Difference between revisions of "CIELO"

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(β†’β€ŽIntroduction πŸ™)
(Large update to jar crystallization and other better methods)
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βˆ’
In this technique (TEK), aqueous alkaline cactus paste (Fig. 2) is extracted with chilled ethyl acetate (Fig. 3). Mescaline citrate is precipitated by citric acid (Figs. 4-5) and collected (Fig. 6).
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In this technique (TEK), cold alkaline cactus paste (Fig. 2) is extracted with chilled ethyl acetate (Fig. 3). Mescaline citrate is precipitated with citric acid (Fig. 4) and collected (Fig. 5).
  
  
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= Materials πŸ›’=
 
= Materials πŸ›’=
βˆ’
*Mescaline Extraction:
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*French press (or similar ensemble)
βˆ’
**Quart jar or french press
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*300g ice cold water
βˆ’
**300g water
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*25g lime
βˆ’
**25g lime
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*100g dry cactus powder
βˆ’
**100g dry cactus powder (outer skin or whole cactus)
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*1qt ethyl acetate (also sold as "MEK substitute")
βˆ’
**~1200g ethyl acetate (sometimes found as "MEK substitute")
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*Coffee filter, support basket, and funnel
βˆ’
**Paper coffee filter, support basket, and funnel
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*Quart jar
βˆ’
**Large jar (~64 oz)
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*4g of citric acid
βˆ’
**5g of citric acid if using outer cactus skin  or 20g if using whole cactus
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*Washing soda (for solvent reclaim)
βˆ’
**Shallow baking dish, lid, and aluminum foil
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βˆ’
**Razor blade
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βˆ’
* Solvent Reclaim:
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[[File:IMG 20210608 223040865 copy 800x600.jpg|center]]
βˆ’
** Washing soda
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<center>''Fig. 1: Materials.</center>
βˆ’
** Water
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βˆ’
** pH paper strips (optional)
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βˆ’
** Separatory funnel or glass turkey baster
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βˆ’
** Coffee filter/filter basket/funnel
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βˆ’
 
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βˆ’
 
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βˆ’
[[File:IMG 20210603 180858748 copy 800x600.jpg|center]]
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βˆ’
<center>''Fig. 1: Materials used (french press option shown).</center>
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= Process πŸ“œ=
 
= Process πŸ“œ=
  
  
βˆ’
== Make Alkaline Paste 🌡 ==
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== Paste 🌡 ==
βˆ’
Mix water and lime in a quart jar or french press. Incorporate cactus while stirring and continue stirring for at least 10 minutes to a smooth paste.
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Mix ice cold water, lime, and cactus in french press for a few minutes to a smooth paste (Fig. 2).
  
  
 
[[File:IMG 20210603 183405358 copy 800x600.jpg|center]]
 
[[File:IMG 20210603 183405358 copy 800x600.jpg|center]]
βˆ’
<center>''Fig. 2: Aqueous alkaline cactus paste.</center>
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<center>''Fig. 2: Alkaline cactus paste.</center>
  
βˆ’
== Pull Alkaline Paste πŸ‘©β€πŸ”¬==
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== Extract πŸ‘¨πŸΎβ€πŸ”¬==
βˆ’
Add ~ 300g of freezer chilled ethyl acetate (~0 F) to the paste, mix thoroughly for for 60 seconds, and decant/filter to a large jar (~64 oz). If using a french press squeeze very gently or not at all to avoid pulling water. Immediately pull 5 more times with ~150g of ethyl acetate stirring thoroughly for 60 seconds each time.  
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Cover cold paste with chilled ethyl acetate (~0F), mix for for 60 seconds and filter to quart jar. Repeat until quart jar is ~80% full (~5x).
  
