Difference between revisions of "CIELO"

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(→‎Salt)
(Big update to use chilled ethyl acetate)
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In this TEK, aqueous alkaline cactus paste is extracted with ethyl acetate. The extract is salted with excess citric acid to force the precipitation of mescaline citrate crystals directly in the solvent.
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In this technique (TEK), aqueous alkaline cactus paste is quickly extracted with chilled ethyl acetate (sometimes sold as "MEK Substitute" in hardware stores). Dissolving excess citric acid in the extract precipitates mescaline citrate crystals.
  
  
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This process was developed in a loving collaboration at the DMT nexus. Deep thanks and gratitude to everyone who contributed or provided support: someblackguy, Benzyme, shroombee, Metta-Morpheus, Downwardsfromzero, Kash, grollum, Mindlusion, Doubledog, Loveall, and others.
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This process was developed in a loving collaboration at the DMT nexus. Deep thanks and gratitude go to everyone who contributed or provided support: someblackguy, Benzyme, shroombee, Metta-Morpheus, Downwardsfromzero, Kash, grollum, Mindlusion, Doubledog, Loveall, and others.
  
 
= Safety =
 
= Safety =
  
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Review ethyl acetate's safety information<ref>Ethyl acetate safety[https://www.msdsonline.com/2015/04/10/ethyl-acetate-a-sweet-smelling-safety-hazard/#:~:text=Ethyl%20acetate%20is%20highly%20flammable,with%20the%20eyes%20or%20skin.]</ref> and check the manufacture's MSDS to verify you have pure ethyl acetate.  
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Review ethyl acetate's safety information<ref>Ethyl acetate safety[https://www.msdsonline.com/2015/04/10/ethyl-acetate-a-sweet-smelling-safety-hazard/#:~:text=Ethyl%20acetate%20is%20highly%20flammable,with%20the%20eyes%20or%20skin.]</ref> 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.
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Make sure any plastic you use is compatible with ethyl acetate and verify your ethyl acetate evaporates cleanly.
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= Materials =
 
= Materials =
  
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* Quart jars (Optional: French press)
 
 
* 300g water
 
* 300g water
−
* 25g Ca(OH)2 (lime)
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* 25g lime
−
* 100g powdered cactus
+
* 100g dry cactus powder
−
* 1000g ethyl acetate ("MEK substitute")
+
* ~1200g ethyl acetate
 
* Coffee filters
 
* Coffee filters
−
* Citric acid
+
* 5g of citric acid
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* Warm water, shallow baking dish, razor blade, storage jar
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* Non-consumables: Scales (g and mg), jars (~32oz, and ~64oz), french press (optional), funnel, and coffee filter support.
 +
 
 +
 
 +
<center>''Fig. 1: Materials used in the CIELO Tek.</center>
  
 
= Process =
 
= Process =
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== Paste ==
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== Make Alkaline Paste ==
  
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Mix water and lime in a quart jar (or optionally a french press) to make milk of lime. Incorporate cactus while stirring. Continue stirring until paste is smooth (about 10 minutes). Allow paste to react for 24 hours and mix again for a few minutes.
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Mix water and lime in a medium (~32 oz) jar, or optionally 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.
  
  
 
[[File:Screenshot_20210311-161134.png|center]]
 
[[File:Screenshot_20210311-161134.png|center]]
 +
<center>''Fig. 2: Reacted alkali cactus paste thoroughly stirred.</center>
  
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== Pull ==
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== Pull Alkaline Paste==
  
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Add ~ 300g of ethyl acetate to cover the paste and mix gently for about 30 seconds to small sandy clumps. After 3 minutes of '''complete rest''', decant/filter to a new jar. Normally only ~150g are recovered in the first pull. If decanting from a french press, squeeze very gently to avoid pulling water.
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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).
  
