride x 1 H2O (or more) so it is quite a common thing and if the Mescalin product is crystalline, then it should not make any problems at all I guess.
 

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Loveall
#1342 Posted : 2/15/2023 2:10:54 AM

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Wow, OK, that sounds very involved 😬

Not sure if it is a clue, but under very dry conditions CIELO Xtals don't like to form. A couple drops of water and it clouds up like crazy. Same can happen for DMT in Ethyl Acetate.

I updated the preliminary NMR calculated purity to 93.1% in the TEK. Thanks endlessness!
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Brennendes Wasser
#1343 Posted : 2/15/2023 8:00:15 AM

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Ah ok but then step 1 could be also skipped, because step 2 would then again remove any water that got inside "by accident" and it not part of any real complexed water hidden inside the crystal grid. Thumbs up
 
Loveall
#1344 Posted : 2/21/2023 11:52:12 AM

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Loveall wrote:
Thanks endlessness/BW.

Could there simply be water in the xtaline structure? Could the product simply be monomescaline citrate (mono/di)ydrate?

For example how would the NMR look for mescaline sulfate dihydrate? Can you see a difference between water "contamination" and water as part of the natural salt?


Hydrate xtals molecules can have half a molecule of water (shared), so perhaps the product we are looking at is,

Mes(โ†‘) + H3Cit(โ†‘) + 1.5H2O โ‡’ (MesH)H2Cit·1.5H2O(โ†“)


With the notation mentioned in the Wiki. This matches endlessness' result result of 49% mescaline.

Would need repeat of the NMR results and verify that the water is not a contaminant.

I've tentatively updated the xtalization precipitation reaction in the WIKI to this.

The hydration would imply that instead of 61% as strong as MesHCl by weight, our product is 57% as strong.


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Twilight Person
#1345 Posted : 2/22/2023 2:37:54 PM

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I see all traditional methods use Ca(OH)2.

But why we dont use Na2CO3?

It is a weaker base and also strong enough for Mesc I guess?

But maybe it will not deprotonate the HO-R Alkaloids and it looks like there are quite many in those cacti. Maybe then the spectrum and experience would be more enriched, like what people claim for cactus tea?

Ca(OH)2 has a pretty bad solubility in water, is that important? Other than that I see no real difference, just carbonates being weaker bases.
~ O ~
 
Loveall
#1346 Posted : 2/22/2023 3:56:15 PM

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Twilight Person wrote:
I see all traditional methods use Ca(OH)2.

But why we dont use Na2CO3?

It is a weaker base and also strong enough for Mesc I guess?

But maybe it will not deprotonate the HO-R Alkaloids and it looks like there are quite many in those cacti. Maybe then the spectrum and experience would be more enriched, like what people claim for cactus tea?

Ca(OH)2 has a pretty bad solubility in water, is that important? Other than that I see no real difference, just carbonates being weaker bases.


Paste made with Na2CO3 becomes gooey quickly and is not loose/sandy. Makes it hard for the ehtyl acetate to get into the paste and extract mescaline effectively.
💚🌵💚 Mescaline CIELO TEK 💚🌵💚
💚🌳💚DMT salt e-juice HIELO TEK💚🌳💚
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Twilight Person
#1347 Posted : 2/22/2023 4:57:55 PM

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Ok I see!

Now when comparing both the really low solubility of Ca-Salts comes in mind.

Is there any chance to try it with CaCO3?

If that shares the same consistency with Ca(OH)2 then maybe could be an option to keep more actives?
~ O ~
 
Loveall
#1348 Posted : 2/22/2023 6:20:32 PM

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Twilight Person wrote:
Ok I see!

Now when comparing both the really low solubility of Ca-Salts comes in mind.

Is there any chance to try it with CaCO3?

If that shares the same consistency with Ca(OH)2 then maybe could be an option to keep more actives?


