Difference between revisions of "Chilled Acetone with IPA and Naphtha"

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(β†’β€ŽPaste 🌡)
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βˆ’
In this technique (TEK), microwaved cactus alkaline paste (Fig. 2) is freeze extracted with ethyl acetate (Fig. 3) . Mescaline citrate is precipitated with citric acid (Fig. 4) and collected (Fig. 5).
+
In this technique (TEK), ethyl acetate is used to extract freebase mescaline from cactus lime paste. Citric acid is added to the ethyl acetate to precipitate a mescaline citrate salt (exact salt form is unknown at this time). The mescaline citrate xtals are then filtered through a coffee filter, dried, and collected.
  
  
βˆ’
Thanks to everyone who contributed to this process: someblackguy, Benzyme, shroombee, Metta-Morpheus, Downwardsfromzero, Kash, grollum, Mindlusion, Doubledog, Dreamer042, Loveall, merkin, and others.
+
Thanks to everyone who contributed to this process: someblackguy, Benzyme, shroombee, Metta-Morpheus, Downwardsfromzero, Kash, grollum, Mindlusion, Doubledog, Dreamer042, merkin, _Trip_, Loveall, and others.
  
 
= Safety ⛑️=
 
= Safety ⛑️=
βˆ’
Review ethyl acetate<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 citric acid<ref>Citric acid safety[https://wiki.dmt-nexus.me/Citric_Acid_Safety#Process_.F0.9F.A5.9E]</ref> safety information. Verify solvent MSDS, plastic compatibility, and clean evaporation.
+
Review ethyl acetate<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 citric acid<ref>Citric Acid Safety[https://wiki.dmt-nexus.me/Citric_Acid_Safety#Process_.F0.9F.A5.9E]</ref> safety information. Verify solvent MSDS, plastic compatibility, and clean evaporation.
 +
 
 +
 
 +
This TEK is food safe if food grade materials are used.
  
  
 
Following this advice does not guarantee safety. It is up to each adult individual to make their own decision.
 
Following this advice does not guarantee safety. It is up to each adult individual to make their own decision.
  
βˆ’
= Materials πŸ›’=
+
=MaterialsπŸ›’=
βˆ’
*Quart mason jars
+
βˆ’
*300g water
+
βˆ’
*25g of lime
+
βˆ’
*100g dry cactus powder (outer skin or whole plant)†
+
βˆ’
*Ethyl acetate (e.g. MEK substitute)
+
βˆ’
*Coffee filter ensemble (funnel/basket)
+
βˆ’
*1/2 tsp Citric acid
+
βˆ’
*Washing soda and activated carbon (for solvent reclaim)
+
  
  
βˆ’
†''If starting with fresh cacti, store the dark for 3 months, slice into ~half inch disks, dry in oven at lowest heat setting, and grind to a fine powder (keeping spines is ok)<ref>Fresh cacti process[https://www.dmt-nexus.me/forum/default.aspx?g=posts&m=1102283#post1102283]</ref>.''
+
==ConsumablesπŸ‘©β€πŸŒΎ==
 +
*100g dry cactus powder
 +
*300g water
 +
*25g lime
 +
*1qt ethyl acetate (also sold as "MEK substitute")
 +
*5g of citric acid (15g is another option)
 +
*Washing soda and pH paper (to wash solvent for reuse)
 +
 
 +
==Equipment🏺==
 +
*Medium sized mixing bowl for mixing water/lime/cactus
 +
*French press for pulling cactus with ethyl acetate (a quart jar also works but is not as easy as the French press)
 +
*Quart jar to collect pulls and precipitate mescaline citrate
 +
*Coffee filters, support basket, and funnel
 +
*Kitchen scale to weigh materials
 +
*Magnetic stirrer (optional)
 +
*Microwave (optional)
 +
*Freezer and fridge (optional)
  
  
 
[[File:IMG 20210608 223040865 copy 800x600.jpg|center]]
 
[[File:IMG 20210608 223040865 copy 800x600.jpg|center]]
βˆ’
<center>''Fig. 1: Over the counter materials (french press and lime options).</center>
+
<center>''Fig. 1: Over the counter materials.</center>
  
βˆ’
= Process πŸ“œ=
+
= Process Overview πŸ‘€ =
 +
 
 +
*Make milky lime water
 +
*Thoroughly mix powered cactus into lime water, let sit 10+ minutes
 +
*Pull several times with ethyl acetate, combine pulls, remove excess particles or water droplets
 +
*Add citric acid to combined pulls to precipitate mescaline citrate
 +
*Filter mescaline citrate xtals by pouring solvent and xtals through coffee filter
 +
*Allow ethyl acetate to evaporate from coffee filter and wash
 +
*Recover dried xtals from coffee filter
 +
*Also wash and recover any xtals on the jar walls
 +
 
 +
= Detailed Process πŸ“œ=
  
  
 
== Paste 🌡 ==
 
== Paste 🌡 ==
 +
Make milky water in a bowl by adding lime to water. Mix so there are no lumps of lime. Without giving lime time to settle, gradually add the cactus powder, stirring thoroughly to ensure the cactus is well incorporated into the milky water. It will take roughly 8-10 minutes to gradually incorporate the cactus into the milky water. The last 25% of the cactus powder volume will be easiest to incorporate by a combination of stirring and mashing. The paste will have a fluffy, smooth texture.  When mixed well an airy texture usually develops.  In case of doubt, mix more.  Let sit for at least 10 more minutes.
 +
  
βˆ’
Mix water, lime and cactus in a quart mason jar. Microwave in short bursts<sub>††</sub> uncovered at ~1000W until 200g of water are removed stirring frequently (about 15 to 20 minutes of irradiation time). Watch the microwave to avoid over boil. Paste will go from crumbly to clumpy to crumbly again.
+
Total mixing and basing time is at least 8+10 = 18 minutes. This paste has the same ratios originally used in 69ron's limonene TEK <ref>69ron's Limonene TEK[https://wiki.dmt-nexus.me/69ron%27s_D-Limonene_Mescaline_Extraction]</ref>.
  
