DMT-Nexus Wiki - User contributions [en]

CIELO

2021-07-25T19:01:03Z

Shroombee: /* Process Overview 👀 */

= Introduction 🙏=
'''CIELO''' stands for '''C'''rystals '''I'''n '''E'''thyl-acetate '''L'''eisurely '''O'''ver-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, Loveall, and others.

= Safety ⛑️=
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.

=Materials🛒=

==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
*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]]
<center>''Fig. 1: Over the counter materials.</center>

= 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 📜=

== 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 <ref>69ron's Limonene TEK[https://wiki.dmt-nexus.me/69ron%27s_D-Limonene_Mescaline_Extraction]</ref>.

'''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]]
<center>''Fig. 2: Cactus lime paste. Appearance can vary.</center>

== Extract 👨🏾‍🔬==
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 <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 ✨==
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.

[[File:IMG 20210311 144419793 (1) copy 800x600.jpg|center]]<center>''Fig. 4: Crystals in ethyl acetate. Appearance will vary.</center>

== 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<ref>Cactus analysis thread[https://www.dmt-nexus.me/forum/default.aspx?g=posts&t=71353]</ref>. Unfortunately, the precise ratio of mescaline and citrate in the precipitate is not known and is under investigation (see development notes below). Depending the mescaline and citrate ratio, the salt made my this process is 62% to 90% as strong by weight as mescaline HCl. 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]]
<center>''Fig. 5: Final mescaline citrate crystals. Appearance will vary.</center>

Mass spectrometry (MS) results from solaris analytical<ref>Solaris analytical service[https://www.solarisanalytical.com/]</ref> indicate the product is very clean mescaline (Fig. 6).

[[File: Cactus-extract copy 800x600_1.jpg|center]]''<center>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. </center>

== Reclaim Solvent 💚==
Reusing solvents is encouraged<ref>On reusing non polar solvent[https://www.dmt-nexus.me/forum/default.aspx?g=posts&t=31398]</ref> 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.<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.

= 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<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,

'''<span style="color: Orange"> <div style="text-align: center;">Chlorophyll + 2OH<sup>-</sup> ⇒ Chlorophyllin<sup>--</sup> + Phytol + Ethanol</div></span>'''

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 👨🏾‍🔬==
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, 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.

'''<span style="color: Orange"> <div style="text-align: center;">nMes<sub>(↑)</sub> + H<sub>3</sub>Cit<sub>(↑)</sub> ⇒ (MesH)<sub>n</sub>H<sub>3-n</sub>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.

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>).

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<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 💖==

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 🗝️=
<references/>

CIELO

2021-07-25T19:00:13Z

Shroombee: /* Extract 👨🏾‍🔬 */

= Introduction 🙏=
'''CIELO''' stands for '''C'''rystals '''I'''n '''E'''thyl-acetate '''L'''eisurely '''O'''ver-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, Loveall, and others.

= Safety ⛑️=
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.

=Materials🛒=

==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
*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]]
<center>''Fig. 1: Over the counter materials.</center>

= 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 and wash
*Recover dried xtals from coffee filter
*Also wash and recover any xtals on the jar walls

= 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 <ref>69ron's Limonene TEK[https://wiki.dmt-nexus.me/69ron%27s_D-Limonene_Mescaline_Extraction]</ref>.

'''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]]
<center>''Fig. 2: Cactus lime paste. Appearance can vary.</center>

== Extract 👨🏾‍🔬==
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 <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 ✨==
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.

[[File:IMG 20210311 144419793 (1) copy 800x600.jpg|center]]<center>''Fig. 4: Crystals in ethyl acetate. Appearance will vary.</center>

== 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<ref>Cactus analysis thread[https://www.dmt-nexus.me/forum/default.aspx?g=posts&t=71353]</ref>. Unfortunately, the precise ratio of mescaline and citrate in the precipitate is not known and is under investigation (see development notes below). Depending the mescaline and citrate ratio, the salt made my this process is 62% to 90% as strong by weight as mescaline HCl. 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]]
<center>''Fig. 5: Final mescaline citrate crystals. Appearance will vary.</center>

Mass spectrometry (MS) results from solaris analytical<ref>Solaris analytical service[https://www.solarisanalytical.com/]</ref> indicate the product is very clean mescaline (Fig. 6).

[[File: Cactus-extract copy 800x600_1.jpg|center]]''<center>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. </center>

== Reclaim Solvent 💚==
Reusing solvents is encouraged<ref>On reusing non polar solvent[https://www.dmt-nexus.me/forum/default.aspx?g=posts&t=31398]</ref> 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.<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.

