TEK Ethyl acetate approach [CIELO]

[Loveall]

You can dry EA with sodium carbonate before salting. 0.3% forms a water layer.

 

[Brennendes Wasser]

So tomorrow I'll separate the goo and try recrystallizing in IPA. I only have 70% so I'll salt out and dry with sodium sulfate.

Maybe I would still try getting 99 % IPA. Not sure if this will be reliable, removing that much water with the sodium sulfate. Just recently I pulled with Acetone from a cactus paste, that was mostly dry, but still contained some water. I then dried the Acetone pulls with magnesium sulfate quite strongly, but then when evaporating all the Acetone, there was still a huge load of water remaining. In Lab work generally Sodium Sulfate is used after washing your NPS with NaCl-saturated water, that will already carry away most of the water in this first step - MgSO4 or Na2SO4 is then only used to get the last bits. So maybe drying 30 % water from IPA could also leave quite some water behind, which would make you loose your crystals :/ (if not evaporating).

 

[downwardsfromzero]

So tomorrow I'll separate the goo and try recrystallizing in IPA. I only have 70% so I'll salt out and dry with sodium sulfate.

Maybe I would still try getting 99 % IPA. Not sure if this will be reliable, removing that much water with the sodium sulfate. Just recently I pulled with Acetone from a cactus paste, that was mostly dry, but still contained some water. I then dried the Acetone pulls with magnesium sulfate quite strongly, but then when evaporating all the Acetone, there was still a huge load of water remaining. In Lab work generally Sodium Sulfate is used after washing your NPS with NaCl-saturated water, that will already carry away most of the water in this first step - MgSO4 or Na2SO4 is then only used to get the last bits. So maybe drying 30 % water from IPA could also leave quite some water behind, which would make you loose your crystals :/ (if not evaporating).

Acetone is pretty hygroscopic, IPA is too. Did you use a protected atmosphere during the evaporation? How many separate batches of MgSO4 did you use during the 'quite strong' drying? If these 'last bits' of water are substantial it may be necessary to dry the solvent again in a fresh container with fresh desiccant. It's a matter of gaining an advantage in the balance between the affinity that the solvent has for water, and the partial vapor pressure of the desiccant salt. There's an analogy with extraction here, in that one big batch does not equal two lots of half the size. Removal of the first lot of desiccant means that that portion of water is taken out of the equation entirely. The second round of desiccant then gets to pull a greater proportion of the remaining water.

The aldol condensation of acetone is at the back of my mind too, since this reaction produces water. It might well be catalysed by amines as much as by Lewis acids.

 

[modern]

So I was able to get a white precipitate from dissolving the goo in warm ISO that I dried. HOWEVER the alcohol that I have is likely not 99% since there is still a clear liquid that isn't flammable with the crystals that still hasn't evaporated. I'm not even sure if it is water to be honest I'll keep it in open air another day or two.

So I first added 1/4 volume salt to the 70% and shook well twice and let it sit for 2 hours. Then I siphoned the top layer didn't see a bottom layer but I assume it is 'under' the salt. I added enough sodium sulfate until it was free floating.

 

[Brennendes Wasser]

How many separate batches of MgSO4 did you use during the 'quite strong' drying?

So I just used 1 but a quite huge load of MgSO4. This was stirred for easily 1 h. As at the end the powder was still free floating instead of forming a solid brick, I was quite sure it did not absorb over-its-maximum and therefore the MgSO4 was enough to absorb all the water. Normally never had problems of remaining H2O, but then on the other hand these cases have mostly been with a brine wash before

The aldol condensation of acetone is at the back of my mind too, since this reaction produces water. It might well be catalysed by amines as much as by Lewis acids.

Wow that would be a quite exotic thing to happen, but sounds definetly possible

So I first added 1/4 volume salt to the 70% and shook well twice and let it sit for 2 hours. Then I siphoned the top layer didn't see a bottom layer but I assume it is 'under' the salt. I added enough sodium sulfate until it was free floating.

Sounds just like my case, also my salt was still free floating, so I assumed it was not over-loaded with water and therefore all the water gone. But I guess then also your IPA was not fully dry. That's why I said it might make sense to still get 99 % IPA or at least 95+ %.

Now the excess Citric Acid (if you have any, but probably likely in the goo) will be also trapped in the water. So when evaporating you will just get all the citric acid back into your crystals. But with some luck it might at least become solid, but chances are you still have a goo and then also with the same composition as before.