  
βˆ’
††''It is possible to skip the shallow baking glass microwave drying and mix the paste directly in the mason jar, but (1) the extract will contain green plant matter and may not be as easy to extract/crystalize, and (2) ethyl acetate may be harder to reuse''
+
'''Microwave option:''' This option breaks down chlorophyll and can make subsequent crystallization and solvent reuse easier. It is believed that this process is more robust to cactus variability. Simply microwave the paste described above in short spurts of a few minutes (watch carefully to avoid over boil), stirring frequently until 2/3 of the water (200g) evaporates. Use a scale to weigh the mixing bowl periodically.  Stop microwaving once the bowl has lost 200 grams of water to evaporation.  Paste will change texture through the process temporarily becoming more liquid, and later becoming loose moist fluff. With this option, the subsequent extract will be tan instead of green and will typically produce larger crystals.
  
  
 
[[File:IMG 20210603 183405358 copy 800x600.jpg|center]]
 
[[File:IMG 20210603 183405358 copy 800x600.jpg|center]]
βˆ’
<center>''Fig. 2: Cactus alkaline paste.</center>
+
<center>''Fig. 2: Cactus lime paste. Appearance can vary.</center>
  
 
== Extract πŸ‘¨πŸΎβ€πŸ”¬==
 
== Extract πŸ‘¨πŸΎβ€πŸ”¬==
βˆ’
Cover paste with freezer chilled ethyl acetate (~0Β°F), cap jar, shake vigorously for 60s, and filter off solvent into separate quart jar. Repeat until quart jar is full (~5x).
+
If available, transfer paste to a French press.  The French press will make it easy to decant the ethyl acetate. Optionally you can use a quart jar, but it's not as easy to decant the ethyl acetate.  The least convenient option is to use a mixing bowl.  If you use a mixing bowl, ensure the material is compatible with ethyl acetate.
  
  
βˆ’
Inspect extract for droplets or particles. If present, remove them. '''Extract needs to be free of debris''' (see Fig. 3).
+
Cover paste with ethyl acetate (~150g) and stir gently for 45-60 seconds. You do not need to stir aggressively as ethyl acetate is very efficient at pulling freebase mescaline from the plant material. Aggressive stirring may cause the plant material to absorb more of the solvent. After stirring, allow to rest for 2 minutes, then decant into quart jar filtering through a coffee filter to catch unwanted plant material. Do not squeeze with the French press, its purpose is to only hold back the paste from falling into the filter. Squeezing can push unwanted plant material or water into the extract. Repeat adding ethyl acetate, stirring, resting, and decanting until quart jar is full.  This will be 5-6 total pulls.
  
  
βˆ’
[[File:IMG 20210618 071818059 copy 600x800.jpg|center]]
+
If the paste absorbs all or most of the ethyl acetate, that's fine.  Just add more ethyl acetate, stir, rest, and decant as explained above.  Do NOT add water or aggressively manipulate the paste in an attempt to force out the ethyl acetate.  Some solvent loss is expected, and is common in dry paste extraction teks.  Even with some solvent stuck in the paste, you will still recover the vast majority of mescaline with your additional pulls.
βˆ’
<center>''Fig. 3: Ethyl acetate extract (yellow or light green color is possible).</center>
+
 
 +
 
 +
All of the extraction pulls should be completed within 30 minutes.  After 30 minutes the paste can begin to congeal, making solvent recovery more difficult and potentially allowing time for unwanted reactions to occur which will complicate the crystallization process.  There is plenty of time to leisurely perform five or six 3-minute pulls by remaining focused on the task.
 +
 
 +
 
 +
Rest the combined extract for at least an hour and then inspect for droplets or particles. If present, allow extract to rest until no more debris form and remove them. '''The extract needs to be clean in order for the crystallization process to happen reliably''' (see Fig. 3). To be sure extract is clean, one extra pass through a fresh coffee filter after settling is recommended.
 +
 
 +
 
 +
'''Cold extract option:''' With this option the paste is cooled in the fridge and fresh ethyl acetate is chilled in the freezer (if using reused solvent filter ice crystals from freezer) for 24h or more. The extraction time per pull is cut down to 60 seconds. The shorter pull time minimizes plant material (such as chlorophyl) in the extract, which we believe helps with crystalization. While a colder extract could theoretically lower the yield, experimentally the yield was ok <ref>Cold extraction results[https://www.dmt-nexus.me/forum/default.aspx?g=posts&m=1108612#post1108612]</ref>.
 +
 
 +
 
 +
[[File:IMG_20210601_122315740_copy_600x800.jpg| center]]
 +
<center>''Fig. 3: Ethyl acetate extract. Color may vary, but extract must be clear and free of debris.</center>
  