  
βˆ’
Inspect extract for droplets or particles. If present, decant/filter to remove them.  
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Inspect extract for droplets or particles. If present, remove them. '''Extract needs to be clean''' (see Fig. 3).
βˆ’
'''Extract needs to be clean''' (see Fig. 3).
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<center>''Fig. 3: Ethyl acetate extract.</center>
 
<center>''Fig. 3: Ethyl acetate extract.</center>
  
βˆ’
== Crystalize Extract πŸ§ͺ==
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== Crystalize ✨==
βˆ’
Let extract reach room temperature and pour it into a shallow baking dish. Gently drop in 5g of citric acid if using outer skin powder or 20g if using whole cactus powder. Do not stir, simply allow citric acid to diffuse into solution forming clouds (Fig. 4).  
+
Drop (do not stir) citric acid into extract. Clouds quickly form first followed after a few hours by mescaline citrate crystals (Fig. 4). Allow crystalization to complete undisturbed (~12 hours).
  
  
βˆ’
[[File:IMG 20210604 121027187 copy 800x600.jpg|center]]
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[[File:IMG 20210609 064813073 copy 800x600 1.jpg|center]]<center>''Fig. 4: Crystals in ethyl acetate.</center>
βˆ’
<center>''Fig. 4: Citric acid granules (left cluster) diffusing into extract as clouds within a few seconds (top view of baking dish).</center>
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 +
== Collect πŸ’–==
 +
Catch crystals in a coffee filter. Rinse jar/filter with room temperature ethyl acetate a couple times and dry (Fig. 5).
  
βˆ’
Cover with a lid protected by a layer of aluminum foil if needed (most shallow baking dish lids are not resistant to ethyl acetate). After a few hours clouds crash as mescaline citrate crystals (Fig. 5). Allow enough time to complete crystallization (~24h is typically sufficient but can vary).
 
  
 +
If some crystals stubbornly remain on the jar walls, dissolve them in hot water, dry in a shallow dish, and scrape.
  
βˆ’
[[File:IMG 20210604 165954132 copy 800x600.jpg|center]]
 
βˆ’
<center>''Fig 5.: Mescaline citrate crystals precipitating in the extract (side view of baking dish).</center>
 
  
βˆ’
== Collect Crystals ✨==
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Yield depends on the cactus and is usually between 0.2% to 2% with ~1% being common<ref>Cactus analysis thread[https://www.dmt-nexus.me/forum/default.aspx?g=posts&t=71353]</ref>.
βˆ’
Decant and rinse crystals with a small amount of fresh ethyl acetate twice (or until off color is mostly removed). Allow crystals to dry and collect them from the shallow baking dish with a razor blade to obtain the final product (Fig. 6).
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[[File:IMG 20210603 130102387 copy 600x800 copy 800x600.jpg|center]]
 
[[File:IMG 20210603 130102387 copy 600x800 copy 800x600.jpg|center]]
βˆ’
<center>''Fig. 6: Collected mescaline citrate crystals.</center>
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<center>''Fig. 5: Collected mescaline citrate crystals.</center>
  
  
βˆ’
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 dependent on cactus material and usually between 0.2% to 2% <ref>Cactus analysis thread[https://www.dmt-nexus.me/forum/default.aspx?g=posts&t=71353]</ref> with ~1% being common.
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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 (Fig. 6).
  
  
βˆ’
[[File: Cactus-extract copy 800x600_1.jpg|center]]''<center>Fig. 7: Mass spectrometry result. Peak near 210.5 is mescaline. Lower mass peaks are mescaline with cleaved functional groups. The peak at 239.5 is not attributed to mescaline. </center>
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[[File: Cactus-extract copy 800x600_1.jpg|center]]''<center>Fig. 6: Mass spectrometry result. Peak near 210.5 is mescaline. Lower mass peaks are mescaline with cleaved functional groups. The peak at 239.5 is not attributed to mescaline. </center>
  
 
== Reclaim Solvent πŸ’š==
 
== Reclaim Solvent πŸ’š==
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βˆ’
Wash spent extract with sodium carbonate saturated water shaking vigorously (emulsions do not form). Citric acid removal can be optionally verified with a strip of pH paper. Separate water layer. Freeze and filter out ice crystals. Store for reuse.
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Wash spent extract with sodium carbonate saturated water shaking vigorously (emulsions do not form). Citric acid removal is complete when CO2 bubbling stops. Filter any excess calcium carbonate and remove water layer. Freeze and filter out ice crystals. Store for reuse.
  
