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Ethyl acetate approach [CIELO] Options
 
Brennendes Wasser
#1641 Posted : 10/17/2023 4:39:17 PM

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Quote:
... was a goo situation!, so i did a re-x with IPA, and looks like an oily light amber powder


Also another thing to consider, I have read also people doing the re-x, but then speaking of "after evaporation" and this sounds like they simply dissolved their goo in boiling IPA and then waited for the IPA to fully evaporate.

This step is not just a way to crystallize it - like you would do with brown DMT oil to white crystals - but instead it will get rid of (potential) excess citric acid too. So if you did the IPA re-x, but did not do a freezer-decanting, then you are most certainly ending up with oily amber material again. The amber colour to me would also suggest again citric acid inside your final product, instead of pure mescaline citrate. So if you did an evaporation instead of freezer-decanting you could try again if this is not originating from using a more exotic plant here.
 

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navegandouniversos
#1642 Posted : 10/18/2023 8:11:24 PM

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[=Did you do the process the way same way when you did it between Pachanoi and Terschekii?]

yes loveall , i did it in the same way for both of them

why fumaric acid ?? have a different reaction than citric acid with water ??


[= So if you did an evaporation instead of freezer-decanting you could try again if this is not originating from using a more exotic plant here.]

thank you BW, the re-x was first with hot ipa, and then freezer-decanting yes .. that was with Terschekii
 
Loveall
#1643 Posted : 10/18/2023 11:34:15 PM

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navegandouniversos wrote:
Loveall wrote:
Did you do the process the way same way when you did it between Pachanoi and Terschekii?


yes loveall , i did it in the same way for both of them

why fumaric acid ?? have a different reaction than citric acid with water


Fumarates may be less hydroscopic than citrates, so they may be able to give xtals even for the possible n-methylated mescaline that you may be getting from Terscheckii.
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Brennendes Wasser
#1644 Posted : 10/19/2023 10:13:20 PM

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Quote:
thank you BW, the re-x was first with hot ipa, and then freezer-decanting yes .. that was with Terschekii


Oh well then maybe the goo was not by excess citric acid remaining ... I believe this step should remove any, although there is no proof yet. But maybe it is because of using this non-classical cactus?
 
navegandouniversos
#1645 Posted : 10/19/2023 10:34:08 PM

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Quote:
Oh well then maybe the goo was not by excess citric acid remaining ... I believe this step should remove any, although there is no proof yet. But maybe it is because of using this non-classical cactus?


Maybe it's because the big Terschekii Big grin , I`ll try with fumaric acid soon, like Loveall mentioned ..

Quote:
Fumarates may be less hydroscopic than citrates, so they may be able to give xtals even for the possible n-methylated mescaline that you may be getting from Terscheckii.


Thanks man, I`ll try with fumaric soon, I'm curious with my dear abuelito Big grin
 
modern
#1646 Posted : 10/24/2023 10:25:25 PM
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So since I didn't follow the tek I once again got goo. I dried excessively with sodium sulfate and got a sticky dark goo. So I added water to try and get crystals but it didn't work and I got the transparent goo again. When trying to fix the goo this time I heated the 99 iso on a hotplate and got a precipitate and reduced the volume a bit since I put excess. I allowed it too cool and it redissolved into the solution. So I then covered it and put it in the freezer. After some 4+ hours the solution was completely clear and nothing salted out. I was about to give up but once the iso solution started to warm up to ambient temperature the color became orange tint of the goo and slowly started to form particulates. After 1 hour sitting and at ambient temperature there is a precipitate that formed.

modern attached the following image(s):
IMG_5599.JPG (1,802kb) downloaded 221 time(s).
IMG_5659.JPG (1,377kb) downloaded 221 time(s).
IMG_5665.JPG (1,290kb) downloaded 220 time(s).
 
Twilight Person
#1647 Posted : 10/24/2023 10:59:48 PM

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So I only tried with etoh which probably still is quite the same in terms of solubility. But man this is way too much that you used Surprised just cover your goo with a little more etoh (so iproh should be same) and heat it to boil while stirring. It should be just that much, that you can still decant something. So if you use too little, the liquid with all the other stuff is hard to be decanted. So just use as much that you are sure you will be able to decant stuff, even when crystals will be forming and growing within that liquid, which would make it hard decanting if liquid is too less. But therefore this was over the top Crying or very sad

Now after crystals stop growing maybe still transfer it to another glas and keep on evaporating it, but of course not to 0%, leave a little that you can still decant to get rid of any potential water or CA so maybe you will get some more stuff.
~ O ~
 
modern
#1648 Posted : 10/24/2023 11:23:11 PM
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The volume of the iso is because I joined all 3 vessels into one since I was gonna evaporate it all. Due to the small scale of the extraction anything under 2-3ml is too small an amount.

The first time I did this with the goo the crystals formed from freezer rest however this time it is very soluble in cold iso. And last time when I heated the iso/goo it just became transparent and where this time it precipitated when heated.

