Difference between revisions of "CIELO"
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*1qt ethyl acetate (also sold as "MEK substitute")
*1qt ethyl acetate (also sold as "MEK substitute")
*5g of citric acid (15g is another option)
*5g of citric acid (15g is another option)
*Washing soda and pH paper (to wash solvent for reuse)
*Washing soda and pH paper (to wash solvent for reuse)
Latest revision as of 20:44, 27 September 2021
- 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 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.
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.
- 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 (sodium carbonate) and pH paper (to wash solvent for reuse)
- 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)
Process Overview 👀
- 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 📜
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 .
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.
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 .
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.
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. 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.
Mass spectrometry (MS) results from solaris analytical indicate the product is very clean mescaline (Fig. 6).
Reclaim Solvent 💚
Reusing solvents is encouraged 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 😉.
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: 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). 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 🔬
No yield improvements were seen with longer basing time, paste drying, or increasing the ionic strength with CaCl2.
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) breaks down esters (generally soluble in ethyl acetate which is itself an ester) into carboxylate ions and organic alcohols. An important example is,
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.
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.
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.
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.
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 ).
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. 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.
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.
- Ethyl acetate safety
- Citric Acid Safety
- 69ron's Limonene TEK
- Cold extraction results
- Cactus analysis thread
- Mescaline Oral Dosage
- Solaris analytical service
- On reusing non polar solvent
- Basing time tests results
- Whole bridgessi precipitate on jar walls 
- Microwave assisted saponification
- Mescaline Citrate conversion to HCl results
- Ethyl acetate approach
- Malic acid test