  
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Immediately pull four more times with ~150g of ethyl acetate (enough to cover the paste). Normally, 150g of solvent are recovered each time. All five pulls should be be done within ~45 minutes.  
+
[[File:IMG_20210601_122315740_copy_600x800.jpg| center]]
 +
<center>''Fig. 3: Clear ethyl acetate extract from cactus alkaline paste.</center>
  
 +
== Crystalize Extract ==
  
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Image below shows the combined pulls against a window with horizontal blinds. Darkness and transparency can vary, but extract should be clear with no clouds.
+
Verify no particles or droplets are in the extract. If any are present, decant/filter to remove them.
  
  
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[[File:Screenshot_20210311-161548.png| center]]
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Dissolve ~ 5g of citric acid into extract. Solution will become cloudy (Fig. 4). Move cloudy extract to the fridge overnight to form mescaline citrate crystals (Fig. 5).
  
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== Salt ==
 
  
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Verify no particles or droplets are in the combined pulls. If any are present, decant/filter to remove them.
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[[File:IMG 20210601 122626621 copy 600x800 1.jpg|center]]
 +
<center>''Fig. 4: Cloudy extract after citric acid addition.</center>
  
  
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Dissolve ~ 20mg/g of citric acid into the extract (for example, add 16g of citric acid to 800g of extract). Solution will become cloudy and crystals will form. Some transparent crystals may stick to the jar walls while others loosely fall out of solution.
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[[File:IMG 20210603 090359363 copy 600x800.jpg|center]]
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<center>''Fig. 5: Mescaline citrate crystals in salted extract.</center>
  
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== Finish ==  
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== Collect Crystals ==  
  
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Pour extract through a coffee filter to catch the loose crystals. Rinse jar walls with a small ammount of fresh ehtyl acetate and send that trough the filter for a wash. Repeat this about two more times until green color is removed.  
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Swirl extract to suspend crystals and catch them in a coffee filter. Repeat with a small amount of fresh ethyl acetate until green color is removed and all crystals are in the filter (2-3 times). Allow crystals to dry and collect them. This is the final product (Fig. 6).
  
  
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Once dry, this how the product caught in the filter looks:
+
Mass spectrometry (MS) results from solaris analytical<ref>Solaris analytical service[https://www.solarisanalytical.com/]</ref> indicate the product is very clean mescaline (Fig. 7). Yield is highly dependent on cactus material, typically from 0.2% to 2% <ref>Cactus analysis thread[https://www.dmt-nexus.me/forum/default.aspx?g=posts&t=71353]</ref>.
  
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[[File:Screenshot 20210312-234218.png|center]]
 
  
 +
[[File:IMG 20210603 130102387 copy 600x800.jpg|center]]
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<center>''Fig. 6: Final product.</center>
  
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Crystals that stick to the jar walls can be recovered with warm water. Evaporation results in needle-like crystals (see image below). Optionally, the fraction of product that was recovered in the coffee filter can also be dissolved in the warm water so all the product is in needle crystal form after evaporation.
 
  
 +
[[File: Screenshot_20210310-062431.png|center]]''<center>Fig. 7: Mass spectrometry result. Peak near 210.5 is mescaline. Peaks at and 193.6, 178.4, and 162.0 are mescaline with amine/methyl/methoxy groups cleaved giving the lower mass spectrum in multiples of ~16 au (16.9, 32.1, and 48.5 respectively). The small peak at 239.5 is not attributed to mescaline. </center>
  
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[[File:Screenshot 20210320-093816.png|center]]
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= Appendix: Development Notes =
  
 +
== What worked ==
  
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[[File: Screenshot_20210401-095800.png|center]]
 
  
 +
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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Mass spectrometry (MS) results from solaris analytical<ref>Solaris analytical service[https://www.solarisanalytical.com/]</ref> indicate the product is very clean mescaline. See MS spectrum below, peak near 210.5 is mescaline. Peaks at and 193.6, 178.4, and 162.0 are believed to be mescaline with amine/methyl/methoxy groups cleaved to generate the lower mass mescaline spectrum in multiples of ~16 au (16.9, 32.1, and 48.5 respectively). The small peak at 239.5 is not attributed to mescaline.
 
  
 +
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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[[File: Screenshot_20210310-062431.png|center]]
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== What didn't work ==
  
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= Appendix: Lab Notes =
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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.
  