 
= Appendix: Development Notes πŸ”¬=
 
= Appendix: Development Notes πŸ”¬=
 
== Paste 🌡==  
 
== Paste 🌡==  
βˆ’
No improvements were seen with longer basing time, microwaving, partially of completely drying (with heat or drying agent), or adding NaCl to increase the ionic strength.
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No improvements were seen with longer basing time, microwaving, drying, or increasing the ionic strength.
  
βˆ’
== Pull πŸ‘¨πŸΎβ€πŸ”¬==  
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== Extract πŸ‘¨πŸΎβ€πŸ”¬==  
βˆ’
It is also possible to obtain good results with 3 minute room temperature pulls (30s of stirring and 150s of rest), but the results may not be as consistent compared to chilled ethyl acetate (60s of stirring). This is thought to be because of increased plant contaminants in the warmer pull at room temperature making crystallization more difficult.
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Longer and/or warmer pulls resulted in darker color, smaller crystals and more absorbed solvent with no yield benefit.
  
  
βˆ’
Long room temperature pulls made the paste congeal and resulted in lower yield. Heating during the pull did not improve yields. Generally, longer times or higher temperatures make the crystalization more difficult without yield improvements and a persistent tan color can contaminate the product.
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Chemically drying the extract before salting had no crystallization or yield benefit.
  
βˆ’
== Extract πŸ§ͺ==  
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== Crystalize ✨==
βˆ’
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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During crystallization, every 233mg of citric acid ('''H3Cit''') react with free base mescaline ('''Mes''') to form to 1g of mescaline citrate (or slightly more if a hydrate is precipitating):
  
  
βˆ’
Droplets or debris not decanted/filtered before adding citric acid can result in crystalization issues. '''It is very important to verify the extract is clean as mentioned in the main TEK'''.
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'''<span style="color: Orange"> <div style="text-align: center;">3Mes<sub>(↑)</sub> + H3Cit<sub>(↑)</sub> β‡’ 3(MesH)Cit<sub>(↓)</sub></div></span>'''
  
βˆ’
== Crystalization ✨==
 
βˆ’
During crystallization, 233mg of citric acid ('''H3Cit''') react with free base mescaline ('''Mes''') to form to 1g of mescaline citrate (or slightly more if a hydrate is precipitating):
 
  
 +
Excess citric acid shifts the precipitation reaction to the right (Le Chatelier's principle), helping overcome water and plant material. There is a lot room for excess citric acid in solution since its solubility is 50mg/g in ethyl acetate. The TEK recommends ~5mg/g but since cacti and pull techniques can vary, users may find other values work better for their specific situation (in one example with whole cactus powder 20mg/g was used <ref>Ethyl acetate approach[https://www.dmt-nexus.me/forum/default.aspx?g=posts&t=96262]</ref>).
  
βˆ’
'''<span style="color: Orange"> <div style="text-align: center;">3Mes<sub>(↑)</sub> + H3Cit<sub>(↑)</sub> β‡’ 3(MesH)Cit<sub>(↓)</sub></div></span>'''
 
  
 +
Several factors can make crystals smaller: Reusing ethyl acetate, warmer pulls, longer pulls, higher citric acid concentration, mechanical agitation, and other potential variables. Small crystals can look like a fine powder. Potency does not seem affected by the crystallization appearance, and a powdery precipitate is not a problem unless it becomes difficult to decant/filter.
  
