Difference between revisions of "CIELO"
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'''Q: The cactus paste turned to goo in ethyl acetate very quickly and I couldn't finish
'''Q: The cactus paste turned to goo in ethyl acetate very quickly and I couldn't finish timed pulls '''
A: Try using less water next time. Excess water can accelerate 'goofication' of the cactus paste. Not all cactus powder is the same, so a 'feel' is needed to achieve the right paste consistency. An absolute pre deteemined water ammount is only a starting guideline.
A: Try using less water next time . Excess water can accelerate 'goofication' of the cactus paste . Not all cactus powder is the same, so a 'feel' is needed to achieve the right paste consistency . An absolute pre deteemined water ammount is only a starting guideline.
= Appendix: Development Notes 🔬=
= Appendix: Development Notes 🔬=
Revision as of 09:26, 16 August 2022
- 1 Introduction 🙏
- 2 Safety ⛑️
- 3 Materials🛒
- 4 Process Overview 👀
- 5 Detailed Process 📜
- 6 Frequently Asked Questions ❓
- 7 Appendix: Development Notes 🔬
- 8 References 🗝️
CIELO stands for Crystals In Ethyl-acetate Laizily Over-the-counter. In this process, mescaline from cactus is precipitated in ethyl acetate as monomescaline citrate crystals (see Fig. 1). This technique (TEK) is specialized for catus, is relatively simple, and avoids harsh chemicals. Other organic acids besides citric can be used as described in the appendix.
The process needs to be followed closely to ensure good results. A good resource for beginners is the no-nonsense TEK description by Cheelin.
Thanks to everyone who contributed to this process: someblackguy, benzyme, shroombee, Metta-Morpheus, Downwardsfromzero, Kash, grollum, Mindlusion, Doubledog, Dreamer042, merkin, _Trip_, Cheelin, Highlightprotein, Loveall, orchidist, and others.
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 personal decisions.
- 300g water
- 25g Ca(OH)2 (lime)
- 100g dry cactus†
- 1qt ethyl acetate (sometimes sold as "MEK substitute")††
- 2.5g of citric acid (~1/2 tsp)
- Washing soda (Na2CO3) saturated water for solvent reuse
† Ingredients can be scaled down to 5g of cactus powder to perform a TEK test run. This is encouraged for beginners to get a feel for the process before commiting more material.
†† Depending on pull technique using two quarts of ethyl acetate may yield a little more mescaline (up to ~+10%). See extraction section for more details.
- Knife, paper bag, dehydrator, food processor, and coffee grinder (to harvest plant, store cutting, and make cactus powder)
- French press (optional, recommended for extraction)
- Kitchen scale (to measure ingredients)
- Coffee filters, support basket, and funnel
- Quart mason glass jars with lids
- Milligram scale (to measure product)
- Pipette, separatory funnel, or freezer (for solvent reuse water separation)
Process Overview 👀
In short:🌵➠🟢➠🧑🏾🔬➠✨➠💖➠💚, where,
- 🌵: Grow, harvest, store, dry, and grind cactus to a fine powder
- 🟢: Mix cactus powder to a wet alkaline paste
- 🧑🏾🔬:Pull paste with ethyl acetate
- ✨: Precipitate mescaline from ethyl acetate with citric acid
- 💖: Collect and wash monomescaline citrate crystals
- 💚: Store ethyl acetate for reuse
Detailed Process 📜
Grow and harvest cactus. Store cuttings in a dark place for at least 3 months (e.g. in a paper bag or wrapped in newspaper). Data shows dark storage increases mescaline content, and that the top part of the plant contains more mescaline. Chop whole cacti (into for example ~1/4 inch thick slices) and dry them with (for example) a food dehydrator at low temp (~115 F).
All parts of the cactus can be used. Outer green skin yields more than the inner white core for the same dry mass, but mescaline is present in both parts of the plant. Outer waxy layers and spines do not yield product, they can optionally be removed but are not detrimental to the extraction.