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Product from cactus stored as powder can have a tan color. This is normal and seems to be only cosmetic. Freshly ground cactus from dried chips gives a whiter product.
 
  
 +
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.
  
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The pulls appear to be very efficient, extracting mescaline within minutes. The similarity between the solvent's ethoxy group and mescaline's methoxy groups could contribute to the excellent solubility. Long pulls make the paste congeal together and trivial to decant, but congealed paste can lower yield and there is a risk of ethyl acetate reacting with lime or free base over time. Whatever the reason(s), quickness gives good yields experimentally and is recommended.
 
  
 +
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.
  
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Heating during the pull was tested and did not improve yields. Adding NaCl to the paste before pulling was also tested, but no improvements were noted.
 
  
 +
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.
  
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It is possible to chemically dry the extract with a drying agent such as anhydrous MgSO4 before salting. However, no clear yield benefit was observed by performing this step. In one example, drying the paste with CaCl2 resulted in a more difficult crystalization and a 40% yield loss. Usually, the water content in ethyl acetate directly from the pulls is naturally in a good range experimentally. However, droplets or debris not decanted/filtered before salting may result in poor crystalization. If issues are encountered while salting, adding more citric acid and shaking may help.
+
== Crystalization details ==
  
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+
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):
−
During salting, every 10mg of citric acid ('''H3Cit''') reacts with enough free base mescaline ('''Mes''') to form to 43mg of mescaline citrate (or slightly more if a hydrate form is precipitating):
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250mg of citric acid are enough to convert mescaline from free base to salt for a typical cactus (100g with up to 1% yield). However, and outlier like the legendary Ogun would need ~1100mg of citric acid for a 4.7% yield for 100g of dry cactus. The excess amount used in this the TEK guarantees salting of the most potent of cacti.
+
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.
  
  
−
Excess acid induces crystalization. '''This is a simple but very important lab observation''', compatible with Le Chatelier's principle. There is room for excess citric acid in solution since 50mg can dissolve per gram of ethyl acetate (50mg/g). Water in the solvent from the pulls may increase this solubility further. The vast majority of excess acid is poured off after salting, and remaining traces are removed when washing the crystals. No new or additional crashes are observed over acidifying after the first crash. The TEK recommends 20mg/g since this was found to be enough to crash mescaline for most users, but others may need more citric acid.
+
Finally, other dry solid organic acids could work. Fumaric, Malic, Tartaric, Ascorbic, Succinic, etc can be tested in future investigations.
−
 
+
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+
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The crystalization could depend on the amount of plant material in the extract (which can be variable between plant sources). [https://www.dmt-nexus.me/forum/default.aspx?g=posts&m=1105396#post1105396 Sometimes] it can take longer for crystals to form and a few days are needed. [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. It has also been reported that 5mg/g of citric acid is 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]). While there is some variability between experiments, given enough citric acid and time, mescaline citrate crystals eventually form from a clean extract in most situations.
+
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+
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+
−
Other solid organic acids could work. Fumaric, Malic, Tartaric, Ascorbic, Succinic, etc can be tested. Sulfuric acid  HCl could be investigated (and crystals have been observed with sulfuric), but may interact with ethyl acetate and break it down, an issue not expected with the milder organic acids.
+
  
 +
== 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<ref>Ethyl acetate approach[https://www.dmt-nexus.me/forum/default.aspx?g=posts&t=96262]</ref>. There could be ways to improve this process.
 
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<ref>Ethyl acetate approach[https://www.dmt-nexus.me/forum/default.aspx?g=posts&t=96262]</ref>. There could be ways to improve this process.
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= References =
 
= References =
 
<references/>
 
<references/>
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== Appendix: Shroombee's Notes ==
 
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=== Experiment #2 ===
 
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'''March 12, 2021'''
 
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'''8:45 am''' Weighed out 100 grams cactus chips (will use 50 grams for this experiment and the other 50 grams in a followup experiment).
 
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'''8:48 am''' Ground cactus chips to very fine powder in Vitamix for 2 minutes, eventually hitting highest speed.
 