 
== Crystalize ✨==
 
== Crystalize ✨==
βˆ’
Drop (do not stir) citric acid into extract. Clouds form quickly, slowly followed by mescaline citrate crystals (Fig. 4). Allow crystalization to complete undisturbed (~12 hours).  
+
Drop 5 grams of citric acid (approximately 5 mg per gram of ethyl acetate) into extract and let it slowly dissolve by diffusion over time. Clouds form, followed by mescaline citrate crystals. Crystals can have different shapes and sometimes also stick to the wall looking transparent. Allow crystalization to complete undisturbed (~24 hours). Swirl extract after crystallization for several minutes to ensure all of the citric acid granules have dissolved. This is sometimes called the "dropping acid" approach.
  
  
βˆ’
Note: If using whole cactus more citric acid may be needed to induce crystallization (up to 1 Tbsp).
+
'''Fast crystalization option:''' Drop 5-15 grams of citric acid (approximately 5-15 mg per gram of ethyl acetate) into extract.  Use a magnetic stirrer or aggressive shaking to quickly dissolve the citric acid and speed up crystallization. This produces a fast crystalization and minimizes crystals that are stuck to the wall. A stirring vortex will go from visible, to not visible as clouds form, to visible again as mescaline citrate precipitates. Crystals may be smaller with this approach, but the vast majority of them will still be caught by a filter in the next step.
  
  
βˆ’
[[File:IMG 20210621 213621074~2 copy 800x600.jpg|center]]<center>''Fig. 4: Crystals in ethyl acetate.</center>
+
[[File:IMG 20210311 144419793 (1) copy 800x600.jpg|center]]<center>''Fig. 4: Crystals in ethyl acetate. Appearance will vary.</center>
  
 
== Collect πŸ’–==  
 
== Collect πŸ’–==  
βˆ’
Swirl crystalized extract to knock off crystals from walls and dissolve any remaining citric acid granules. Catch floating crystals in a coffee filter. Repeat with a small amount (~1oz) of fresh room temperature ethyl acetate until all crystals are in the filter and off color is washed (~2-3x). Dry and collect from filter (Fig. 5).  
+
Catch loose crystals in a coffee filter. Rinse crystals on wall and filter with fresh ethyl acetate (~2-3x until off color is removed). Collect crystals stuck on the jar walls by dissolving them in warm water, evaporating in a shallow dish, and scraping up dry crystals. Combine with the collected crystals from the filter to obtain the final product (Fig. 5).  
  
  
βˆ’
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>.
+
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>. The precise ratio of  mescaline and citrate in the precipitate is not known and is under investigation (see development notes below). Preliminarily data indicate the salt made my this process is ~60% as strong as mescaline HCl and consistent with the salt form (MesH)H<sub>2</sub>Cit. Approximate oral dosage recommendations for mescaline HCl can be found elsewhere<ref>Mescaline Oral Dosage[https://wiki.dmt-nexus.me/Mescaline#Dosages_and_consumption_methods]</ref>.
  
  
 
[[File:IMG 20210603 130102387 copy 600x800 copy 800x600.jpg|center]]
 
[[File:IMG 20210603 130102387 copy 600x800 copy 800x600.jpg|center]]
βˆ’
<center>''Fig. 5: Final mescaline citrate crystals.</center>
+
<center>''Fig. 5: Final mescaline citrate crystals. Appearance will vary.</center>
  
  
Line 86: Line 122:
  
  
βˆ’
Wash extract with sodium carbonate saturated water shaking vigorously (emulsions do not form). Filter any excess calcium carbonate and remove water layer. Freeze and filter out ice crystals. If after multiple reuses a yellow or green color develops it can be removed by resting solvent over activated carbon for several days.
+
Used solvent from the microwave paste process saturates with tan color and can be reused many times. This process is recommended for reuse. The non microwaved paste seems to load the solvent with chlorophyll indefinitely, making it black/opaque and difficult to reuse.
 +
 
 +
 
 +
Wash spent extract with sodium carbonate saturated water (35% by weight). About 1/5 of the solvent volume as saturated water is enough. Shake vigorously (emulsions do not form). CO2 bubbles may be visible during citric acid neutralization. Keep an eye on any bubbles and release any pressure buildup regularly. Neutralization can be optionally verified with pH paper. Filter any excess sodium carbonate/citrate and remove the water layer. Tan solvent can be reused on another microwaved paste.
 +
 
 +
 
 +
If planning to extract cold, chilled reused paste will have ice crystals that can be removed with a filter before the cold extraction.
 +
 
 +
= Frequently Asked Questions ❓ =
 +
'''Q: Why does the TEK have so many options. I feel like I'm choosing my own adventure!'''
 +
 
 +
A: The options exist to help with crystallization for variable starting plant material. The easiest material to crystalize experimentally seems to be aged pachanoi outer skin powder (aged long enough to change color from green to tan). A more difficult material to crystalize is whole bridgessi powder recently dried and ground. For outer skin pachanoi the simpler path has worked for many without adding any options: no microwave, room temp extraction, citric acid diffusion. For whole cactus more work may be needed to keep plant material interfering with crystallization by adding all options: microwave paste, cold extraction, citric acid added with continuous magnetic stirrer. Finally, to grow large crystals good options are to microwave the paste and use cold pulls (while allowing citric acid to diffuse slowly). Current general guidelines (as of summer 2021):
 +
* Outer skin pachanoi: Use no options.
 +
* Whole cactus: Use all options, or at least the microwave option.
 +
*Planning to reuse solvent: Use microwave option.
 +
* Max size crystals: Use outer skin powder with microwave paste and cold extraction options. Fresh ethyl acetate is recommended also. To crystallize, drop acid in an isolated quiet room for 12 hours πŸ˜‰.
 +
 
