Difference between revisions of "CIELO"

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(What worked)
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Chilled ethyl acetate was found to make the process robust experimentally, presumably by minimizing water and plant material while remaining efficient with mescaline. By minimizing plant matter in the pull, in situ crystallization is improved across different cacti sources, which is important when skipping the classic liquid-liquid extraction (LLE) steps.
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Chilled ethyl acetate was found to make the process robust experimentally, presumably by minimizing water and plant material while remaining efficient pulling mescaline. By minimizing plant matter crystallization is improved.
  
  
It is also possible to obtain good results with 3 minute room temperature pulls, but the results may not be as consistent between users as with chilled ethyl acetate. [https://www.dmt-nexus.me/forum/default.aspx?g=posts&m=1105396#post1105396 Sometimes] it can take longer for crystals to form, while [https://www.dmt-nexus.me/forum/default.aspx?g=posts&m=1098483#post1098483 other times] crystalization can be very quick when using a magnetic stirrer. With room temperature solvent 5mg/g of citric acid can be enough when working with outer cactus skin, but not when working with the [https://www.dmt-nexus.me/forum/default.aspx?g=posts&m=1102283#post1102283 whole plant].
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It is also possible to obtain good results with room temperature pulls, but the results may not be as consistent. [https://www.dmt-nexus.me/forum/default.aspx?g=posts&m=1105396#post1105396 Sometimes] it can take longer for crystals to form, while [https://www.dmt-nexus.me/forum/default.aspx?g=posts&m=1098483#post1098483 other times] crystalization can be very quick when using a magnetic stirrer. With room temperature solvent 5mg/g of citric acid can be enough when working with outer cactus skin, but not when working with the [https://www.dmt-nexus.me/forum/default.aspx?g=posts&m=1102283#post1102283 whole plant].
  
 
== What didn't work ==
 
== What didn't work ==

Revision as of 00:29, 4 June 2021

Introduction

CIELO stands for Crystals In Ethyl-acetate Leisurely OTC (Over The Counter).


In this technique (TEK), aqueous alkaline cactus paste is quickly extracted with chilled ethyl acetate (sometimes sold as "MEK Substitute" in hardware stores). Excess citric acid is added to the extract to precipitate mescaline citrate crystals.


This TEK was developed in a loving collaboration at the DMT nexus. Deep thanks and gratitude go to everyone who contributed: someblackguy, Benzyme, shroombee, Metta-Morpheus, Downwardsfromzero, Kash, grollum, Mindlusion, Doubledog, Loveall, and others.

Safety

Review ethyl acetate's safety information[1] and check the manufacture's MSDS to verify you have pure ethyl acetate. Make sure any plastic you use is compatible with ethyl acetate and verify your ethyl acetate evaporates cleanly.


Following this advice does not guarantee safety. It is up to each adult individual to make their own decision on proceeding with this process.

Materials

  • 300g water
  • 25g lime
  • 100g dry cactus powder
  • ~1200g ethyl acetate
  • Coffee filters
  • 5g of citric acid
  • Non-consumables: Quart jar or french press (preferred), Large jar (~64 oz), funnel, coffee filter support, shallow baking dish with ethyl acetate resistant lid.
IMG 20210603 180858748 copy 800x600.jpg
Fig. 1: Materials used (french press option).

Process

Make Alkaline Paste

Mix water and lime in a quart jar, or preferably a french press, to make milk of lime. Incorporate cactus while stirring and continue stirring for at least 10 minutes to a smooth paste. Allow paste to react for 24 hours and mix again for a few minutes.


IMG 20210603 183405358 copy 800x600.jpg
Fig. 2: Reacted alkali cactus paste thoroughly stirred.

Pull Alkaline Paste

Add ~ 300g of freezer chilled ethyl acetate (~0 F) to the paste, mix for 60 seconds, and decant/filter to a large jar (~64 oz). If using a french press squeeze very gently to avoid pulling water. Immediately pull 5 more times with ~150g of ethyl acetate stirring for 60 seconds each time. Final extract should be clear with no droplets or particles (see Fig. 3).