Grind dry cactus slices to a fine powder. This can be done in two steps, first through a food processor (coarse grind) and then through a coffee grinder (fine grind).
It is very important to make a uniform cactus powder that is dry (<10% moisture) and finely ground. Clouds of fine dust fly into the air when handling a good powder, reminiscent of flour (but green). Store properly sealed to avoid moisture absorption over time (redry before extracting if needed). Old cactus powder may change to a tan color, and still works well in this process (extract may be tan instead of green).
Reserve ~30ml of water. Make milky water in a french press, quart jar, or mixing bowl by mixing lime with the rest of the water (~270ml). 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. Goal is to get a "stiff mashed potatoes" consistency (Fig. 3), gradually add the reserved water as needed to achieve this consistency. With practice and experience with a specific powder, a know water amount can be added at the beginning.
If the paste is too dry and clumpy, free base conversion and/or ethyl acetate penetration diminishes lowering yields. If there is too much water the paste will emulsify with ethyl acetate lowering yields and wasting solvent (see FAQ). However, the water process window for a good paste is large, estimated at ±30ml, and with attention to detail a good paste can be made. Achieving the right paste consistency is more important than the exact amount of water added (which may vary for different cacti and pulp/skin ratios). Ideal paste consistency is reminiscent of stiff yet fluffy mashed potatoes. Drier consistency and more compact paste (~play doh) has been reported to give good yields. Give paste homogeneous texture by stirring vigorously for at least 5 minutes. In case of doubt, mix more.
This paste has the same ratios originally used in 69ron's limonene TEK . However, with ethyl acetate it is very important to mix the paste well and obtain the proper texture. Some elbow grease is required, so mix with intent.
If available, the paste should be in a french press. The french press will make it easy to decant the ethyl acetate. Optionally the paste can be in a a quart jar, but it's not as easy to decant the ethyl acetate. It is possible to have the paste in a mixing bowl, but decanting may be cumbersome.
Cover paste ethyl acetate (~200g) and stir for one minute. Do not to stir too aggressively as that may cause plant material to absorb excess solvent. A good paste becomes sandy during extraction and is very easy to handle, but other textures also work. After stirring, rest for two minutes, and decant into a quart jar filtering through a paper coffee filter (do NOT skip or substitute the coffee filter). If using a french press (preferred), only squeeze lightly to accelerate decanting (keeping plastic parts away from the solvent). Squeezing too aggressively can release unwanted water into the extract which will need to be separated in the next step.
If the paste absorbs all or most of the ethyl acetate during the first pull, 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 absorption during the first pull is common. If an emulsion forms see the FAQ below.
Repeat the extraction with ~125g of ethyl acetate until the extraction jar is full (5-6 total pulls). It is normal for paste to become more sticky as the pulls progress. A small yield boost can be done by optionally doing more pulls into a second jar. This second jar is also a good check on the effectiveness of the pulls in the main jar the first time this TEK is performed. Poor technique will give a larger yield boost in the second jar, <10% boost is considered good.
All of the extraction pulls should be completed within 45 minutes. After 45 minutes the paste can begin to congeal, making solvent penetration and recovery more difficult. There is plenty of time to lazily perform the pulls by remaining focused on the task.
Rest the combined extract for at least an hour and then inspect for droplets or particles. More aggressive paste squeezing can result in small water droplets that need time to settle and accumulate so they can be removed. If debris are seen, allow extract to rest until no more debris form and remove them. With experience and confidence this step can be skipped if no debris are seen consistently. Conversely, inexperienced beginners are encouraged to allow extract to rest for 24 hours in a refrigerator. The extract needs to be clear, particle free, and without water droplets for the crystallization process to happen reliably (see Fig. 4). Water solubility in ethyl acetate decreases with temperarure. Resting temperature should not be higher than the crystalization temperature (next step) to avoid water dropping out of solution at the crystalization temperature and potentially causing goo.