 +
 
 +
'''Q: Does increasing the basing time increase the yield?'''
 +
 
 +
A: No.  Shroombee has tested 15 minute, 24 hour, and 72 hour basing times and there was no difference in yield.  Other process variables were 8 minutes incorporating milky water with cactus, 6x3 minute pulls, and 15 mg/gram citric acid added with the fast crystallization method.  Loveall has confirmed in his experiments that 10 minute and 24 hour basing times produce the same yield.  So we assume that any basing time from 10 minutes through 72 hours will produce the same yield.  See a detailed explanation in this post.<ref>Basing time tests results[https://www.dmt-nexus.me/forum/default.aspx?g=posts&m=1109045#post1109045]</ref>
 +
 
 +
 
 +
'''Q: What’s the difference between adding 5 mg/gram and 15 mg/gram of citric acid in the fast crystalization method?'''
 +
 
 +
A: In general, adding more citric acid and aggressively stirring or shaking will force xtals to form faster.  However, the xtals will be smaller and more dense.  5mg/g produces fluffier xtals that are more likely to stick to the sides of the container, thus requiring a wash and evaporation process to recover these sticky xtals.  15 mg/g produces smaller, denser xtals that are less likely to stick to the sides of the container.  When pouring through a coffee filter, a negligible amount of tiny xtals will drop through the coffee filter.
 +
 
 +
 
 +
'''Q: What is the upper limit of citric acid that can be added to the extract?'''
 +
 
 +
A: The solubility of citric acid in ethyl acetate is over 50 mg citric acid per gram of ethyl acetate.  Note that plant matter or other unwanted extraction products may affect the solubility.  Stay well under 50 mg/gram to ensure no undissolved citric acid is mixed in with the mescaline citrate.
 +
 
 +
 
 +
'''Q: After adding citric acid, I saw clouds followed by precipitation, but the precipitate reminds me of citric acid. How do I know a mescaline salt is precipitating and not citric acid?'''
 +
 
 +
A: Citric acid does not precipitate and stays in solution because it is well bellow its solubility limit (50mg/g) in the TEK. The white particles that form from the clouds are salts and not citric acid. A thorough swirl may be needed at the end to make sure all the added citric acid has dissolved. Once it has dissolved it will not come out of solution as citric acid.
 +
 
 +
 
 +
'''Q: After adding citric acid, I saw clouds but didn't get any solid precipitation, what gives?'''
 +
 
 +
A: First make sure the TEK instructions were followed, in particular: well mixed paste, short pull times, no squeezing, clean extract free of debris, citric acid is in range, etc. Before adding citric acid, allow the extract to rest, if it has excess water drops will form on the jar walls that need to be decanted. If nothing is precipitating, bring up the citric acid concentration up to 20mg/g and wait a few days. Check the jar walls, a transparent product may have precipitated there (e.g. this has been reported for whole bridgessi<ref>Whole bridgessi precipitate on jar walls [https://mycotopia.net/topic/111136-lets-talk-about-cactus-extractions/#entry1487992]</ref>). Whole cactus seems more difficult to precipitate. A microwave paste treatment and colder pulls with ethyl acetate chilled down to 0F grow larger crystals and should be easier to precipitate because they contain less plant material. If all else fails, pulling the extract with water, evaporating, and washing with fresh ethyl acetate should leave behind a potent residue (dose will be less accurate and can be made proportional to starting cactus amount).
 +
 
 +
 
 +
'''Q: Why don't we know the precise salt form and why does it matter?'''
 +
 
 +
A: We think it depends on what crashes first as the acid and base react. Work is ongoing to experimentally verify what that is. In practice this affects yield and dosage numbers as the (di) hydrogen salts are less potent by weight. Update: Early data indicates the dihydrogen salt is forming in this TEK (see below).
  
 
= Appendix: Development Notes πŸ”¬=
 
= Appendix: Development Notes πŸ”¬=
 
== Paste 🌡==  
 
== Paste 🌡==  
βˆ’
Sodium bases and salts (sodium carbonate, sodium hydroxide, and sodium chloride) where tested but made the paste congeal lowering yields. Exclusive use of calcium cations give the paste a "sandy" structure that has more surface area and gives good yields.
+
No improvements were seen with longer basing time, drying, or increasing the ionic strength.
  
  
βˆ’
In the TEK, two paste treatments on the calcium alkaline paste combine to reduce the amount of plant matter in the extract helping crystallization and purity:
+
Paste made with sodium carbonate saturated water congeals over time and requires long solvent soaks which are darker and don't crystallize to large loose crystals (small sticky crystals were obtained).
  