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'''8:50 am''' Weighed out 12.5 grams lime, 153.1 grams purified water, 50.5 grams finely ground cactus powder.
 
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'''8:58 am''' Mixed water and lime together in a stainless steel mixing bowl to make a milky water.  Gradually added cactus powder, incorporating powder into milky water.  Cactus gets to a fluffy texture and then transitions to being a little more clumpy.  Finished mixing at 9:05 am.
 
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'''9:11 am''' Added 99.8 grams ethyl acetate to the cactus for pull #1.  Mixed gently for 30 seconds.
 
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'''In retrospect, do not mix at all.  Just push the cactus around a little so the ethyl acetate can run through the cactus.'''  Solvent quickly turns green.
 
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'''9:23 am''' After letting the cactus and ethyl acetate sit for 10 minutes, decanted the ethyl acetate into a beaker with a metal coffee filter sitting inside the top of the beaker (works well).  Beaker plus filter beforehand was 342.3 grams.  After decanting solvent into it, 372.8 grams.
 
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'''Solvent recovery for pull #1 = 30.5 grams (out of 99.8 grams added).'''  For next experiment, see if not mixing at all will reduce the amount of solvent that the cactus absorbs.  A drop of solvent on pH paper turns the paper dark green (not blackish green though).
 
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'''9:28 am''' Added 110.1 grams fresh ethyl acetate to cactus for pull #2.  Very gently pushing the cactus for about 10 seconds, just to get the solvent to run through the cactus.  The ethyl acetate quickly turns green.
 
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'''9:31 am''' Moved pull #1 to a mason jar.  Mason jar beforehand is 426.8 grams.  After is 456.6 grams.  29.8 grams solvent moved from beaker to mason jar.
 
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'''9:38 am''' After 10 minutes sitting with the cactus, decanted pull #2 into the beaker.  Beaker is 342.3 grams before, 447.9 grams after.
 
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'''Solvent recovery for pull #2 = 105.6 grams (out of 110.1 grams added).'''  pH paper is medium dark green.
 
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'''9:45 am''' Added 103.3 grams fresh ethyl acetate to the cactus for pull #3.  Almost no manipulation of the cactus at this point.  Solvent quickly gets green color.
 
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'''9:46 am''' Moved pull #2 to the mason jar (combining with pull #1).  Mason jar beforehand is 456.4 grams.  After is 560.4 grams.  104.0 grams solvent moved from beaker to mason jar.  Interesting at 9:31 am the mason jar weighed 456.6 grams.  15 minutes later it weighs 456.4 grams.  Is this evaporation of ethyl acetate or error in the scale?  Scale supposed to be accurate to 0.1 grams.
 
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'''9:55 am''' After 10 minutes sitting with the cactus, decanted pull #3 into the beaker.  Beaker is 342.5 grams before, 450.3 grams after.
 
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'''Solvent recovery for pull #3 = 107.8 grams (out of 103.3 grams added).'''  We got back the amount we added for pull #3, plus a few more grams.  The paste is starting to stick to itself, making it easy to decant and pour solvent out of the mixing bowl by holding the paste back with a strainer/skimmer ladle.  pH paper is light green.
 
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'''10:00 am''' Added 103.9 grams fresh ethyl acetate to the cactus for pull #4.  As with pull #3, almost no manipulation of the cactus.  Just pushing the cactus under the solvent.  Solvent picks up green color.
 
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'''10:08 am''' Moved pull #3 to the mason jar (combining with pull #1 and pull #2).  Mason jar beforehand is 560.2.  After is 667.0 grams.  106.8 grams solvent moved from beaker to mason jar.  As before, mason jar seems to have lost 0.2 grams of solvent.  The solvent in the mason jar is a beautiful emerald green.
 
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'''10:10 am''' After 10 minutes sitting with the cactus, decanted pull #4 into the beaker.  Beaker is 342.7 grams before, 444.7 grams after.
 
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'''Solvent recovery for pull #4 = 102.0 grams (out of 103.9 grams added).'''  pH paper is faint green.  After drying, the paper barely has any greenish tint.
 
