Revision as of 13:31, 5 July 2021

Introduction 🙏

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 mescaline citrate. 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, 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.

Consumables 🛒

• 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
• Quart jar to collect pulls and precipitate mescaline citrate
• Coffee filters, support basket, and funnel
• Kitchen scale to weigh materials
• French press for pulls (optional, but highly recommended)
• Magnetic stirrer (optional)
• Microwave (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
• 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
• Recover dried xtals from coffee filter

Detailed Process 📜

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.

Extract 👨🏾‍🔬

If available, transfer paste to a French press. The French press will make it easy to decant the ethyl acetate. Cover paste with ethyl acetate (~150g), stir gently for 45-60 seconds, 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, waiting, and decanting until quart jar is full. This will be 5-6 total pulls.

Extraction should be complete in less than 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 the pulls by remaining focused on the task.

Inspect extract for droplets or particles. If present, 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.

Crystalize ✨

Slow crystalization option: 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.

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.

Collect 💖

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^[4]. By weight, mescaline citrate is equivalent to mescaline sulfate dihydrate and 90% as strong as mescaline hydrochloride. Approximate oral dosage recommendations can be found elsewhere^[5].

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

Reclaim Solvent 💚

Reusing solvents is encouraged^[7] 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. 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.

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.^[8]

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 butb didn't get any precipitation, what gives?

A: First make sure the TEK instructions where followed, in particular: well mixed paste, short pull times, no squeezing, clean extract free of debris, citric acid is in range, etc. 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^[9]). 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 accurately in proportion not starting cactus amount).

Appendix: Development Notes 🔬

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^[10]) 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 required to obtain a product.

Extract 👨🏾‍🔬

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.

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):

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 ^[11]).

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^[12]. 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 💖

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 🗝️

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