βˆ’
The TEK calls for more citric acid than would be needed for titration because excess citric acid shifts the precipitation reaction to the right (Le Chatelier's principle), helping overcome water and plant material. There is a lot room for excess citric acid in solution since its solubility is 50mg/g in ethyl acetate. The TEK recommends 5mg/g for outer skin cactus powder and 20mg/g for whole cactus powder based on early experiments<ref>Ethyl acetate approach[https://www.dmt-nexus.me/forum/default.aspx?g=posts&t=96262]</ref>, but since cacti and pull techniques can vary, users may find other values work better for their specific situation.
 
  
 +
After the initial crystallization, adding more citric acid and/or moving the extract to the refrigerator did not result in any more precipitation. Moving the extract to the freezer produced ice crystals.
  
βˆ’
Mescaline citrate grows as needles in ethyl acetate (Fig. 4) that can be up to several mm long. Reused ethyl acetate, warmer pulls, longer pulls, higher citric acid concentration, agitation, and colder temperatures tend to make the needles smaller. Very small needles can look like a powder. Potency does not seem affected by the crystallization appearance, and a powdery precipitate is not an problem unless it becomes difficult to decant/filter.
 
  
 +
Other dry organic acids could work. Fumaric, Malic, Tartaric, Ascorbic, Succinic, etc can be tested in future investigations.
  
βˆ’
After the main TEK's room temperature crystallization, adding more citric acid and/or moving the extract to the refrigerator did not result in any more precipitation. Moving the extract to the freezer produced only ice crystals.
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== Collect πŸ’–==
  
  
βˆ’
Other dry organic acids could work. Fumaric, Malic, Tartaric, Ascorbic, Succinic, etc can be tested in future investigations.
+
Washing crystals over a filter gave better results than decanting. The filter paper wicked away plant off colors forming a ring. Unlike the pulls, warmer ethyl acetate is an advantage because the goal is to dissolve away plant matter.
 +
 
  
βˆ’
== Disclaimer πŸ€·β€β™‚οΈ==
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The jar wash should be done immediately. If any straggler crystals dry in the jar they stuck to the wall.
βˆ’
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. There could be ways to improve this process.
+
  
 
= References πŸ—οΈ=
 
= References πŸ—οΈ=
 
<references/>
 
<references/>

Revision as of 14:00, 9 June 2021

Introduction πŸ™

CIELO stands for Crystals In Ethyl-acetate Leisurely Over-the-counter.


In this technique (TEK), cold alkaline cactus paste (Fig. 2) is extracted with chilled ethyl acetate (Fig. 3). Mescaline citrate is precipitated with citric acid (Fig. 4) and collected (Fig. 5).


Thanks to everyone who contributed: someblackguy, Benzyme, shroombee, Metta-Morpheus, Downwardsfromzero, Kash, grollum, Mindlusion, Doubledog, Dreamer042, Loveall, and others.

Safety ⛑️

Review ethyl acetate's safety information[1]. Verify MSDS, plastic compatibility, and clean evaporation.


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

Materials πŸ›’

  • French press (or similar ensemble)
  • 300g ice cold water
  • 25g lime
  • 100g dry cactus powder
  • 1qt ethyl acetate (also sold as "MEK substitute")
  • Coffee filter, support basket, and funnel
  • Quart jar
  • 4g of citric acid
  • Washing soda (for solvent reclaim)


IMG 20210608 223040865 copy 800x600.jpg
Fig. 1: Materials.

Process πŸ“œ

Paste 🌡

Mix ice cold water, lime, and cactus in french press for a few minutes to a smooth paste (Fig. 2).


IMG 20210603 183405358 copy 800x600.jpg
Fig. 2: Alkaline cactus paste.

Extract πŸ‘¨πŸΎβ€πŸ”¬

Cover cold paste with chilled ethyl acetate (~0F), mix for for 60 seconds and filter to quart jar. Repeat until quart jar is ~80% full (~5x).