Stir ~2.5 grams (~1/2 teaspoon) of citric acid powder granules into extract until citric acid dissolves clouding the extract. This should only take a few minutes. Leave extract undisturbed for a few hours. Crystals of monomescaline citrate should begin to appear after a few hours. Crystals can have different shapes and can stick to the wall (sometimes looking transparent and difficult to see). After the solution clears, allow crystalization to complete (~up to 72 hours).
Fast crystalization option: Add up to 15 grams of citric acid powder granules 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. If shaking, clouds form and disappear within minutes, leaving product behind. Crystals will be smaller with this approach and look like a powder, but the vast majority of them will still be caught by a filter in the next step. They are denser and easier to pack in capsules, but not as pretty to look at. As with the previous option, allow crystalization to complete undisturbed (~72 hours).
If no crystals form and goo appears, see FAQ below.
Swirl ethyl acetate to knock crystals loose. Crystals that cling to the wall can sometimes be dislodged by shaking or with a knife/spoon. Send solvent trough a double coffee filter to catch loose crystals. Rinse any crystals remaining on jar walls with fresh ethyl acetate and send wash through filter to also wash the crystals there and collect any new crystals that are dislodged (repeat ~2-3x until off color is mostly removed).
After the solvent washes are fully dry in the filter and jar:
- Collect crystals in the filter by simply sliding them off. Rubbing the inside of the filter against itself with the palms of the hands can help loosen the last bit of crystals. Do not introduce water into the filter since it could pick up plant matter left behind by ethyl acetate in the filter fibers (or if this is done, keep this water separate from the rest of the product in case it has plant matter).
- Collect crystals that remain stuck on the jar walls (if any) by dissolving them in warm water, evaporating water in a shallow dish, and scraping. When deciding if it is necessary to do this step keep in mind that sometimes the wall crystals form a transparent layer difficult to see.
Combine with the collected crystals to obtain the final product (Fig. 6). Reagent results for the product from this TEK have been published by _Trip_.
Yield depends on the cactus and is usually between 0.2% to 2% with ~1.2% being common. The product is monomescaline citrate salt, (MesH)H2Cit (see appendix), which is ~61% as strong as MesHCl. Approximate oral dosage recommendations for mescaline  roughly converted to monomescaline citrate based on molecular weight and subjective user experience:
- Threshold: 100 - 200 mg
- Light: 200 - 350 mg
- Common: 350 - 700 mg
- Strong: 700 - 1400 mg
- Heavy: 1400 mg+
Attempting to smoke the product is not recommended as potentially unwanted compounds can form .
Mass spectrometry (MS) results from solaris analytical indicate the product is very clean mescaline (Fig. 7) in one example where pachanoi was used. It is unknown if cacti with different starting starting alkaloid profiles would give the same result, and more data is needed to make that claim.
Reusing solvents is encouraged at the DMT nexus.
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. Rest washed solution until clear (up to a day or more).
Remove the water layer with a pipette or separatory funnel. Freezing the solvent and filtering the ice slush that forms with a metal strainer is also an option. Finally, decant off any excess solid sodium carbonate/citrate.
Frequently Asked Questions ❓
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.
Q: I got a en emulsion while pulling, what do I do?
A:If the paste and solvent form an emulsion, it is likely that the paste was too watery. Add lime and dry magnesium sulfate until the paste becomes chunky again and solvent is released. Keep the lime to magnesium sulfate ratio above 1 to ensure paste remains alkaline. Next time, use less water to make the paste.
Q: What’s the difference between the two crystalization methods?
A: In general, adding more citric acid and aggressively stirring or shaking will:
- Force crystals to form faster
- Form smaller and denser crystals less likely to stick to the jar walls
- Cause a negligible amount of tiny crystals to 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 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, nothing precipitated, what gives?