= 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<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,

'''<span style="color: Orange"> <div style="text-align: center;">Chlorophyll + 2OH<sup>-</sup> ⇒ Chlorophyllin<sup>--</sup> + Phytol + Ethanol</div></span>'''

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 👨🏾‍🔬==
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, 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.

'''<span style="color: Orange"> <div style="text-align: center;">nMes<sub>(↑)</sub> + H<sub>3</sub>Cit<sub>(↑)</sub> ⇒ (MesH)<sub>n</sub>H<sub>3-n</sub>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.

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>).

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<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 💖==

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 🗝️=
<references/>

CIELO

2021-07-25T18:58:09Z

Shroombee: /* Extract 👨🏾‍🔬 */

= Introduction 🙏=
'''CIELO''' stands for '''C'''rystals '''I'''n '''E'''thyl-acetate '''L'''eisurely '''O'''ver-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, Loveall, and others.

= Safety ⛑️=
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.

=Materials🛒=

==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
*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]]
<center>''Fig. 1: Over the counter materials.</center>

= 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 and wash
*Recover dried xtals from coffee filter
*Also wash and recover any xtals on the jar walls

= 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 <ref>69ron's Limonene TEK[https://wiki.dmt-nexus.me/69ron%27s_D-Limonene_Mescaline_Extraction]</ref>.

'''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]]
<center>''Fig. 2: Cactus lime paste. Appearance can vary.</center>

== Extract 👨🏾‍🔬==
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.

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 ✨==
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.

[[File:IMG 20210311 144419793 (1) copy 800x600.jpg|center]]<center>''Fig. 4: Crystals in ethyl acetate. Appearance will vary.</center>

== 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<ref>Cactus analysis thread[https://www.dmt-nexus.me/forum/default.aspx?g=posts&t=71353]</ref>. Unfortunately, the precise ratio of mescaline and citrate in the precipitate is not known and is under investigation (see development notes below). Depending the mescaline and citrate ratio, the salt made my this process is 62% to 90% as strong by weight as mescaline HCl. 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]]
<center>''Fig. 5: Final mescaline citrate crystals. Appearance will vary.</center>

Mass spectrometry (MS) results from solaris analytical<ref>Solaris analytical service[https://www.solarisanalytical.com/]</ref> indicate the product is very clean mescaline (Fig. 6).

[[File: Cactus-extract copy 800x600_1.jpg|center]]''<center>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. </center>

== Reclaim Solvent 💚==
Reusing solvents is encouraged<ref>On reusing non polar solvent[https://www.dmt-nexus.me/forum/default.aspx?g=posts&t=31398]</ref> 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.<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.

= 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<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,

'''<span style="color: Orange"> <div style="text-align: center;">Chlorophyll + 2OH<sup>-</sup> ⇒ Chlorophyllin<sup>--</sup> + Phytol + Ethanol</div></span>'''

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 👨🏾‍🔬==
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, 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.

'''<span style="color: Orange"> <div style="text-align: center;">nMes<sub>(↑)</sub> + H<sub>3</sub>Cit<sub>(↑)</sub> ⇒ (MesH)<sub>n</sub>H<sub>3-n</sub>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.

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>).

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<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 💖==

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 🗝️=
<references/>

CIELO

2021-07-25T18:54:17Z

Shroombee: /* Extract 👨🏾‍🔬 */

= Introduction 🙏=
'''CIELO''' stands for '''C'''rystals '''I'''n '''E'''thyl-acetate '''L'''eisurely '''O'''ver-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, Loveall, and others.

= Safety ⛑️=
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.

=Materials🛒=

==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
*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]]
<center>''Fig. 1: Over the counter materials.</center>

= 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 and wash
*Recover dried xtals from coffee filter
*Also wash and recover any xtals on the jar walls

= 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 <ref>69ron's Limonene TEK[https://wiki.dmt-nexus.me/69ron%27s_D-Limonene_Mescaline_Extraction]</ref>.

'''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]]
<center>''Fig. 2: Cactus lime paste. Appearance can vary.</center>

== Extract 👨🏾‍🔬==
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.

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.

Rest extract for at least an hour and 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 ✨==
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.

[[File:IMG 20210311 144419793 (1) copy 800x600.jpg|center]]<center>''Fig. 4: Crystals in ethyl acetate. Appearance will vary.</center>

== 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<ref>Cactus analysis thread[https://www.dmt-nexus.me/forum/default.aspx?g=posts&t=71353]</ref>. Unfortunately, the precise ratio of mescaline and citrate in the precipitate is not known and is under investigation (see development notes below). Depending the mescaline and citrate ratio, the salt made my this process is 62% to 90% as strong by weight as mescaline HCl. 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]]
<center>''Fig. 5: Final mescaline citrate crystals. Appearance will vary.</center>

Mass spectrometry (MS) results from solaris analytical<ref>Solaris analytical service[https://www.solarisanalytical.com/]</ref> indicate the product is very clean mescaline (Fig. 6).