  
βˆ’
*Microwave Assisted Saponification (MAS<ref>Microwave assisted saponification[https://www.mdpi.com/2304-8158/10/2/445/pdf]</ref>) breaks down esters (generally soluble in ethyl acetate which is itself an ester) into carboxylate ions and organic alcohols. An important example is,
+
In the optional microwave treatment, Microwave Assisted Saponification (MAS<ref>Microwave assisted saponification[https://www.mdpi.com/2304-8158/10/2/445/pdf]</ref>) breaks down esters (generally soluble in ethyl acetate which is itself an ester) into carboxylate ions and organic alcohols. An important example is,
βˆ’
'''<span style="color: Orange"> <div style="text-align: center;">Chlorophyll + 2OH<sup>-</sup> β‡’ Chlorophyllin<sup>--</sup> + Phytol + Ethanol</div></span>'''
+
  
  
βˆ’
* CaCl2 addition to ~20% water solution enables extraction below ~0F (see Fig. 7). The cold temperature reduces general plant matter solubility in ethyl acetate while mescaline's solubility remains favorable.
+
'''<span style="color: Orange"> <div style="text-align: center;">Chlorophyll + 2OH<sup>-</sup> β‡’ Chlorophyllin<sup>--</sup> + Phytol + Ethanol</div></span>'''
  
  
βˆ’
 
+
This breakdown reduces the total amount of plant matter in the extract. In general, large complex esters become smaller organic alcohols. The resulting extract has improved crystallization, but this step is not always required to obtain a product, especially when starting with aged tan outer skin powder.
βˆ’
[[File:Eapfig16.gif|center]]
+
  
 
== Extract πŸ‘¨πŸΎβ€πŸ”¬==  
 
== Extract πŸ‘¨πŸΎβ€πŸ”¬==  
βˆ’
Longer/warmer pulls resulted in darker extract, more difficult crystalization, smaller or sticky crystals, solvent paste absorption, congealing of paste, and no yield benefit.
+
Tests with longer/warmer pulls resulted in darker extract, smaller crystals, solvent paste absorption, congealing of paste, and no yield benefit.
  
  
βˆ’
Chemically drying the extract had no benefits.
+
Chemically drying the extract with a drying agent such as anhydrous CaCl2 or MgSO4 had no benefits in preliminarily experimental example. However, depending on the worker and techniques used, a chemical dry with CaCl2 pellets (available commercially as de-icer) could reduce water content in the solvent and possibly make crystallization easier.
  
 +
== Crystalize ✨==
 +
During crystallization, citric acid ('''H<sub>3</sub>Cit''') reacts with free base mescaline ('''Mes''') to form to form a mescaline citrate salt. The number of mescaline molecules ('''n''') that react with one molecule of citric acid and precipitate is unknown.
  
βˆ’
An additional long room temperature pull on the TEK's spent paste only yielded 4mg of very small crystals, indicating the chilled pulls are efficient.
 
  
βˆ’
== Crystalize ✨==
+
'''<span style="color: Orange"> <div style="text-align: center;">nMes<sub>(↑)</sub> + H<sub>3</sub>Cit<sub>(↑)</sub> β‡’ (MesH)<sub>n</sub>H<sub>3-n</sub>Cit<sub>(↓)</sub></div></span>'''
βˆ’
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’
'''<span style="color: Orange"> <div style="text-align: center;">3Mes<sub>(↑)</sub> + H3Cit<sub>(↑)</sub> β‡’ 3(MesH)Cit<sub>(↓)</sub></div></span>'''
+
Where '''n''' could be 1, 2, or 3. The resulting mescaline citrate salt's strength relative to mescaline HCl is 62%, 81%, and 90% respectively. Preliminarily experimental results indicate n=1<ref>Mescaline Citrate conversion to HCl results[https://www.dmt-nexus.me/forum/default.aspx?g=posts&m=1111858#post1111858]</ref>.
  
  
βˆ’
Excess citric acid shifts the precipitation reaction to the right (Le Chatelier's principle), helping overcome any water and plant material in the solvent. There is a lot room for excess citric acid in solution since its solubility is 50mg/g in ethyl acetate. The TEK suggests ~3mg/g but since cacti and worker techniques can vary, users may find other values work better for their specific situation (in one specific 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>).
+
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 has options ranging from ~6 to 18mg/g and 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>).
  
  
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βˆ’
Other dry organic acids could work. Fumaric, Malic, Tartaric, Ascorbic, Succinic, etc can be tested in future investigations.
+
Other dry organic acids could work. Malic was tested but did not work as well as citric<ref>Malic acid test[https://www.dmt-nexus.me/forum/default.aspx?g=posts&m=1097979#post1097979]</ref>. Fumaric, Tartaric, Ascorbic, Succinic, etc can be tested in future investigations.
 +
 
 +
 
 +
10% sulfuric acid was tested and while some crystals formed, a separate liquid layer also appeared making the process not practical.
  
 
== Collect πŸ’–==  
 
== Collect πŸ’–==  
  
  
βˆ’
Washing crystals in a filter appears to wick away plant colors and superior to decanting. Unlike the pulls, warmer ethyl acetate is preferred to wash off plant matter.
+
Washing crystals in a filter appears to wick away plant colors and superior to decanting.
  
  
βˆ’
The quart jar wash should be done immediately. If any straggler crystals dry in the jar they may stick to the wall. To recover from such a situation, dissolve stuck crystals in hot water, dry in a shallow dish, and scrape.
+
The washed crystals in the filter can also be dissolved in warm water along with any wall crystals. This will give then final product a uniform appearence.
  