Maybe you could try what DF0 was recommending, if you cant get your hands on 99 % IPA:

Wait until all the water evaporated. Meanwhile add more dry MgSO4 or dry Na2SO4, stirring for 10 min or resting for 1 h, decant and repeat this 2-3 x. Maybe this can get all the water out, but just buying some 95+ % IPA will be more on the safe side.



PS: You were just fine not having 2 layers. The drying agent will bind the water inside of it's own structure = Absorption. You start with a dry salt - either Na2SO4 or MgSO4 - and then slowly absorb more water molecules onto the salt. They both have a different maximum of how much water they can bind, I think it was:

Na2SO4 x 12 H2O
MgSO4 x 8 H2O

So you see MgSO4 will bind less water in total, but actually it seems to absorb it faster, that is why some people in the lab prefer it, as you would then simply use a few more spoons. But for practical efforts there is not any real big difference.

 

[modern]

So there was some evaporation but not gone... I actually think that this liquid layer is the goo that has just become transparent after the cold iso wash. I ended up pouring off the liquid that had some white precipitate in it to a new glass and will allow the original pour to dry better.

I have purchased 99.6% iso (likely just 99%) which I'll have onhand for any future extractions and perhaps I'll try another ISO freeze to remove this liquid that doesn't seem to want to go away.

 

[downwardsfromzero]

Na2SO4 x 12 H2O
MgSO4 x 8 H2O

Bear in mind that these sulfates have a couple of differrent hydrates depending on the ambient temperature. In the case of sodium, it's actually the decahydrate that is the maximum degree of hydration, occurring of course at and below the lowest inflection of the solubility curve. There's a heptahydrate that's unstable in the presence of liquid water but it may well play a rôle in nonaqueous systems.

[Edit: OK, that doesn't show up - I'll see if I can sort this out.]
And here's a diagram which nicely shows how the hydration enthalpy of sodium sulfate decahydrate varies with temperature:

[Edit: and that doesn't show up either...]
I'm not entirely sure how much use it is to us here though :lol:
Here's another diagram to help sustain the illusion that I'm of any use:

It does come with some context (but not that much).

The stable form of fully hydrated magnesium sulfate at STP is the heptahydrate, although it does form an undecahydrate at fridge temperatures. The phase diagram is even more complicated as there are a couple of intermediate hydrates stable at various temperatures:

The main thing I can take away from this is that Epsom salts would be absolutely useless as a deicer :lol:

While we're at it, here's a nice phase diagram of the sodium carbonate x-hydrates vs. sodium bicarbonate:

 

[merkin]

Wow :shock: this chemistry stuff gets pretty complex! Kinda relieved somehow that I only failed with CIELO my first time really, before goo was a thing Not sure why but mixing the lime with water before adding to cactus powder and the fridge rest/decant changed it all for me. Never had an issue once thereafter. I just love the absolute simplicity of CIELO and the beauty of the process and product and super grateful it works for me.

 

[Loveall]

Wow :shock: this chemistry stuff gets pretty complex! Kinda relieved somehow that I only failed with CIELO my first time really, before goo was a thing Not sure why but mixing the lime with water before adding to cactus powder and the fridge rest/decant changed it all for me. Never had an issue once thereafter. I just love the absolute simplicity of CIELO and the beauty of the process and product and super grateful it works for me.

The system EA, water, mescaline, and citric acid is interesting, hopefully someone studies it formally someday.

I agree, if the TEK is followed properly with the correct materials, xtals precipitate reliably.

xtals also appear under some variations of the fridge rest (70F to 40F, which decreases water content from 2.9 to 2.3%) and decant:

- Freeze, filter ice, and add 1% water.
- Add 0.3% Na2CO3 and decant the layer that forms
- Add 250ml of dry EA per 1000ml of extract (in theory since 2.9/(1000+250) ~ 2.3, has anyone done this?)
- Extract with cold EA salting at a warmer temperature

Interestingly goo has formed under the following conditions:

- Too much water (presumably beginers' poor decanting)
- Too little water, if for example ice is filtered and no water added. Interestingly, after adding some water (5ml or roughly 0.5%), this goo changed into xtals according to one report.
- Not enough excess citric acid

So there could be different goo sources (?). There seems to be a phase diagram where xtals form inside a certain % water window after a minimal % citric acid excess. Outside of that, goo precipitates instead of xtals. Both goo and xtals are a mixture of mescaline, citric acid, and water. Xtals have 1:1;1
5 molecular ratio (respectively). General goo has different ratios tending to have more citric acid and water than the xtals.