Maybe? I don't know. I would worry it may not give a high enough pH. I never tried it but you can if you want.
💚🌵💚 Mescaline CIELO TEK 💚🌵💚
💚🌳💚DMT salt e-juice HIELO TEK💚🌳💚
💚🍃💚 Salvinorin Chilled Acetone with IPA and Naphtha re-X TEK💚🍃💚
 
Toshido
#1349 Posted : 3/6/2023 10:45:59 PM

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How can I tell if my Citric Acid is Monohydrate or Anhydrous? Any way to tell without testing it with Ethyl Acetate? I have some citric acid but it doesn't specify.

Also, is food grade Calcium Hydroxide (pickling lime) ok to use?
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🙌 "Dang, that's really impressive for a first extraction. Those xtals are nicely resolved." - Benzyme 🙌

 
Loveall
#1350 Posted : 3/6/2023 11:38:33 PM

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It doesn't matter if the citric acid is anhydrous. This is because there will be 2.5% water after the fridge rest, and that will wet anhydrous acid if present (may take a little longer to dissolve).

Food grade Calcium Hydroxide is good to use 👍
💚🌵💚 Mescaline CIELO TEK 💚🌵💚
💚🌳💚DMT salt e-juice HIELO TEK💚🌳💚
💚🍃💚 Salvinorin Chilled Acetone with IPA and Naphtha re-X TEK💚🍃💚
 
Toshido
#1351 Posted : 3/6/2023 11:45:41 PM

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Loveall wrote:
It doesn't matter if the citric acid is anhydrous. This is because there will be 2.5% water after the fridge rest, and that will wet anhydrous acid if present (may take a little longer to dissolve).

Food grade Calcium Hydroxide is good to use 👍


Thank you. I saw that Endlessness used CASEA (Citric Acid Saturated Ethyl Acetate) that he simply added to his pulls. So I guess I will just test it out first.
🌳👨โ€🔬🌳 - My A/B Hot Plate TEK - 🌳👨โ€🔬🌳
🍜🍜🍜 - Don't Heat Your Naphtha, Heat Your Soup! - 🍜🍜🍜
โœดโœดโœด - White Spice vs Yellow Spice - 🌟🌟🌟
"You are an explorer, and you represent our species, and the greatest good you can do is to bring back a new idea, because our world is endangered by the absence of good ideas. Our world is in crisis because of the absence of consciousness." - Terence McKenna
🙌 "Dang, that's really impressive for a first extraction. Those xtals are nicely resolved." - Benzyme 🙌

 
Loveall
#1352 Posted : 3/6/2023 11:58:07 PM

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widderic wrote:
Loveall wrote:
It doesn't matter if the citric acid is anhydrous. This is because there will be 2.5% water after the fridge rest, and that will wet anhydrous acid if present (may take a little longer to dissolve).

Food grade Calcium Hydroxide is good to use 👍


Thank you. I saw that Endlessness used CASEA (Citric Acid Saturated Ethyl Acetate) that he simply added to his pulls. So I guess I will just test it out first.


If you want to use CASEA, then it does matter. When preparing CASEA using dry entyl acetate and anhydrous citric acid you may need to add 2% water to get the citric acid to dissolve.
💚🌵💚 Mescaline CIELO TEK 💚🌵💚
💚🌳💚DMT salt e-juice HIELO TEK💚🌳💚
💚🍃💚 Salvinorin Chilled Acetone with IPA and Naphtha re-X TEK💚🍃💚
 
Toshido
#1353 Posted : 3/7/2023 3:25:16 AM

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Loveall wrote:

If you want to use CASEA, then it does matter. When preparing CASEA using dry entyl acetate and anhydrous citric acid you may need to add 2% water to get the citric acid to dissolve.


Oh ok great thanks for letting me know in case I run into that issue. As for dry ethyl acetate... what makes it.... dry? As I am using MEK Substitute as stated in the TEK which is 100% ethyl acetate.
🌳👨โ€🔬🌳 - My A/B Hot Plate TEK - 🌳👨โ€🔬🌳
🍜🍜🍜 - Don't Heat Your Naphtha, Heat Your Soup! - 🍜🍜🍜
โœดโœดโœด - White Spice vs Yellow Spice - 🌟🌟🌟
"You are an explorer, and you represent our species, and the greatest good you can do is to bring back a new idea, because our world is endangered by the absence of good ideas. Our world is in crisis because of the absence of consciousness." - Terence McKenna
🙌 "Dang, that's really impressive for a first extraction. Those xtals are nicely resolved." - Benzyme 🙌

 
Loveall
#1354 Posted : 3/7/2023 8:53:15 PM

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widderic wrote:
Loveall wrote:

If you want to use CASEA, then it does matter. When preparing CASEA using dry entyl acetate and anhydrous citric acid you may need to add 2% water to get the citric acid to dissolve.


