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TEK Ethyl acetate approach [CIELO]

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Welcome to the cactus fluffy xtal party endlessness 🥰

I assume you decanted after the fridge and left some stuff behind?

Yes, we have found that anhydrous citric acid has difficulty dissolving in anhydrous EA. Theoretically it should dissolve, but you are right that there seems to be difficulty.

I think the TEK as is will work with anhydrous EA, because after the fridge rest the extract is still ~2% water. Coincidentally, that is what you ended up with CASEA.

Happy the CASEA worked so well ☺️ It could be re-assuring for anyone worrying about undissolved anhydrous citric acid. I don't think there it is an issue, but we do get questions about it from time to time.

Looking forward to lab test results 😀
 

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I have a little air destiller that I have used to provide me almost pure ethanol with addittion of a 3a molecular sieve and I was wondering if I can use it with Ethyl acetate. This device has a temperature controller. I know about the ethyl acetate flammable vapor, but with some caution I think maybe it can be used.

Any thoughs on this? Thanks

https://imgur.com/a/0URCSMz
 
Ethyl acetate has a very similar boiling point to that of ethanol. However, it might attack any plastic components so you'd best take a careful look at how your device is built. In your picture I would guess the black bit is ABS and the clear/blue lid of the jug is acrylic. Neither of these would last very long in the proximity of ethyl acetate.

If you can keep your distillate in an ice bath, and avoid the use of that lid, the black plastic cowl around the air intake might be ok, given the airflow keeps the bulk of the EA vapours moving away from it. There should be no plastic at all further downstream than this.

Other factors you might want to nerd out on are comparison of the latent heat of vaporization, the specific heat capacity, the viscosity, and the density of both the liquid and the vapour, for both ethanol and ethyl acetate. For starters, it's easy to tell that the vapour density of ethyl acetate will be nearly twice that of ethanol. Maybe that is slightly advantageous here, in the sense that it will sink away from the plastic.
 
downwardsfromzero said:
Ethyl acetate has a very similar boiling point to that of ethanol. However, it might attack any plastic components so you'd best take a careful look at how your device is built. In your picture I would guess the black bit is ABS and the clear/blue lid of the jug is acrylic. Neither of these would last very long in the proximity of ethyl acetate.

If you can keep your distillate in an ice bath, and avoid the use of that lid, the black plastic cowl around the air intake might be ok, given the airflow keeps the bulk of the EA vapours moving away from it. There should be no plastic at all further downstream than this.

Other factors you might want to nerd out on are comparison of the latent heat of vaporization, the specific heat capacity, the viscosity, and the density of both the liquid and the vapour, for both ethanol and ethyl acetate. For starters, it's easy to tell that the vapour density of ethyl acetate will be nearly twice that of ethanol. Maybe that is slightly advantageous here, in the sense that it will sink away from the plastic.
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Thanks for the reply, I wont use that jug of course..I never have used it in fact, just glass jars.
Thanks for the idea of ice bath the collected EA to avoid any fumes from it... I could use a peltier device instead ..but just try to avoid more electric components.

The inner chamber and the serpentine are both stainless steel and the EA fumes do no reach any plastic.. The holes of the lid are only the air intake for the fan that cool the serpentine.
 
The large seal ring between the distiller steel bowl and steel lid looks to be silicone from what I saw on amazon, like the kind you'd see on an electric pressure cooker lid. It's pretty thick but that might get some wear and tear with ethyl acetate.
 
starbob said:
The large seal ring between the distiller steel bowl and steel lid looks to be silicone from what I saw on amazon, like the kind you'd see on an electric pressure cooker lid. It's pretty thick but that might get some wear and tear with ethyl acetate.
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Yes, that was my main concern, but I read somewhere that EA is not agressive on silicone, at the other hand..in normal alcohol destilation, the first fraction known as head, contains ethyl acetate among other sovents like methanol , so this device is supossed to cope with it...
 
Nachooo said:
... but I read somewhere that EA is not agressive on silicone...
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Shroombee mentioned using silicone lid gaskets no problem with EA. Even if it does deteriorate to some extent after many uses you can probably get a replacement gasket easily. EA compatible or not, I'm considering getting one of these now 😁
 
starbob said:
Nachooo said:
... but I read somewhere that EA is not agressive on silicone...
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Shroombee mentioned using silicone lid gaskets no problem with EA. Even if it does deteriorate to some extent after many uses you can probably get a replacement gasket easily. EA compatible or not, I'm considering getting one of these now 😁
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I got mine with a discount for about 70$... Right now the only issue I saw is that the serpentin maybe has to cool a little more if you use temps above 85 C..as EA boils at 78 C . I would not use temps above 85C with EA. And as was mentioned earlier..just some refrigeration in the recover jar and probably I will add to the final dripping tube some more copper or stainless tube in serepentine form, just to reduce the temps a few more. Using it I would recommend check the initial volume and the recovered one, and let always some final volume of EA in the device to avoid it working empty after all EA has been evaporated. Of course lot of caution using this kind of apparatus good ventilation, no flames etc etc..
 
Got the biggest xtlas yet. Dime size. Not sure why, happened on resused solvent. Xtalization was slower than usual. Another jar xtalized faster from the same paste and had smaller xtals. They remind me of stars. Same salting. The difference was the solvent source (different reuses).

When the CIELO clouds clear, the stars come out 😉
 

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Wiki has been updated for CIELO:

- Added preliminary NMR results from Endlessness. He has confirmed the monomescaline citrate salt form which we had concluded before with crude kitchen tests. Purity came out to 91% which seems low, so he is repeating the measurent/calculation. There was not water signal, so the salt is not a hydrate.
- Moved alternative salting methods to the appendix, including Endlessness' new CASEA approach
- Other minor updates

Feedback welcome.
 
Updated the TEK again with more pictures. Added credits to the images. There are two I may have gotten wrong.

The reagent result was from Merkin?
The succinic result was from _Trip_?

I can't recall, will investigate/verify or correcr later, but if anyone knows for sure please let me know.

Thanks for all the help everyone!
 
Hey!

So just to clarify a couple of things you could edit the wiki, Loveall.

The NMR results show 93.1% purity for mescaline citrate (48.75% of mescaline base in the sample). The only other detectable signal is water so the other 6.9% could simply be this water (moisture from the air? left overs from water in ethyl acetate that didnt fully evaporate?). The thing is we cannot know with this particular experiment because we used D20 as a solvent and deuterium oxide generally has traces of H2O.

I will repeat the experiment again to give a more accurate result and confirm the final purity.
 
To see if the water is indeed that contamination you could run the measurement in DMSO, which will also dissolve any salt for sure.

Then the water peak will move from 4,79 ppm (in D2O) to 3,3 ppm (in DMSO). If the peak at 4,79 ppm stays exactly like it then it could be indeed some kind of contamination ... but actually that range is rarely seen as organic molecules more commonly 'populate' the area just above 6+ or below 4- ppm.

To know if it is from the solvent and therefore inside of the sample and therefore either a "water contamination" or maybe complexed water which might always be present you could run a NMR measurement with no sample.

Then you can compare the intensity of the water peak with sample / without sample and then you know if it maybe comes just from the solvent itself. Chances might be still that the Citrate will catch up complexed water, which will then always be present, but if everything is crystalline and otherwise pure I guess that does absolutely nothing bad :love:


Loveall said:
Fig. 2a: Cactus life stages. [...]
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Cool pictures and I love the last one, showing the dried Cactus powder as one of his Life Stages hehehe :twisted: 😁
 
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?
 
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.
 
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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