 
= References πŸ—οΈ=
 
= References πŸ—οΈ=
 
<references/>
 
<references/>

Revision as of 10:32, 28 July 2021

CIELO

Introduction πŸ™

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


In this technique (TEK), ethyl acetate is used to extract freebase mescaline from cactus lime paste. Citric acid is added to the ethyl acetate to precipitate a mescaline citrate salt (exact salt form is unknown at this time). The mescaline citrate xtals are then filtered through a coffee filter, dried, and collected.


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

Safety ⛑️

Review ethyl acetate[1] and citric acid[2] safety information. Verify solvent MSDS, plastic compatibility, and clean evaporation.


This TEK is food safe if food grade materials are used.


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

MaterialsπŸ›’

ConsumablesπŸ‘©β€πŸŒΎ

  • 100g dry cactus powder
  • 300g water
  • 25g lime
  • 1qt ethyl acetate (also sold as "MEK substitute")
  • 5g of citric acid (15g is another option)
  • Washing soda and pH paper (to wash solvent for reuse)

Equipment🏺

  • Medium sized mixing bowl for mixing water/lime/cactus
  • French press for pulling cactus with ethyl acetate (a quart jar also works but is not as easy as the French press)
  • Quart jar to collect pulls and precipitate mescaline citrate
  • Coffee filters, support basket, and funnel
  • Kitchen scale to weigh materials
  • Magnetic stirrer (optional)
  • Microwave (optional)
  • Freezer and fridge (optional)


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Fig. 1: Over the counter materials.

Process Overview πŸ‘€

  • Make milky lime water
  • Thoroughly mix powered cactus into lime water, let sit 10+ minutes
  • Pull several times with ethyl acetate, combine pulls, remove excess particles or water droplets
  • Add citric acid to combined pulls to precipitate mescaline citrate
  • Filter mescaline citrate xtals by pouring solvent and xtals through coffee filter
  • Allow ethyl acetate to evaporate from coffee filter and wash
  • Recover dried xtals from coffee filter
  • Also wash and recover any xtals on the jar walls

Detailed Process πŸ“œ

Paste 🌡

Make milky water in a bowl by adding lime to water. Mix so there are no lumps of lime. Without giving lime time to settle, gradually add the cactus powder, stirring thoroughly to ensure the cactus is well incorporated into the milky water. It will take roughly 8-10 minutes to gradually incorporate the cactus into the milky water. The last 25% of the cactus powder volume will be easiest to incorporate by a combination of stirring and mashing. The paste will have a fluffy, smooth texture. When mixed well an airy texture usually develops. In case of doubt, mix more. Let sit for at least 10 more minutes.


Total mixing and basing time is at least 8+10 = 18 minutes. This paste has the same ratios originally used in 69ron's limonene TEK [3].


Microwave option: This option breaks down chlorophyll and can make subsequent crystallization and solvent reuse easier. It is believed that this process is more robust to cactus variability. Simply microwave the paste described above in short spurts of a few minutes (watch carefully to avoid over boil), stirring frequently until 2/3 of the water (200g) evaporates. Use a scale to weigh the mixing bowl periodically. Stop microwaving once the bowl has lost 200 grams of water to evaporation. Paste will change texture through the process temporarily becoming more liquid, and later becoming loose moist fluff. With this option, the subsequent extract will be tan instead of green and will typically produce larger crystals.


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Fig. 2: Cactus lime paste. Appearance can vary.

Extract πŸ‘¨πŸΎβ€πŸ”¬

If available, transfer paste to a French press. The French press will make it easy to decant the ethyl acetate. Optionally you can use a quart jar, but it's not as easy to decant the ethyl acetate. The least convenient option is to use a mixing bowl. If you use a mixing bowl, ensure the material is compatible with ethyl acetate.


Cover paste with ethyl acetate (~150g) and stir gently for 45-60 seconds. You do not need to stir aggressively as ethyl acetate is very efficient at pulling freebase mescaline from the plant material. Aggressive stirring may cause the plant material to absorb more of the solvent. After stirring, allow to rest for 2 minutes, then decant into quart jar filtering through a coffee filter to catch unwanted plant material. Do not squeeze with the French press, its purpose is to only hold back the paste from falling into the filter. Squeezing can push unwanted plant material or water into the extract. Repeat adding ethyl acetate, stirring, resting, and decanting until quart jar is full. This will be 5-6 total pulls.


If the paste absorbs all or most of the ethyl acetate, that's fine. Just add more ethyl acetate, stir, rest, and decant as explained above. Do NOT add water or aggressively manipulate the paste in an attempt to force out the ethyl acetate. Some solvent loss is expected, and is common in dry paste extraction teks. Even with some solvent stuck in the paste, you will still recover the vast majority of mescaline with your additional pulls.


All of the extraction pulls should be completed within 30 minutes. After 30 minutes the paste can begin to congeal, making solvent recovery more difficult and potentially allowing time for unwanted reactions to occur which will complicate the crystallization process. There is plenty of time to leisurely perform five or six 3-minute pulls by remaining focused on the task.


Rest the combined extract for at least an hour and then inspect for droplets or particles. If present, allow extract to rest until no more debris form and remove them. The extract needs to be clean in order for the crystallization process to happen reliably (see Fig. 3). To be sure extract is clean, one extra pass through a fresh coffee filter after settling is recommended.