[[File: Cactus-extract copy 800x600_1.jpg|center]]''<center>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. </center>

== Reclaim Solvent 💚==
Reusing solvents is encouraged<ref>On reusing non polar solvent[https://www.dmt-nexus.me/forum/default.aspx?g=posts&t=31398]</ref> 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.<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.

= 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<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,

'''<span style="color: Orange"> <div style="text-align: center;">Chlorophyll + 2OH<sup>-</sup> ⇒ Chlorophyllin<sup>--</sup> + Phytol + Ethanol</div></span>'''

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 👨🏾‍🔬==
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, 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.

'''<span style="color: Orange"> <div style="text-align: center;">nMes<sub>(↑)</sub> + H<sub>3</sub>Cit<sub>(↑)</sub> ⇒ (MesH)<sub>n</sub>H<sub>3-n</sub>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.

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>).

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<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 💖==

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 🗝️=
<references/>

CIELO

2021-07-05T22:45:02Z

Shroombee: /* Extract 👨🏾‍🔬 */

= Introduction 🙏=
'''CIELO''' stands for '''C'''rystals '''I'''n '''E'''thyl-acetate '''L'''eisurely '''O'''ver-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<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.

=Materials🛒=

==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
*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)

[[File:IMG 20210608 223040865 copy 800x600.jpg|center]]
<center>''Fig. 1: Over the counter materials.</center>

= 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 <ref>69ron's Limonene TEK[https://wiki.dmt-nexus.me/69ron%27s_D-Limonene_Mescaline_Extraction]</ref>.

'''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]]
<center>''Fig. 2: Cactus lime paste. Appearance can vary.</center>

== Extract 👨🏾‍🔬==
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.

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.

'''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 ✨==
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 "drop 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.

[[File:IMG 20210311 144419793 (1) copy 800x600.jpg|center]]<center>''Fig. 4: Crystals in ethyl acetate. Appearance will vary.</center>

== 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<ref>Cactus analysis thread[https://www.dmt-nexus.me/forum/default.aspx?g=posts&t=71353]</ref>. 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<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]]
<center>''Fig. 5: Final mescaline citrate crystals. Appearance will vary.</center>

Mass spectrometry (MS) results from solaris analytical<ref>Solaris analytical service[https://www.solarisanalytical.com/]</ref> indicate the product is very clean mescaline (Fig. 6).

[[File: Cactus-extract copy 800x600_1.jpg|center]]''<center>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. </center>

== Reclaim Solvent 💚==
Reusing solvents is encouraged<ref>On reusing non polar solvent[https://www.dmt-nexus.me/forum/default.aspx?g=posts&t=31398]</ref> 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.

= 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 magnetic stirrer running. 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.<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 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. 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).

= 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<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,

'''<span style="color: Orange"> <div style="text-align: center;">Chlorophyll + 2OH<sup>-</sup> ⇒ Chlorophyllin<sup>--</sup> + Phytol + Ethanol</div></span>'''

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 👨🏾‍🔬==
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):

'''<span style="color: Orange"> <div style="text-align: center;">3Mes<sub>(↑)</sub> + H3Cit<sub>(↑)</sub> ⇒ 3(MesH)Cit<sub>(↓)</sub></div></span>'''

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>).

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<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 💖==

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 🗝️=
<references/>

CIELO

2021-07-05T22:32:30Z

Shroombee: /* Extract 👨🏾‍🔬 */

= Introduction 🙏=
'''CIELO''' stands for '''C'''rystals '''I'''n '''E'''thyl-acetate '''L'''eisurely '''O'''ver-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<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.

=Materials🛒=

==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
*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)

[[File:IMG 20210608 223040865 copy 800x600.jpg|center]]
<center>''Fig. 1: Over the counter materials.</center>

= 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 <ref>69ron's Limonene TEK[https://wiki.dmt-nexus.me/69ron%27s_D-Limonene_Mescaline_Extraction]</ref>.

'''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]]
<center>''Fig. 2: Cactus lime paste. Appearance can vary.</center>

== Extract 👨🏾‍🔬==
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, 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.

'''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 ✨==
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 "drop 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.

[[File:IMG 20210311 144419793 (1) copy 800x600.jpg|center]]<center>''Fig. 4: Crystals in ethyl acetate. Appearance will vary.</center>

== 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<ref>Cactus analysis thread[https://www.dmt-nexus.me/forum/default.aspx?g=posts&t=71353]</ref>. 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<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]]
<center>''Fig. 5: Final mescaline citrate crystals. Appearance will vary.</center>

Mass spectrometry (MS) results from solaris analytical<ref>Solaris analytical service[https://www.solarisanalytical.com/]</ref> indicate the product is very clean mescaline (Fig. 6).