At first I thought it was DNA but that usually precipitates when in COLD iso not boiling.

This is behaving the exact opposite of how it should no?
 
Twilight Person
#1649 Posted : 10/25/2023 8:21:09 AM

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Sounds unusual but well if the result looks crystalline i guess there is not much to worry about Razz just make sure to decant the very last bit instead of full evaporation.
~ O ~
 
Loveall
#1650 Posted : 10/25/2023 1:37:59 PM

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Yes it sounds opposite.

I would put it back in the freezer now that it is precipitating. Give it time (a few days). Xtalization likes time, it should all crash eventually.
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modern
#1651 Posted : 10/25/2023 2:39:09 PM
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Loveall wrote:
Yes it sounds opposite.

I would put it back in the freezer now that it is precipitating. Give it time (a few days). Xtalization likes time, it should all crash eventually.


I decanted and put the orange iso into the freezer and I'll leave it there for a few days... There were a lot of crystals that crashed out in the ambient temperature solution. I'll share some pictures later. Very pretty needles with a jewelers microscope
 
modern
#1652 Posted : 10/25/2023 4:52:15 PM
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So the still wet crystals ended up forming a goo again. I added isopropanal again and will try to decant once more. Same as last time the crystals precipitate in ambient temperature. This time when decanting I'll keep the crystals in this small beaker if it goes to goo again I'll preform a nano extraction again basing pulling again.

EDIT: There are two different crystals types. One that is soluble in cold iso and one that precipitates in cold iso. I think the precipitate that crashed in ambient temps is some sort of sodium sulfate contamination? The bottom photo is from ambient temps in the iso.
modern attached the following image(s):
IMG_5671.JPG (1,707kb) downloaded 179 time(s).
 
Brennendes Wasser
#1653 Posted : 10/26/2023 9:41:32 PM

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I also observed 2 types of crystals from ISO rex, but only at freezing temperatures ... that is what I called the rock chunks that form at the bottom and which are easy to decant from IPA and the very fine snow that will be too fine for decanting and requires filtering. But both only came in freezer Surprised Anyways if you only got Mescaline Citrate / CA / Water then any crystals can only be the true Mescaline Citrate, so hopefully it's just fine?

About Sodium Sulfate I would really say no. In general you can say it being like this:

REX vom NPS: used for Freebase-Alkaloid, Salts from Alkaloids + low-polarity organic acids (boiling Heptane even dissolves a very small amount of DMT-Benzoate) but no Alkaloids + mineral acids (*HCl, *H2SO4, ...)

REX vom Alcohols (MeOH, EtOH, IPrOH, Butanol): used for Salts from Alkaloids + organic acids, Salts from Alkaloids + mineral acids (*HCl, *H2SO4, ...) but no Freebase-Alkaloids (will not precipitate)

So you see when using a solvent which is very non polar (Toluene to Heptane) you can rex at maximum a salt which has 2 components that are organic molecules.

When using a solvent which has 1x R-OH (even lower polarity like Butanol) you can rex at maximum a salt which has 1 component that is inorganic (like anion = Cl-). But in order to dissolve and precipitate a salt which has 2 components that are inorganic (like Na+ OH-) it is still not enough. Only a few examples still dissolve in alcohols, like KOH partially.

Therefore 2Na+ SO4(2-) would probably not even dissolve in hot IPA. But in any way, a simple rule how you can start with REX if you dont know much about polarity:

Freebase = NPS like Heptane
Salt from Freebase + low-polarity acid = NPS like Toluene
Salt from Freebase + high-polarity acid = (any aliphatic) Alcohol


Citric acid is super polar, so only IPA will work, as solubility in EA (already very polar) is still pretty much 0.
 
Brennendes Wasser
#1654 Posted : 11/10/2023 5:27:04 PM

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Apparently there is quite a little water in the crystals, as Endlessness found like 7 % water via NMR. Also the crystallization does not work if 0 % water is present - well the same amount of precipitate was at least formed in a test I did, but it was just a white coating across the glass. In any way the crystals also contain some water, so I wanted to make a small experiment.

Is that water strongly bound and part of the crystal structure or just like an artefact from crystal formation, that can be removed with force?

85,50 mg Mescaline Citrate in Oven @ 50 °C / 0,04 bar for 24 h

weight afterwards ...

84,57 mg Mescaline Citrate

so even hardcore physico-chemical water removal did not do anything, must be totally locked within the crystal grid.

Could also just verify a little more quantitative by NMR, but I already have no access to any analysis method anymore and the one at my Friend's place is still broken Rolling eyes .
 
Twilight Person
#1655 Posted : 11/14/2023 11:32:19 AM

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Good news! If you remember I tried some CIELO and miserably failed as i constantly posted pictures from goo. Then i tried this etoh rex method (or ipa as it now seems better??) and at least got some solid stuff to work with... But still not pretty happy as the marvelous CIELO crystals make up 50% of the reward and that white chunks are just not as nice.

So while my cacti are now sleeping i took that one who was still awake (the white thing, remember?) and slashed him to powder...