 

[Loveall]

I'll redo it with 20-25% EtAc next time to see if it works. Anything over that amount might be too much to make it worth while. And the fridge step might be best option.

I wanted to try drying with sodium sulfate but at the moment I forgot I had it and didn't use it.

Ok, remember that the fridge rest and decant reduces water content from 2.9 to 2.3%.

For perfectly dry EA, you need 250ml per 1000ml of extract to replicate this drop. If the EA is not dry (say 99%), then 450ml would be needed. Unless my math is wrong...

 

[modern]

So after using the 99+% iso (made a difference) I got .038g from 4.188 starting so .9%. I added what passed the filter paper and the iso to the freezer and might get a little more but I doubt enough to change the final weight.

Pretty good for my first run and I think the ethylene vs control showed a massive difference since there was zero precipitate from the same materials used on the two.

I'll be using ceilo for micro extractions. But I think I'd have trouble using under 3.5 grams starting material. Anyone have link of photos some mirco extractions? someone mentioned 1g extractions which is awesome but I wouldn't be able to weight it.

 

[Loveall]

so you recovered xtals after 99% ISO?

In the future you should get xtals right away from EA if doing the TEK whith good materials and technique.

 

[modern]

Yea. I got a goo since I skipped the fridge rest so likely had water still.

I got a precipitate from my 'dry 70% iso' but there was still water since it never dried after 2-3 days. There was still a goo. Once I used my 99% iso I filtered and the white crystals were dry very quickly after it evaporated.

There is a small amount of iso in the fridge to see if I can rescue some more but likely have most.


I'm getting a manual coffee grinder so I can start with a powder and I'll do the fridge rest or freezer step since I skipped it last time likely the cause of the goo.

 

[navegandouniversos]

hello friends!
After a few weeks of absence here in the nexus, I come to tell you that I got my first extract of beautiful and big needles:d !!!!

1 exact gram obtained from 100 grams of nopal (T.pachanoi)
I am flying with joy to see these beauties, and knowing that soon, I will test them, a few days later, I am still very soft after a deep iboga shot...

I wish everyone here the best in your lives and once again express my gratitude and appreciation for your kindness and commitment to the psychedelic world:grin:
Hugs!

 

[Loveall]

hello friends!
After a few weeks of absence here in the nexus, I come to tell you that I got my first extract of beautiful and big needles:d !!!!

1 exact gram obtained from 100 grams of nopal (T.pachanoi)
I am flying with joy to see these beauties, and knowing that soon, I will test them, a few days later, I am still very soft after a deep iboga shot...

I wish everyone here the best in your lives and once again express my gratitude and appreciation for your kindness and commitment to the psychedelic world:grin:
Hugs!

so this is different from Trichocereus Terschekii, right?

Nopal is called San Pedro in Argentina? In the US nopal is a different cacti.

Any news in your Trichocereus Terschekii extractions would be great

Enhora burena obteniendo estrallas blancas despues de aclararse las nubes en el cielo, San Pedro esta contento.

 

[navegandouniversos]

Hi loveall,

Yes this is different, was T. pachanoi that i used, i didn't try again with Terschekii, ( in Argentina it's called with some many diferent names, Wachuma, Wachumita, Achuma, Abuelo, San pedro with the influence of the Colonos), but, probably this tays i'll do it again with Terschekii, and for sure report the results

The Terschekii extract that i made, was a goo situation!, so i did a re-x with IPA, and looks like an oily light amber powder, What you think about one more IPA re-x ??

Thanks so much !

Hugs!!

 

[Loveall]

Hi loveall,

Yes this is different, was T. pachanoi that i used, i didn't try again with Terschekii, ( in Argentina it's called with some many diferent names, Wachuma, Wachumita, Achuma, Abuelo, San pedro with the influence of the Colonos), but, probably this tays i'll do it again with Terschekii, and for sure report the results

The Terschekii extract that i made, was a goo situation!, so i did a re-x with IPA, and looks like an oily light amber powder, What you think about one more IPA re-x ??

Thanks so much !

Hugs!!

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

Sometimes people do the TEK better the second time around after some practice.

If you did the process the same way, and Terscheckii gives goo and there is still some goo even after IPA re-X, it could be due to the methylated mescaline precipitating not as xtals. I would try to precipitate Terscheckii with fumaric acid next time.

 

[Brennendes Wasser]

... 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.

 

[navegandouniversos]

[=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]

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.