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'''10:16 am''' Added 104.0 grams fresh ethyl acetate to the cactus for pull #5.  Almost no manipulation of the cactus.  Solvent picks up a light green tint.
 
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'''10:20 am''' Moved pull #4 to the mason jar (combining with pull #1-3).  Mason jar beforehand is 666.9 grams.  After is 767.8 grams.  100.9 grams solvent moved from beaker to mason jar.  Mason jar lost 0.1 grams solvent since 10:08 am.
 
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'''10:26 am''' After 10 minutes sitting with the cactus, decanted pull #5 into the beaker.  Beaker is 342.5 grams before, 446.0 grams after.
 
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−
'''Solvent recovery for pull #5 = 103.5 grams (out of 104.0 grams added).'''  pH paper has no materially significant color change.  After drying, the paper shows no color change.  This pull is NOT being combined with pulls #1-4 since it does not appear to have any freebase mescaline.  Will consider what technique to use to see if there is any mescaline to be obtained from this pull.
 
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'''Total solvent added = 99.8 + 110.1 + 103.3 + 103.9 + 104.0 = 521.1 grams.  Total solvent recovered = 30.5 + 105.6 + 107.8 + 102.0 + 103.5 = 449.4 grams.  Lost 71.7 grams solvent to the cactus (almost all in pull #1).'''
 
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'''10:46 am''' Washed and dried the metal coffee filter.  Then added a paper filter into the metal filter.  Ran pulls #1-4 through the metal+paper filter and into a new mason jar.  Ran pull #5 through the metal+paper filter and into a separate mason jar.  The purpose of filtering again is that I noticed a few bits of cactus material got into the combined decanted solvent.  I don't know how that occurred since the metal filter is a fine mesh filter.  In any case, now we have filtered solvent.
 
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'''10:52 am''' Added 254 grams of citric acid to the combined pulls mason jar.  Clouds form in the solvent.  Stirred gently with a spoon.  pH paper comes out yellow.
 
−
 
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'''10:56 am''' Put a stainless steel lid with silicone liner on the mason jar.  Put mason jar into the frig to wait for crystals.
 
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'''1:45 pm''' Mason jar is in the frig.  Solvent is opaque.  No crystals yet.
 
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''Added by Loveall: This looks promising. If xtals do not form, I would try adding citric acid until pH paper has some red coloring (maybe another 250mg will do). If xtals still don't form, I would add water at ~0.5% increments (~2.2g), shaking and waiting to see if xtals form. I added a picture of how the pH paper looks from an extract that crystalized well in the main TEK.''
 
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=== Experiment #1 ===
 
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'''March 9, 2021'''
 
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'''6:42 pm'''
 
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100 grams Peruvian Torch chips
 
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−
298 grams purified water
 
−
 
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Blended cactus chips in the Vitamix dry container so it becomes a fine powder.
 
−
 
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'''6:58 pm'''
 
−
Mixed cactus powder and water in a plastic mixing bowl rather than a mason jar because it seems easier.  Product is a fluffy texture, olive green color.  There is no excess water.
 
−
 
−
The bowl plus cactus plus silicone mixing spoon weighs 826.5 grams.  Microwave on high for 30 seconds, mix, then weigh.  This is pretty easy.  I wouldn't want to do this in a mason jar.  The cactus does not bubble and there is no issue at 30 seconds with anything bubbling over.  Weight after each 30 second cycle:
 
−
 
−
825.6 grams
 
−
 
−
823.9 grams
 
−
 
−
820.2 grams
 
−
 
−
816.0 grams
 
−
 
−
808.7 grams
 
−
 
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800.7 grams
 
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791.3 grams
 
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783.2 grams
 
−
 
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775.8 grams
 
−
 
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765.8 grams
 
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−
DONE
 
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−
After a couple of the microwaving cycles, the cactus lost its fluffiness and became like light bread dough, not sticking much to the bowl.
 