Just tried a different way of water removal which was FREEZER. I know the tek says freezer removes too much water, but well i had nothing to loose and after filtering off the diffuse ice that is formed and threw the citric inside, voila = the true CIELO crystals formed.

I have no clue what is the reason, maybe something wrong with fridge or whatever, but probably from now will always go with 'freezer decant' as anything else gave goo. Just in case somebody else has same problem, maybe just try that 1x.

Cheers Love Love Love
~ O ~
 
modern
#1656 Posted : 11/14/2023 12:36:40 PM
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yea I have issue with crystalization... Maybe my fridge isn't cold enough?

Someone mentioned they do freezer and a Saturated citric acid EtOAc solution.

 
Twilight Person
#1657 Posted : 11/15/2023 6:12:33 PM

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Yes just also try freezer. For me it works now. I have 0 clue but i dont care as long as i will not have goo anymore Love if you already make a huge effort with the liquid-liquid extraction maybe just give that a try. Of course cacti powder is not for free, but you may at some point just make a tiny test during your next trials.

The ice is somehow diffuse and not frozen on the bottom as i thought

So dont decant, but let it flow through a funnel with a sneeze tissue inside, will run fast and still keep the ice in filter. Just remove it after all EA has made it s way through or it will slowly melt and get also back down. Can shake it a little bit to get all the EA through that is stuck in the diffuse ice, it s like 5-10% of whole EA at the end. Water removed must be even more than at 0°c in that table, as probably the 'mixability' is decreased even more when going to -20°c, though not 0% i guess(?). Not sure how much water truly stays behind but well for me it works so give it a try?
~ O ~
 
modern
#1658 Posted : 11/15/2023 8:23:52 PM
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Salt brine at 25g/100ml worked for me. I'll have to retry slightly higher salt content to see if any benefit. Only been 24 hours now but crystals look different. I don't wanna use the fridge since smell tends to 'leak'.
 
Orion
#1659 Posted : 11/25/2023 12:36:35 PM

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Last time I used this method to convert mescaline HCL at a fairly high concentration in solution and got goo. This time I used the cactus it was created from as per the usual tek. I it also created goo. When I checked the PH after adding the recommended amount of citric I noticed it was actually close to neutral. This is an important factor. I have added enough citric acid to get the PH up (confirmed with a PH paper) to see if it can crystalize the goo over time.

The cactus is a Bridgesii, some think it may be a lumberjack and it has always had quite high yields.

I think what might be happening for some people with high yielding cactus is that there is so much mescaline and the solution actually more alkaline than you think. Then when you add the citric acid you are crystalizing at too high of a PH and creating trimescalne citrate instead of monomescaline citrate. This is why PH testing is important.

I wonder if both trimescaline citrate and monomescaline citrate can be crystalized by an IPA re-x as some people have recently shown ? I feel like it's quite important to know as it affects dosages.
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Loveall
#1660 Posted : 11/25/2023 7:18:26 PM

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Orion wrote:
Last time I used this method to convert mescaline HCL at a fairly high concentration in solution and got goo. This time I used the cactus it was created from as per the usual tek. I it also created goo. When I checked the PH after adding the recommended amount of citric I noticed it was actually close to neutral. This is an important factor. I have added enough citric acid to get the PH up (confirmed with a PH paper) to see if it can crystalize the goo over time.

The cactus is a Bridgesii, some think it may be a lumberjack and it has always had quite high yields.

I think what might be happening for some people with high yielding cactus is that there is so much mescaline in solution that it is actually more alkaline than you think. Then when you add the citric acid you are crystalizing at too low of a PH and creating trimescalne citrate instead of monomescaline citrate. This is why PH testing is important.

I wonder if both trimescaline citrate and monomescaline citrate can be crystalized by an IPA re-x as some people have recently shown ? I feel like it's quite important to know as it affects dosages.


Agree that this could be happening if decanting was indeed done carefully. The goo from undersalting tends to be hard and doesnt move, while the goo from an improper fridge rest/decant flows more. Maybe we should simply update the TEK to salt with two teaspoons of citric acid?

During IPA re-X a pH strip may be informative. I'm going to guess that trimescaline citrate goo re-X will be neutral and mono-mescaline citrate re-X will be slightly acidic. If trimescaline citrate doesn't re-X well, adding citric acid before the cold step should crash the usual monomescaline citrate in cold acidic conditions, but not sure if a tiny bit of water will be needed or not (it is a hydrated salt in the usual TEK per NMR).

Overtime gardeners are going to keep on selecting the higher yielding cacti so doubling the teaspoons of citric acid may make it more future proof. This by the way is why citric acid is recommended, it has good solubility in EA and a huge process window for the lazy people among us who don't want to be bothered with careful measurments.
💚🌵💚 Mescaline CIELO TEK 💚🌵💚
💚🌳💚DMT salt e-juice HIELO TEK💚🌳💚
💚🍃💚 Salvinorin Chilled Acetone with IPA and Naphtha re-X TEK💚🍃💚
 
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