Oh ok great thanks for letting me know in case I run into that issue. As for dry ethyl acetate... what makes it.... dry? As I am using MEK Substitute as stated in the TEK which is 100% ethyl acetate.


It is pretty dry out of the can. If exposed to water it reaches equilibrium at ~3% water at room temp and ~2.5% at fridge temp. After it absorbs water it can be dried again by one of several methods, but that is not needed for this TEK.
💚🌵💚 Mescaline CIELO TEK 💚🌵💚
💚🌳💚DMT salt e-juice HIELO TEK💚🌳💚
💚🍃💚 Salvinorin Chilled Acetone with IPA and Naphtha re-X TEK💚🍃💚
 
Toshido
#1355 Posted : 3/8/2023 9:36:09 AM

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Loveall wrote:

It is pretty dry out of the can. If exposed to water it reaches equilibrium at ~3% water at room temp and ~2.5% at fridge temp. After it absorbs water it can be dried again by one of several methods, but that is not needed for this TEK.


So free of water, makes sense. Thank you for clarifying! My brain is swollen from all of the learning in the last few months haha. Not a bad thing.
🌳👨โ€🔬🌳 - My A/B Hot Plate TEK - 🌳👨โ€🔬🌳
🍜🍜🍜 - Don't Heat Your Naphtha, Heat Your Soup! - 🍜🍜🍜
โœดโœดโœด - White Spice vs Yellow Spice - 🌟🌟🌟
"You are an explorer, and you represent our species, and the greatest good you can do is to bring back a new idea, because our world is endangered by the absence of good ideas. Our world is in crisis because of the absence of consciousness." - Terence McKenna
🙌 "Dang, that's really impressive for a first extraction. Those xtals are nicely resolved." - Benzyme 🙌

 
endlessness
#1356 Posted : 3/16/2023 7:35:32 PM

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Got my best yield yet, 2.4% !

It was from a mix of cact (whole cact, spines, core and all), there was maybe 70% of some cact I had extracted from before and had gotten 1% yield, but it was a couple of pieces that were cut during winter and didn´t heal/scar properly so they were rotting near the cut.. The other 30% was a bridgesii I hadnt extracted before. So either rotting cact creates more mesc and/or my bridgesii has a crazy high yield...

Also, it was with reused ethyl acetate, and I made the whole extraction in like 10 mins of work plus some waiting, was crazy simple and easy.

I also didn´t want to wait for the fridge step overnight duration so what I did instead is to put the ethyl acetate in the freezer for a couple of hours until there was some frozen water slush in the ethyl acetate, then I took it out of the freezer and let it stand in room temperature for half an hour or so until the ice slush had melted and there was a water puddle on the bottom of ethyl acetate, so I just decanted the ethyl acetate away from that and used to make the pulls.

I did very quick pulls and then crystallized by dumping Citric Acid Saturated Ethyl Acetate (CASEA) that had about 10g citric acid into the 1L mescaline-laden ethyl acetate and let it crystallize overnight. Prob because of the reused ethyl acetate I got a mix of different types of crystals, some fluffy needles mixed with some more amorphous crystals, as seen below:

 
famine
#1357 Posted : 3/16/2023 11:57:43 PM

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endlessness wrote:
Got my best yield yet, 2.4% !

It was from a mix of cact (whole cact, spines, core and all), there was maybe 70% of some cact I had extracted from before and had gotten 1% yield, but it was a couple of pieces that were cut during winter and didn´t heal/scar properly so they were rotting near the cut.. The other 30% was a bridgesii I hadnt extracted before. So either rotting cact creates more mesc and/or my bridgesii has a crazy high yield...

Also, it was with reused ethyl acetate, and I made the whole extraction in like 10 mins of work plus some waiting, was crazy simple and easy.