Cold extract option: With this option the paste is cooled in the fridge and fresh ethyl acetate is chilled in the freezer (if using reused solvent filter ice crystals from freezer) for 24h or more. The extraction time per pull is cut down to 60 seconds. The shorter pull time minimizes plant material (such as chlorophyl) in the extract, which we believe helps with crystalization. While a colder extract could theoretically lower the yield, experimentally the yield was ok [4].


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Fig. 3: Ethyl acetate extract. Color may vary, but extract must be clear and free of debris.

Crystalize ✨

Drop 5 grams of citric acid (approximately 5 mg per gram of ethyl acetate) into extract and let it slowly dissolve by diffusion over time. Clouds form, followed by mescaline citrate crystals. Crystals can have different shapes and sometimes also stick to the wall looking transparent. Allow crystalization to complete undisturbed (~24 hours). Swirl extract after crystallization for several minutes to ensure all of the citric acid granules have dissolved. This is sometimes called the "dropping acid" approach.


Fast crystalization option: Drop 5-15 grams of citric acid (approximately 5-15 mg per gram of ethyl acetate) into extract. Use a magnetic stirrer or aggressive shaking to quickly dissolve the citric acid and speed up crystallization. This produces a fast crystalization and minimizes crystals that are stuck to the wall. A stirring vortex will go from visible, to not visible as clouds form, to visible again as mescaline citrate precipitates. Crystals may be smaller with this approach, but the vast majority of them will still be caught by a filter in the next step.


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Fig. 4: Crystals in ethyl acetate. Appearance will vary.

Collect πŸ’–

Catch loose crystals in a coffee filter. Rinse crystals on wall and filter with fresh ethyl acetate (~2-3x until off color is removed). Collect crystals stuck on the jar walls by dissolving them in warm water, evaporating in a shallow dish, and scraping up dry crystals. Combine with the collected crystals from the filter to obtain the final product (Fig. 5).


Yield depends on the cactus and is usually between 0.2% to 2% with ~1% being common[5]. The precise ratio of mescaline and citrate in the precipitate is not known and is under investigation (see development notes below). Preliminarily data indicate the salt made my this process is ~60% as strong as mescaline HCl and consistent with the salt form (MesH)H2Cit. Approximate oral dosage recommendations for mescaline HCl can be found elsewhere[6].


IMG 20210603 130102387 copy 600x800 copy 800x600.jpg
Fig. 5: Final mescaline citrate crystals. Appearance will vary.


Mass spectrometry (MS) results from solaris analytical[7] 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[8] at the DMT nexus.


Used solvent from the microwave paste process saturates with tan color and can be reused many times. This process is recommended for reuse. The non microwaved paste seems to load the solvent with chlorophyll indefinitely, making it black/opaque and difficult to reuse.


Wash spent extract with sodium carbonate saturated water (35% by weight). About 1/5 of the solvent volume as saturated water is enough. Shake vigorously (emulsions do not form). CO2 bubbles may be visible during citric acid neutralization. Keep an eye on any bubbles and release any pressure buildup regularly. Neutralization can be optionally verified with pH paper. Filter any excess sodium carbonate/citrate and remove the water layer. Tan solvent can be reused on another microwaved paste.


If planning to extract cold, chilled reused paste will have ice crystals that can be removed with a filter before the cold extraction.

Frequently Asked Questions ❓

Q: Why does the TEK have so many options. I feel like I'm choosing my own adventure!

A: The options exist to help with crystallization for variable starting plant material. The easiest material to crystalize experimentally seems to be aged pachanoi outer skin powder (aged long enough to change color from green to tan). A more difficult material to crystalize is whole bridgessi powder recently dried and ground. For outer skin pachanoi the simpler path has worked for many without adding any options: no microwave, room temp extraction, citric acid diffusion. For whole cactus more work may be needed to keep plant material interfering with crystallization by adding all options: microwave paste, cold extraction, citric acid added with continuous magnetic stirrer. Finally, to grow large crystals good options are to microwave the paste and use cold pulls (while allowing citric acid to diffuse slowly). Current general guidelines (as of summer 2021):

  • Outer skin pachanoi: Use no options.
  • Whole cactus: Use all options, or at least the microwave option.
  • Planning to reuse solvent: Use microwave option.
  • Max size crystals: Use outer skin powder with microwave paste and cold extraction options. Fresh ethyl acetate is recommended also. To crystallize, drop acid in an isolated quiet room for 12 hours πŸ˜‰.


Q: Does increasing the basing time increase the yield?

A: No. Shroombee has tested 15 minute, 24 hour, and 72 hour basing times and there was no difference in yield. Other process variables were 8 minutes incorporating milky water with cactus, 6x3 minute pulls, and 15 mg/gram citric acid added with the fast crystallization method. Loveall has confirmed in his experiments that 10 minute and 24 hour basing times produce the same yield. So we assume that any basing time from 10 minutes through 72 hours will produce the same yield. See a detailed explanation in this post.[9]


Q: What’s the difference between adding 5 mg/gram and 15 mg/gram of citric acid in the fast crystalization method?

A: In general, adding more citric acid and aggressively stirring or shaking will force xtals to form faster. However, the xtals will be smaller and more dense. 5mg/g produces fluffier xtals that are more likely to stick to the sides of the container, thus requiring a wash and evaporation process to recover these sticky xtals. 15 mg/g produces smaller, denser xtals that are less likely to stick to the sides of the container. When pouring through a coffee filter, a negligible amount of tiny xtals will drop through the coffee filter.