IMG 20210601 122315740 copy 600x800.jpg
Fig. 3: Clear ethyl acetate extract from cactus alkaline paste.

Crystalize Extract

Verify no particles or droplets are in the extract. If any are present, decant/filter to remove them.


Pour extract into shallow baking dish and add 5g of citric acid. Cover with ethyl acetate resistant lid and move to the fridge overnight. Citric acid will diffuse into solution and form mescaline citrate crystals (Fig. 4).


IMG 20210603 090359363 copy 600x800.jpg
Fig. 4: Mescaline citrate crystals in extract.

Collect Crystals

Pour extract through a coffee filter. Rinse baking dish with a small amount of fresh ethyl acetate and send that through the filter. Repeat until green color is removed (2-3 times). Allow crystals to dry and collect them from the filter and baking dish. This is the final product (Fig. 5).


Mass spectrometry (MS) results from solaris analytical[2] indicate the product is very clean mescaline (Fig. 6). Yield is highly dependent on cactus material, typically from 0.2% to 2% [3].


IMG 20210603 130102387 copy 600x800.jpg
Fig. 5: Final product.


Screenshot 20210310-062431.png
Fig. 6: Mass spectrometry result. Peak near 210.5 is mescaline. Peaks at and 193.6, 178.4, and 162.0 are mescaline with cleaved functional groups. The peak at 239.5 is not attributed to mescaline.

Appendix: Development Notes

What worked

Chilled ethyl acetate was found to make the process robust experimentally, presumably by minimizing water and plant material while remaining efficient pulling mescaline. By minimizing plant matter crystallization is improved.


It is also possible to obtain good results with room temperature pulls, but the results may not be as consistent. Sometimes it can take longer for crystals to form, while other times crystalization can be very quick when using a magnetic stirrer. With room temperature solvent 5mg/g of citric acid can be enough when working with outer cactus skin, but not when working with the whole plant.

What didn't work

Paste modifications: No improvements seen with microwaving, partially drying, adding NaCl, or extending the reaction time beyond 24h. Completely drying the paste made the process not work, apparently some water is needed in this process.


Pull modifications: Long room temperature pulls made the paste congeal and resulted in lower yield. Heating during the pull did not improve yields. In general the crystalization is more difficult and the product can aquire a tan color if the pulls are more aggressive with no improvement to yield.


Extract modifications: Chemically drying the extract with a drying agent such as anhydrous MgSO4 before salting had no yield benefit. In one example, drying the extract with CaCl2 resulted in a more difficult crystalization and a 40% yield loss. In general, any water content in ethyl acetate directly from the pulls is already in a good range experimentally.


Note: Droplets or debris not decanted/filtered before salting will result in crystalization issues. It is very important to verify the extract is clean before salting.

Crystalization details

During crystallization, every 10mg of citric acid (H3Cit) reacts with free base mescaline (Mes) to form to 43mg of mescaline citrate (or slightly more if a hydrate form is precipitating):


3Mes(↑) + H3Cit(↑) ⇒ 3(MesH)Cit(↓)


The TEK calls for a lot more citric acid than would be needed for titration. The reason is that excess citric acid induces crystalization to overcome any water or plant material that would otherwise keep mescaline citrate in solution. This is a simple but very important lab observation, compatible with Le Chatelier's principle. There is a lot room for excess citric acid in ethyl acetate since its solubility is 50mg/g (and water in the solvent from the pulls may increase this solubility further). The TEK recommends 5mg/g since this was found to be enough to crash mescaline for most users when using chilled ethyl acetate, buy going above this recommendation is OK if issues are encountered to try to force crystalization due to plant variability and/or technique issues.


Finally, other dry solid organic acids could work. Fumaric, Malic, Tartaric, Ascorbic, Succinic, etc can be tested in future investigations.

Disclaimer

It is possible that some of the assumptions and conclusions in these lab notes are incorrect or incomplete. The process was tested in several ways, but the search was not exhaustive[4]. There could be ways to improve this process.

References

  1. Ethyl acetate safety[1]
  2. Solaris analytical service[2]
  3. Cactus analysis thread[3]
  4. Ethyl acetate approach[4]