I also didn´t want to wait for the fridge step overnight duration so what I did instead is to put the ethyl acetate in the freezer for a couple of hours until there was some frozen water slush in the ethyl acetate, then I took it out of the freezer and let it stand in room temperature for half an hour or so until the ice slush had melted and there was a water puddle on the bottom of ethyl acetate, so I just decanted the ethyl acetate away from that and used to make the pulls.

I did very quick pulls and then crystallized by dumping Citric Acid Saturated Ethyl Acetate (CASEA) that had about 10g citric acid into the 1L mescaline-laden ethyl acetate and let it crystallize overnight. Prob because of the reused ethyl acetate I got a mix of different types of crystals, some fluffy needles mixed with some more amorphous crystals, as seen below:


Dry your ethyl acetate before freezing just... Shocked
 
Orion
#1358 Posted : 3/17/2023 3:33:19 AM

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Well... this thread took forever to read through but it was worth it. There is some seriously thorough work in these pages! I'll definitely be trying this.

Endlessness, nice crystal assortment. You mentioned freezing and I wonder: could the ethyl acetate not be poured away from the ice ? Is there a reason to allow it to thaw first ?

EDIT: For the sake of growing crystals for fun before any harvests, what would be a good way to test converting HCl to citrate using this method ? Half a gram for example. Add water, base with lime, dry, pull with ethyl acetate and proceed as normal ?
Art Van D'lay wrote:
Smoalk. It. And. See.
 
Quetzal7
#1359 Posted : 3/17/2023 7:39:10 AM

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I'm getting ready to try that tek soon =) =)

Question : did anybody tried to put fresh cactus in the blender and add to lime to it directly?

I remember adding lime to dry cactus powder (Q21 tek kind of approach) and making the opposite as what is describes here : it got goey really really fast, but 2 days after, the texture changed completly and it was sandier (but not sandy sandy, still has some elasticity to it)

While , as a test, i put fresh cactus in the blender and lime, it was much much better texture imho =)
(but i didn't tried to pull, it was just information... you know... casuality making cactus-lime smoothies with the vitamix... )
 
endlessness
#1360 Posted : 3/17/2023 8:06:58 AM

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famine wrote:
]
Dry your ethyl acetate before freezing just... Shocked


This was tried already before by Loveall and others and drying your ethyl acetate with magnesium sulphate for example will interfere with crystallization and result in lower yields. One possibility is that the mescaline citrate is crystallized as monohydrate and it needs some of the extra water for proper crystallization, so a fully dried solvent isnt wanted in this case. I haven´t tested this in a side by side experimentally (would of course be interested if anybody does) but I have extracted and crystallized mescaline several times now with the Ethyl acetate containing water within these acceptable ranges and it works perfectly. As they say, don´t change a winning team Very happy

Orion wrote:
Well... this thread took forever to read through but it was worth it. There is some seriously thorough work in these pages! I'll definitely be trying this.

Endlessness, nice crystal assortment. You mentioned freezing and I wonder: could the ethyl acetate not be poured away from the ice ? Is there a reason to allow it to thaw first ?

EDIT: For the sake of growing crystals for fun before any harvests, what would be a good way to test converting HCl to citrate using this method ? Half a gram for example. Add water, base with lime, dry, pull with ethyl acetate and proceed as normal ?


Orion, I didnt pour away/filter the ice because I didn´t want to remove too much water that potentially would interfere with crystallization later on. Also I am not sure of the solubility of mescaline in Ethyl Acetate at freezing temperatures so I was worried that some of the mescaline might have separated from ethyl acetate and be filtered away. One could of course test this easily experimentally but I didn´t want to do a side by side, I just wanted to make sure I got all my mescaline in a short time, so I figured that would be the easiest way.

And yeah I think you could convert your HCl to citrate that way. If you add just enough water for the HCl to dissolve, when you add lime it will already be quite dry so you can pull with ethyl acetate straight away without having to dry it. And a bit of extra water shouldn´t be a problem in any case as mentioned above, specially if you do a fridge (or quick freeze and thaw) step to get the water content to that acceptable range.
 
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