Revision as of 18:17, 21 December 2021

Introduction 🙏

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

The technique (TEK) to obtain mescaline crystals is simple. Cactus powder is mixed with lime and water into a paste. The cooled paste is pulled with ethyl acetate. Finally, the extract is salted with citric acid to precipitate mescaline citrate crystals which are collected, washed, and dried.

Thanks to everyone who contributed to this process: someblackguy, benzyme, shroombee, Metta-Morpheus, Downwardsfromzero, Kash, grollum, Mindlusion, Doubledog, Dreamer042, merkin, _Trip_, Cheelin, Highlightprotein, 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.

Materials🛒

Consumables👩‍🌾

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

†Outer green skin yields significantly more than the inner white core. Outer waxy layers and and spines do not yield product. Data reported by _Trip_^[3]

Equipment🏺

• Food dehydrator or oven to dry cactus chunks at low heat (~175F, if needed)
• Coffee grinder to finely powder dry cactus (if needed)
• French press for mixing the cactus paste and pulling with ethyl acetate (a quart jar or even a mixing bowl also works but these options are not as easy to use as the french press)
• Coffee filters, support basket, and funnel
• Quart jars to collect filtered pulls and precipitate mescaline citrate
• Fridge
• Kitchen scale to weigh materials
• Magnetic stirrer (optional)

Process Overview 👀

• Make alkaline cactus water paste
• Pull with ethyl acetate
• Precipitate mescaline citrate crystals with citric acid
• Collect and wash crystals
• Reclaim solvent

Detailed Process 📜

Paste 🌵

It is very important to start with a well made cactus powder. Harvested chopped cactus needs to be dried dried very well and ground very finely (for example with a coffee grinder). Clouds of fine dust fly into the air when handling a good powder, reminiscent of flour.

Verify your starting cactus powder is fully dry and very fine. If in doubt, dehydrate with low heat in the oven for a few hours, checking for evaporative weight loss, and/or grind with a coffee grinder. Once you are certain the cactus powder is fully dry and finely ground, proceed with the TEK. Do not proceed if you doubt the dryness or fine grind of your cactus powder.

Make milky water in the extraction vessel or a separate 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 ^[4].

It is very important to mix the paste well and obtain the proper texture. Some elbow grease is required, so mix with intent.

Boiling water option: This option breaks down chlorophyll making the solvent pulls have less of a green color and less plant material. Simply mix the cactus powder and lime first, then add 275ml of boiling water and mix very well. Rest for a few hours to room temperature. Mix in 25ml of boiling water right before extracting to loosen up the paste (it may gel while cooling).

Extract 👨🏾‍🔬

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 will be cumbersome.

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 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. Even with some solvent stuck in the paste, you will still recover the vast majority of mescaline during subsequent pulls.

All of the extraction pulls should be completed within 30 minutes. After 30 minutes the paste can begin to congeal, making solvent penetration and recovery more difficult. There is plenty of time to leisurely perform five to 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. If using the boiling water option, rest extract in the fridge overnight and decant/filter a white precipitate that may appear. 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 chlorophyll) in the extract. While a colder extract could theoretically lower the yield, experimentally the yield was ok in one case ^[5] but lower in another ^[6].

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. The boiling water option tends to minimize xtals sticking and grows larger crystals. Allow crystalization to complete undisturbed so xtals stop growing (~up to 72 hours). Swirl extract after crystallization for several minutes to ensure all of the citric acid granules have dissolved and to knock of xtals of the wall (stubborn xtals can sometimes be knocked off with a spoon). 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. As with the 5mg/g option, Allow crystalization to complete undisturbed (~24 hours, but could be longer).

Collect 💖

Swirl ethyl acetate to knock crystals loose. Crystals that cling to the wall can sometimes be dislodged with a knife or spoon. Send solvent trough a 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). Collect crystals stuck on the jar walls (if any) by dissolving them in warm water, evaporating in a shallow dish, and scraping up dry crystals. Sometimes, the wall crystals form a transparent layer difficult to see. 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^[7]. 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 MesHCl and consistent with the salt form (MesH)H₂Cit. Approximate oral dosage recommendations for MesHCl can be found elsewhere^[8].

Mass spectrometry (MS) results from solaris analytical^[9] indicate the product is very clean mescaline (Fig. 6).

Reclaim Solvent 💚

Reusing solvents is encouraged^[10] at the DMT nexus.

Used solvent from the boiling water paste is recommended for reuse. The room temperature paste loads the solvent with chlorophyll, making it darker and possibly more 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.

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 try to make the TEK more robust. However, it has been argued that no options are needed, and crystals reliably form with good technique without having to add any options to the main TEK ^[11].

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.^[12]

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^[13]). Making the paste with boiling water 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 🔬

Paste 🌵

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).

Use of lime and boiling water causes the saponification of chlorophyll with heat ^[14]:

Chlorophyll is soluble in Ethyl Acetate, but Chlorophyllin and Phytol are not^[15]. Saponification in hot water gives an extract with less plant matter, less green color, improved crystallization, and is assumed a priori to be easier to reuse.

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 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.

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.

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^[16].

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 ^[17]).

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^[18]. 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 is superior to decanting if the goal is white xtals.

The washed crystals in the filter can be dissolved in warm water along with any wall crystals. This will give then final product a uniform appearance with large needles forming during slow water evaporation.

References 🗝️

1. ↑ Ethyl acetate safety[1]
2. ↑ Citric Acid Safety[2]
3. ↑ Result for different cactus powdered parts[3]
4. ↑ 69ron's Limonene TEK[4]
5. ↑ Cold extraction results[5]
6. ↑ Cheelin's results[6]
7. ↑ Cactus analysis thread[7]
8. ↑ Mescaline Oral Dosage[8]
9. ↑ Solaris analytical service[9]
10. ↑ On reusing non polar solvent[10]
11. ↑ Cheeling's argument [11]
12. ↑ Basing time tests results[12]
13. ↑ Whole bridgessi precipitate on jar walls [13]
14. ↑ Hot water saponification with lime[14]
15. ↑ Phytol not present in Ethyl Acetate plant extract[15]
16. ↑ Mescaline Citrate conversion to HCl results[16]
17. ↑ Ethyl acetate approach[17]
18. ↑ Malic acid test[18]