A: Check the jar walls, a transparent product may have precipitated there (e.g. this has been reported for whole bridgessi). If product bid not present on walls as a transparent film, bring up the citric acid concentration up to 20mg/g or more (stay below 40mg/g due to solubility concerns) and wait a few days. Keep in mind that if your cactus is not active, no mescaline citrate will form. If all else fails, pulling the salted extract with water, evaporating, and washing citric acid with fresh ethyl acetate should leave behind a residue containing any mescaline in the cactus (dose will be less accurate and can be made proportional to starting cactus amount). The crystallization temperature should not be colder than the previous extraction settling temperature. Water layer formation is sensitive to temperature, and lower temperatures can producte a new water layer since the water solubility in ethyl acetate is decrease.
Q: After adding citric acid, goo/oil precipitated instead of crystals, what gives?
This is the most common issue people encouncer. Cause/Causes are unknown, but there are some theories:
- Poor TEK execution: This is believed to be the most common issue. Make sure the TEK instructions were followed, in particular: well mixed paste, short pull times, clean extract free of debris (including water droplets), citric acid is in range, rest temperature not higher than xtalization temperature, etc. In particular, before adding citric acid, allow the extract to rest at a temperature not hotter than the planned xtalization temperature and ensure any water droplets stay behind when decanting.
- Cactus powder: Some cacti or parts of some cacti may cause goo. orchidist showed that in one case, use of fumaric acid resulted in crystals, while citric acid resulted in goo.
- Xtalization dynamics: A separate water phase presenting as a visible layer on the bottom of the solution with salt/acid could separate before xtals form, resulting in an oily mixture of citric acid and mescaline citrate. One proposed, but not yet tested solution to this problem is to create a saturated solution of citric acid in ethyl acetate, and add that dropwise into the extract, instead of direct addition of solid citric acid crystals. Another suggestion is to chemichally dry the ehtyl acetate before salting. An effective and easy to use drying agent example is K2CO3. Drying the solvent may also be a "guardrail" for people learning how to execute the TEK.
- Rest/decanting and crystalization temperatures: Water solubility in ethyl acetate decreases with temperarure. If the crystalization temperature is lower than the rest/decanting temperature water may crash from solution causing goo.
If you see or overcome goo, please report it on the forum. You could help solve this issue that some workers come across.
Q: I recovered the goo/oil precipitate instead of crystals, what do I do?
A: In one example from Cheelin the goo was 65% mescaline citrate. There are four main options. (1) Do an A/B extraction on the goo, (2) If a TEK execution is suspect, add the goo to cactus paste and do the TEK properly, increasing citric acid by the amount of expected mescaline present in the goo, (3) decant off the solvent and cover the goo in fresh EA, it has been observed that crystals can grow out of the goo after a few days sitting in fresh solvent and stirring can help the process move along. If crystal formation stops and there is still goo left, discard the solvent and add more (4) if goo forms repeatedly, retry the TEK using fumaric acid instead of citric acid (fumaric may be more robust at forming xtals)
Q: How quickly can the extraction process be done?
A: With experience, it is possible to go go from raw cactus powder to dry crystals in under an hour by choosing the fast crystalization method shaking the salted extract vigorously. Current documented world record is 48 minutes to go from cactus powder to dry mescaline crystals ready to use..
Q: The cactus paste turned to goo in ethyl acetate very quickly and I couldn't finish the timed pulls with a sandy consistency. How can I give myself more time?
A: Try using less water next time amd keep resting powder time to 10 minutes. Excess water can accelerate 'goofication' of the cactus paste and decrease yield as it is harder to extract from goo due to poor solvent penetration. Not all cactus powder is the same, so a 'feel' is needed to achieve the right paste consistency before pulling. An absolute pre deteemined water ammount is only a starting guideline.
Appendix: Development Notes 🔬
No improvements were seen with longer basing time, paste oven drying, or increasing the ionic strength with CaCl2. Microwave treatment or boiling water resulted in a small yield loss.
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).
Use of lime and boiling water causes the saponification of chlorophyll over time :
Chlorophyll is soluble in Ethyl Acetate, but Chlorophyllin and Phytol are not. Saponification in hot water gives an extract with less plant matter and lighter color, however yields where slightly lower with this approach.