Inspect extract for droplets or particles. If present, remove them. Extract needs to be clean (see Fig. 3).


IMG 20210601 122315740 copy 600x800.jpg
Fig. 3: Ethyl acetate extract.

Crystalize ✨

Drop (do not stir) citric acid into extract. Clouds quickly form first followed after a few hours by mescaline citrate crystals (Fig. 4). Allow crystalization to complete undisturbed (~12 hours).


IMG 20210609 064813073 copy 800x600 1.jpg
Fig. 4: Crystals in ethyl acetate.

Collect πŸ’–

Catch crystals in a coffee filter. Rinse jar/filter with room temperature ethyl acetate a couple times and dry (Fig. 5).


If some crystals stubbornly remain on the jar walls, dissolve them in hot water, dry in a shallow dish, and scrape.


Yield depends on the cactus and is usually between 0.2% to 2% with ~1% being common[2].


IMG 20210603 130102387 copy 600x800 copy 800x600.jpg
Fig. 5: Collected mescaline citrate crystals.


Mass spectrometry (MS) results from solaris analytical[3] indicate the product is very clean mescaline (Fig. 6).


Cactus-extract copy 800x600 1.jpg
Fig. 6: Mass spectrometry result. Peak near 210.5 is mescaline. Lower mass peaks are mescaline with cleaved functional groups. The peak at 239.5 is not attributed to mescaline.

Reclaim Solvent πŸ’š

Reusing solvents is encouraged[4] at the DMT nexus.


Wash spent extract with sodium carbonate saturated water shaking vigorously (emulsions do not form). Citric acid removal is complete when CO2 bubbling stops. Filter any excess calcium carbonate and remove water layer. Freeze and filter out ice crystals. Store for reuse.

Appendix: Development Notes πŸ”¬

Paste 🌡

No improvements were seen with longer basing time, microwaving, drying, or increasing the ionic strength.

Extract πŸ‘¨πŸΎβ€πŸ”¬

Longer and/or warmer pulls resulted in darker color, smaller crystals and more absorbed solvent with no yield benefit.


Chemically drying the extract before salting had no crystallization or yield benefit.

Crystalize ✨

During crystallization, every 233mg of citric acid (H3Cit) react with free base mescaline (Mes) to form to 1g of mescaline citrate (or slightly more if a hydrate is precipitating):


3Mes(↑) + H3Cit(↑) β‡’ 3(MesH)Cit(↓)


Excess citric acid shifts the precipitation reaction to the right (Le Chatelier's principle), helping overcome water and plant material. There is a lot room for excess citric acid in solution since its solubility is 50mg/g in ethyl acetate. The TEK recommends ~5mg/g but since cacti and pull techniques can vary, users may find other values work better for their specific situation (in one example with whole cactus powder 20mg/g was used [5]).


Several factors can make crystals smaller: Reusing ethyl acetate, warmer pulls, longer pulls, higher citric acid concentration, mechanical agitation, and other potential variables. Small crystals can look like a fine powder. Potency does not seem affected by the crystallization appearance, and a powdery precipitate is not a problem unless it becomes difficult to decant/filter.


After the initial crystallization, adding more citric acid and/or moving the extract to the refrigerator did not result in any more precipitation. Moving the extract to the freezer produced ice crystals.


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

Collect πŸ’–

Washing crystals over a filter gave better results than decanting. The filter paper wicked away plant off colors forming a ring. Unlike the pulls, warmer ethyl acetate is an advantage because the goal is to dissolve away plant matter.


The jar wash should be done immediately. If any straggler crystals dry in the jar they stuck to the wall.

References πŸ—οΈ

  1. ↑ Ethyl acetate safety[1]
  2. ↑ Cactus analysis thread[2]
  3. ↑ Solaris analytical service[3]
  4. ↑ On reusing non polar solvent[4]
  5. ↑ Ethyl acetate approach[5]