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?
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TEK Ethyl acetate approach [CIELO]
- Thread starter Loveall
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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
Esteemed member
Maybe it's because the big Terschekii
, I`ll try with fumaric acid soon, like Loveall mentioned .. Thanks man, I`ll try with fumaric soon, I'm curious with my dear abuelito
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.
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Twilight Person
Esteemed member
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 
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.
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.
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?
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
Esteemed member
Sounds unusual but well if the result looks crystalline i guess there is not much to worry about just make sure to decant the very last bit instead of full evaporation.
just make sure to decant the very last bit instead of full evaporation.
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 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.
Loveall said:
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
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.
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.
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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:
Citric acid is super polar, so only IPA will work, as solubility in EA (already very polar) is still pretty much 0.
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
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.
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 :roll: .
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 :roll: .
Twilight Person
Esteemed member
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
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
Twilight Person
Esteemed member
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 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?
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?
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.
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.
Orion said:
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.
modern said:
If smell tends to leak, you are not sealing the extrac. This could alow moisture into the extract and be the reason you are having issues here, or reddit, and on youtube. If that is also your xtalization vessel, your xtals could turn to goo overtime as moisture is absorbed from the atmosphere. I believe you have been told this repeatedly?
I'm assuming you are the guy with aluminum foil over beakers? That could be your issue. The TEK asked for sealed containers, specifically mason jars that can hold a vacuum.
I think the brine wash is likely to work. Not as lazy as a proper fridge rest in my opinion.
I like your ethylene gas idea by the way. Interested in your results once you figure out the TEK. I think not hermetically sealing your containers is giving you unnecessary headaches and causing you delays + extra work.
Yea I don't have any seal-able containers. You did mention that it needs to be sealed to prevent getting moisture from the air...
The salt brine does skip the need for me to do the fridge rest. The cielo tek is pretty easy for most but I've had issues even when doing fridge rest but maybe it was the lack of a seal container IDK. Also instead of an extra day fridge rest I can reduce it by a day.
I'll see if I can get an old olive or other container for it to be sealed to prevent other issues but mason jars besides not being readily available are not the cheapest here.
Also my balance isn't the best since it's pretty beat up so need to wait for larger cuttings to more accurately measure the results.
The salt brine does skip the need for me to do the fridge rest. The cielo tek is pretty easy for most but I've had issues even when doing fridge rest but maybe it was the lack of a seal container IDK. Also instead of an extra day fridge rest I can reduce it by a day.
I'll see if I can get an old olive or other container for it to be sealed to prevent other issues but mason jars besides not being readily available are not the cheapest here.
Also my balance isn't the best since it's pretty beat up so need to wait for larger cuttings to more accurately measure the results.
With some exprience over the years and dozens of cacti extractions, I have become convinced that the fridge rest is not needed if the paste is not too wet to begin with. I now believe that the ideal paste has just enough water to moisten the cactus powder with no dry spots. Any water beyond that, is not usefull and seems to be the cause of some beginners get5ing goo. Side note: it also seems helpfull to let the paste air out for a few minutes to allow the ammonia smell to dissipate.
There are several kind of paste after mixing well
- Too dry: some dry powder remains.
- Ideal: just enough water is added so all the cactus powder is wet. Consistensy is similar to play-doh. Fridge rest and decant is not needed, but it eont hurt.
- Accceptable: More water than ideal, but the paste can still hold its shape. Consistency is similar to moist mash potatoes. Fridge rest reccomended to avoid goo.
- Too wet: Paste is so wet it begins to not offer resistance to holding its shape (soggy mashed potatoe consitency or beyond). Fridge rest may not be enough to avoid goo. More extensive drying with a freezer or sodium carbonate step may be required (however, excessive drying can cause other issues such as sticky powder, hard goo, or no clouding reaction). If goo is obtained, 99% IPA re-X will recover xtaline product.
With an ideal paste, and by not undersalting (at least 5g citric acid per quart of extract), the process is very robust in my opinion.
I'm planning on updating the TEK soon. In particular, making it clear that the Ideal paste is preffered instead of the Acceptable one. Wondering if anyone has any feedback or different/alternative observations before that.
There are several kind of paste after mixing well
- Too dry: some dry powder remains.
- Ideal: just enough water is added so all the cactus powder is wet. Consistensy is similar to play-doh. Fridge rest and decant is not needed, but it eont hurt.
- Accceptable: More water than ideal, but the paste can still hold its shape. Consistency is similar to moist mash potatoes. Fridge rest reccomended to avoid goo.
- Too wet: Paste is so wet it begins to not offer resistance to holding its shape (soggy mashed potatoe consitency or beyond). Fridge rest may not be enough to avoid goo. More extensive drying with a freezer or sodium carbonate step may be required (however, excessive drying can cause other issues such as sticky powder, hard goo, or no clouding reaction). If goo is obtained, 99% IPA re-X will recover xtaline product.
With an ideal paste, and by not undersalting (at least 5g citric acid per quart of extract), the process is very robust in my opinion.
I'm planning on updating the TEK soon. In particular, making it clear that the Ideal paste is preffered instead of the Acceptable one. Wondering if anyone has any feedback or different/alternative observations before that.