−
 
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'''7:25 pm''' Begin slowly mixing in 25 grams pickling lime.  Started with the plastic bowl but switched to a ceramic bowl after a minute, not knowing how the plastic would react to the base.  Bowl appears fine after washing it out.
 
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'''7:39 pm''' I'm using a fork to try to get the lime mixed evenly.  I figure my Kitchenaid stand mixer will be easier so I break that out.
 
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'''7:45 pm''' Letting the Kitchenaid stir the cactus for me.  Much easier!
 
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'''7:53 pm''' Added 25 grams calcium chloride.  Before adding, the cactus paste was fluffy and stuck to the sides of the stainless steel bowl.  After adding the calcium chloride, the cactus became like clumpy sand and hardly stuck to the sides of the bowl.
 
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'''7:58 pm''' Stopped mixing.
 
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'''8:05 pm''' Transferred cactus to a wide mouth quart mason jar and added 220 ml of ethyl acetate (weighing 199.9 grams).  The ethyl acetate came up to approximately 540 ml on the side of the mason jar.  After shaking, the cactus looked like fluffy beach sand.
 
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'''8:28 pm''' Shake for a minute.
 
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'''9:00 pm''' Shake for a minute.
 
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'''9:22 pm''' No shaking, I notice the ethyl acetate is light green.
 
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'''10:30 pm''' Shake for a minute.  The cactus is starting to get a little stickier, leaving streaks on the glass.
 
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'''11:00 pm''' Ethyl acetate comes up to exactly 500 ml on the side of the mason jar.  Versus ~540 ml at 8:05 pm when the ethyl acetate was first added.  '''What accounts for this 40 ml difference?'''
 
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'''12:00 am''' Shake for a minute.
 
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'''1:06 am''' Weighed mason jar with cactus: 1001.4 grams.
 
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'''March 10, 2021'''
 
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'''7:57 am''' Weighed mason jar with cactus: 1001.1 grams.
 
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Ready to decant ethyl acetate.  Large pyrex beaker with metal coffee filter weighs 342.3 grams.  Ethyl acetate is a medium, emerald green.  Definitely not light green and not yellow.
 
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−
Using a small ladle to decant, which gets most of the ethyl acetate with no plant matter.  Beaker weighs 427.2 grams meaning we recovered 84.9 grams of ethyl acetate.  Not too good.
 
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I transferred the cactus to a french press to see if I could recover more ethyl acetate.  The sticky paste does not compress and I recovered an additional ~6 grams ethyl acetate.  '''French press is obviously not worth the effort!'''
 
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'''8:21 am''' Done with decanting, transferring, french pressing, weighing, et cetera.  Total recovery for this pull is 90.6 grams ethyl acetate.
 
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'''8:23 am''' Added 90.7 grams of fresh ethyl acetate to the mason jar.  Stirred ethyl acetate into the sticky cactus, did not shake.  Ethyl acetate is already changing to green color.
 
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−
'''8:33 am''' Photo of pH paper.  Paper is dark green.  pH 10 or 11?  Also tested using the 4 color pH strips.  More difficult to judge the pH with these. 
 
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'''8:34 am''' Photo of recovered ethyl acetate showing it is an emerald green color.
 
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'''8:45 am''' Poured 10 ml of ethyl acetate into a small beaker.  Added 13 mg of citric acid.  Lower half of the beaker turned milky, cloudy.  Checked pH and it's basically the same as the rest of the solvent.  So the small amount of citric acid didn't change the pH much.  I used a disposable pipette and pulled from the top of the solvent, so perhaps the top layer didn't have a chance to react yet.
 
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'''8:49 am''' Photo showing cloudy 10 ml in small beaker.
 
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'''8:50 am''' Poured the 10 ml and the rest of the solvent into a mini Pyrex baking dish, using the larger volume of solvent to rinse out of the small beaker.  I probably should have left the solvent in a mason jar or beaker rather than adding to the baking dish.  Added 95 mg of citric acid.  Stirred a little because I wanted to get a more accurate pH.  pH was about 7.  Added an additional 61 mg citric acid.  pH went to about 6.  Total citric acid added to the 90.6 grams ethyl acetate is 169 mg.  Even after rinsing with the main solvent, the bottom of the small beaker has some spots that look like something crystalizing.  I don't know if it's just sticky citric acid or ???
 