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 anhydrous CaCl2 had no benefits, while drying with MgSO4 was problematic. 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. Washing soda (when sold as Na2CO3 in monohydrate form, or when making the anhydrous form from baking soda with an oven) may also dry the extract and be beneficial in such cases (but that is currently an assumption based on other lab techniques).
During crystallization, excess citric acid (H3Cit) reacts with free base mescaline (Mes) to form to form the monomescaline citrate salt (MesH)H2Cit:
Monomescaline citrate salt's strength relative to mescaline HCl is 61% (assuming no hydrate formation). By not using excess citric acid, different salt forms can be precipitated, but that process is more complex than the simpler excess citric acid approach.
There is a lot room for excess citric acid in solution since its solubility is 50mg/g in ethyl acetate. In extracts with crystallization issues, adding more citric acid can help force precipitation: in one example with whole cactus powder 20mg/g was used .
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 does not result in any more precipitation. Moving the extract to the freezer produced ice crystals.
Other dry organic acids have been tested,. Fumaric and tartaric crystalized well as monomescaline and could be a substitute for citric. Malic also crystallized but took longer to do so, and a crude mass measurement indicated the dimescaline form. See Fig. 8 for resulting citrate, tartrate, fumarate, and malate crystals. Succinic also crystalized from a chemichally dried extract (without drying xtals did not form) as the monomescaline form (see Fig. 9). Ascorbic, and benzoic did not crystalize well. Other organic acids (lactic, oxalic, etc) have not been tested yet at the time of this writing. For the organic acids that crystalized, Mescaline HCl equivalent is (assuming no hydrate formation):
- Monomescaline Citrate: 61%
- Monomescaline Tartrate: 69%
- Monomescaline Fumarate or Succinate: 75%
- Dimescaline Malate: 89%
For a comprehensive reference of mescaline salt weight conversion see orchidist's calculator.
10% sulfuric acid was tested and while some crystals formed, a separate liquid layer also appeared making the process not practical. HCl has not been tested as it may break down ethyl acetate.
Washing crystals in a filter appears to wick away plant colors and is superior to decanting if the goal is white xtals.
The washed crystals in the filter can be dissolved in warm water after collecting them (do not "pull" filter with water as that can be a source of plant matter) along with any wall crystals. This will give then final product a uniform appearance with large needles forming during slow water evaporation.
Dark extract can be cleared up with activated carbon (also called activated charcoal). Use dustless pellets (typically rinsed with water and dried before use).
While it is easier to work with a solvent that is not dark, a quantifiably benefit of using activated charcoal to decolor the used solvent is not clear (pun intended). The environmental benefit of regenerating a colorless solvent is in question since ethyl acetate is easy to produce and activated charcoal requires resources to manufacture.
- Cheelin's no nonsense TEK description
- Ethyl acetate safety
- Citric Acid Safety
- Cheelin's beginner recommendation
- Cactus growing guide
- Dark storage data
- Paper with vertical signal
- Result for different cactus parts
- Minimum water paste
- Excessive water paste
- Cheelin paste making skews
- Drier paste example
- 69ron's Limonene TEK
- Second set of pulls 
- Reagent results
- Cactus analysis thread
- Mescaline Oral Dosage
- Citric acid heat degradation
- Solaris analytical service
- On reusing non polar solvent
- Basing time tests results
- Lime and magnesium sulfate ratio vs pH
- Whole bridgessi precipitate on jar walls 
- orchidist fumaric goo fix
- Goo conversion to crystals
- Crystallization from oil after solvent washing
- Plant to crystal record 
- Hot water saponification with lime
- Phytol not present in Ethyl Acetate plant extract
- Mescaline citrate vs HCl
- Trimescaline citrate candidate
- Ethyl acetate approach
- Organic acid tests
- Succinic test
- Wet solvent succinic salting
- Orchidist's mescaline salt calculator