Q: What is the upper limit of citric acid that can be added to the extract?

A: The solubility of citric acid in ethyl acetate is over 50 mg citric acid per gram of ethyl acetate. Note that plant matter or other unwanted extraction products may affect the solubility. Stay well under 50 mg/gram to ensure no undissolved citric acid is mixed in with the mescaline citrate.


Q: After adding citric acid, I saw clouds followed by precipitation, but the precipitate reminds me of citric acid. How do I know a mescaline salt is precipitating and not citric acid?

A: Citric acid does not precipitate and stays in solution because it is well bellow its solubility limit (50mg/g) in the TEK. The white particles that form from the clouds are salts and not citric acid. A thorough swirl may be needed at the end to make sure all the added citric acid has dissolved. Once it has dissolved it will not come out of solution as citric acid.


Q: After adding citric acid, I saw clouds but didn't get any solid precipitation, what gives?

A: First make sure the TEK instructions were followed, in particular: well mixed paste, short pull times, no squeezing, clean extract free of debris, citric acid is in range, etc. Before adding citric acid, allow the extract to rest, if it has excess water drops will form on the jar walls that need to be decanted. If nothing is precipitating, bring up the citric acid concentration up to 20mg/g and wait a few days. Check the jar walls, a transparent product may have precipitated there (e.g. this has been reported for whole bridgessi[10]). Whole cactus seems more difficult to precipitate. A microwave paste treatment and colder pulls with ethyl acetate chilled down to 0F grow larger crystals and should be easier to precipitate because they contain less plant material. If all else fails, pulling the extract with water, evaporating, and washing with fresh ethyl acetate should leave behind a potent residue (dose will be less accurate and can be made proportional to starting cactus amount).


Q: Why don't we know the precise salt form and why does it matter?

A: We think it depends on what crashes first as the acid and base react. Work is ongoing to experimentally verify what that is. In practice this affects yield and dosage numbers as the (di) hydrogen salts are less potent by weight. Update: Early data indicates the dihydrogen salt is forming in this TEK (see below).

Appendix: Development Notes πŸ”¬

Paste 🌡

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


Paste made with sodium carbonate saturated water congeals over time and requires long solvent soaks which are darker and don't crystallize to large loose crystals (small sticky crystals were obtained).


In the optional microwave treatment, Microwave Assisted Saponification (MAS[11]) breaks down esters (generally soluble in ethyl acetate which is itself an ester) into carboxylate ions and organic alcohols. An important example is,


Chlorophyll + 2OH- β‡’ Chlorophyllin-- + Phytol + Ethanol


This breakdown reduces the total amount of plant matter in the extract. In general, large complex esters become smaller organic alcohols. The resulting extract has improved crystallization, but this step is not always required to obtain a product, especially when starting with aged tan outer skin powder.

Extract πŸ‘¨πŸΎβ€πŸ”¬

Tests with longer/warmer pulls resulted in darker extract, smaller crystals, solvent paste absorption, congealing of paste, and no yield benefit.


Chemically drying the extract with a drying agent such as anhydrous CaCl2 or MgSO4 had no benefits in preliminarily experimental example. However, depending on the worker and techniques used, a chemical dry with CaCl2 pellets (available commercially as de-icer) could reduce water content in the solvent and possibly make crystallization easier.

Crystalize ✨

During crystallization, citric acid (H3Cit) reacts with free base mescaline (Mes) to form to form a mescaline citrate salt. The number of mescaline molecules (n) that react with one molecule of citric acid and precipitate is unknown.


nMes(↑) + H3Cit(↑) β‡’ (MesH)nH3-nCit(↓)


Where n could be 1, 2, or 3. The resulting mescaline citrate salt's strength relative to mescaline HCl is 62%, 81%, and 90% respectively. Preliminarily experimental results indicate n=1[12].


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 has options ranging from ~6 to 18mg/g and 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 [13]).


Several factors can make crystals smaller: Reusing ethyl acetate, longer/warmer 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. Malic was tested but did not work as well as citric[14]. Fumaric, Tartaric, Ascorbic, Succinic, etc can be tested in future investigations.


10% sulfuric acid was tested and while some crystals formed, a separate liquid layer also appeared making the process not practical.

Collect πŸ’–

Washing crystals in a filter appears to wick away plant colors and superior to decanting.


The washed crystals in the filter can also be dissolved in warm water along with any wall crystals. This will give then final product a uniform appearence.

References πŸ—οΈ

  1. ↑ Ethyl acetate safety[1]
  2. ↑ Citric Acid Safety[2]
  3. ↑ 69ron's Limonene TEK[3]
  4. ↑ Cold extraction results[4]
  5. ↑ Cactus analysis thread[5]
  6. ↑ Mescaline Oral Dosage[6]
  7. ↑ Solaris analytical service[7]
  8. ↑ On reusing non polar solvent[8]
  9. ↑ Basing time tests results[9]
  10. ↑ Whole bridgessi precipitate on jar walls [10]
  11. ↑ Microwave assisted saponification[11]
  12. ↑ Mescaline Citrate conversion to HCl results[12]
  13. ↑ Ethyl acetate approach[13]
  14. ↑ Malic acid test[14]