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'''9:07 am''' Photo of 3 pH test strips.
 
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'''3:42 pm''' Moving the dish to the freezer.  Solvent is clear (and has been clear for at least a few hours).  Initially I thought there were droplets on the bottom of the dish (around 11:00 am).  Then tried to scrape at them with a knife and not seeing any movement, I figured they were a reflection from the surface because I noticed some tiny droplets on the surface if I caught the light at the right angle.  Then as I tipped the dish at 3:42pm to move it into the freezer, I now see the droplets really are at the bottom of the dish.  Sort of an oily substance.  There are no crystals.
 
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'''8:00 pm''' Retrieving pull #2.  Beaker plus metal coffee filter weigh 342.3 grams.  Weighs 407.5 grams after decanting.  Recovered 65.2 grams.  Looks like the cactus sucked up more solvent even though I didn't shake.  pH is basic, although the pH paper is not as dark green as pull #1.
 
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'''8:09 pm''' Removed a few tablespoons of sticky slimy cactus and put it into a separate bowl. Mixed in 5.4 grams of calcium chloride (which is a lot relative to the amount of cactus).  Even waiting more than 30 minutes, no additional solvent is released.  The cactus is drier though, more clumpy, and lost some gooey sliminess.
 
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'''8:27 pm''' Since only 65.2 grams of solvent was retrieved, I decided adding this amount of fresh solvent for pull #3 would be too inefficient.  I added 197.6 grams fresh ethyl acetate and stirred for 1-2 minutes.  Solvent turned a light green fairly quickly.
 
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'''8:38 pm''' Added 49 mg citric acid to the recovered solvent.  Bottom of jar got milky.  Tested pH with 3 strips.  (1) Took a solvent sample towards the bottom of the jar at the clouds: pH about 5.  (2) Solvent sample at the surface: pH about 7.  (3) Swirled the jar around then took a solvent sample.  pH about 6.
 
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'''8:45 pm''' Put jar into freezer.
 

Revision as of 19:40, 3 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). Dissolving excess citric acid in the extract precipitates mescaline citrate crystals.


This process was developed in a loving collaboration at the DMT nexus. Deep thanks and gratitude go to everyone who contributed or provided support: 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: Scales (g and mg), jars (~32oz, and ~64oz), french press (optional), funnel, and coffee filter support.


Fig. 1: Materials used in the CIELO Tek.

Process

Make Alkaline Paste

Mix water and lime in a medium (~32 oz) jar, or optionally 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.


Screenshot 20210311-161134.png
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.


Dissolve ~ 5g of citric acid into extract. Solution will become cloudy (Fig. 4). Move cloudy extract to the fridge overnight to form mescaline citrate crystals (Fig. 5).


IMG 20210601 122626621 copy 600x800 1.jpg
Fig. 4: Cloudy extract after citric acid addition.


IMG 20210603 090359363 copy 600x800.jpg
Fig. 5: Mescaline citrate crystals in salted extract.

Collect Crystals

Swirl extract to suspend crystals and catch them in a coffee filter. Repeat with a small amount of fresh ethyl acetate until green color is removed and all crystals are in the filter (2-3 times). Allow crystals to dry and collect them. This is the final product (Fig. 6).


Mass spectrometry (MS) results from solaris analytical[2] indicate the product is very clean mescaline (Fig. 7). Yield is highly dependent on cactus material, typically from 0.2% to 2% [3].


IMG 20210603 130102387 copy 600x800.jpg
Fig. 6: Final product.


Screenshot 20210310-062431.png
Fig. 7: Mass spectrometry result. Peak near 210.5 is mescaline. Peaks at and 193.6, 178.4, and 162.0 are mescaline with amine/methyl/methoxy groups cleaved giving the lower mass spectrum in multiples of ~16 au (16.9, 32.1, and 48.5 respectively). The small 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 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.


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. 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]
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