[[File: Cactus-extract copy 800x600_1.jpg|center]]''<center>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. </center>

== Reclaim Solvent 💚==
Reusing solvents is encouraged<ref>On reusing non polar solvent[https://www.dmt-nexus.me/forum/default.aspx?g=posts&t=31398]</ref> 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.

= 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 magnetic stirrer running. 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.<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 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. 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).

= 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<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,

'''<span style="color: Orange"> <div style="text-align: center;">Chlorophyll + 2OH<sup>-</sup> ⇒ Chlorophyllin<sup>--</sup> + Phytol + Ethanol</div></span>'''

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 👨🏾‍🔬==
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):

'''<span style="color: Orange"> <div style="text-align: center;">3Mes<sub>(↑)</sub> + H3Cit<sub>(↑)</sub> ⇒ 3(MesH)Cit<sub>(↓)</sub></div></span>'''

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>).

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<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 💖==

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 🗝️=
<references/>

CIELO

2021-07-05T22:29:21Z

Shroombee: /* Extract 👨🏾‍🔬 */

= Introduction 🙏=
'''CIELO''' stands for '''C'''rystals '''I'''n '''E'''thyl-acetate '''L'''eisurely '''O'''ver-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<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.

=Materials🛒=

==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
*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)

[[File:IMG 20210608 223040865 copy 800x600.jpg|center]]
<center>''Fig. 1: Over the counter materials.</center>

= 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 <ref>69ron's Limonene TEK[https://wiki.dmt-nexus.me/69ron%27s_D-Limonene_Mescaline_Extraction]</ref>.

'''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]]
<center>''Fig. 2: Cactus lime paste. Appearance can vary.</center>

== Extract 👨🏾‍🔬==
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, 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.

'''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. This minimizes plant material in the extract to hell with crystalization. While colder extract could lower 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 ✨==
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 "drop 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.

[[File:IMG 20210311 144419793 (1) copy 800x600.jpg|center]]<center>''Fig. 4: Crystals in ethyl acetate. Appearance will vary.</center>

== 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<ref>Cactus analysis thread[https://www.dmt-nexus.me/forum/default.aspx?g=posts&t=71353]</ref>. 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<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]]
<center>''Fig. 5: Final mescaline citrate crystals. Appearance will vary.</center>

Mass spectrometry (MS) results from solaris analytical<ref>Solaris analytical service[https://www.solarisanalytical.com/]</ref> indicate the product is very clean mescaline (Fig. 6).

[[File: Cactus-extract copy 800x600_1.jpg|center]]''<center>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. </center>

== Reclaim Solvent 💚==
Reusing solvents is encouraged<ref>On reusing non polar solvent[https://www.dmt-nexus.me/forum/default.aspx?g=posts&t=31398]</ref> 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.

= 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 magnetic stirrer running. 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.<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 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. 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).

= 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<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,

'''<span style="color: Orange"> <div style="text-align: center;">Chlorophyll + 2OH<sup>-</sup> ⇒ Chlorophyllin<sup>--</sup> + Phytol + Ethanol</div></span>'''

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 👨🏾‍🔬==
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):

'''<span style="color: Orange"> <div style="text-align: center;">3Mes<sub>(↑)</sub> + H3Cit<sub>(↑)</sub> ⇒ 3(MesH)Cit<sub>(↓)</sub></div></span>'''

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>).

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<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 💖==

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 🗝️=
<references/>

CIELO

2021-07-05T22:25:25Z

Shroombee: /* Equipment🏺 */

= Introduction 🙏=
'''CIELO''' stands for '''C'''rystals '''I'''n '''E'''thyl-acetate '''L'''eisurely '''O'''ver-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<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.

=Materials🛒=

==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
*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)

[[File:IMG 20210608 223040865 copy 800x600.jpg|center]]
<center>''Fig. 1: Over the counter materials.</center>

= 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 <ref>69ron's Limonene TEK[https://wiki.dmt-nexus.me/69ron%27s_D-Limonene_Mescaline_Extraction]</ref>.

'''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]]
<center>''Fig. 2: Cactus lime paste. Appearance can vary.</center>

== 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.

'''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. This minimizes plant material in the extract to hell with crystalization. While colder extract could lower 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 ✨==
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 "drop 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.

[[File:IMG 20210311 144419793 (1) copy 800x600.jpg|center]]<center>''Fig. 4: Crystals in ethyl acetate. Appearance will vary.</center>

== 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<ref>Cactus analysis thread[https://www.dmt-nexus.me/forum/default.aspx?g=posts&t=71353]</ref>. 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<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]]
<center>''Fig. 5: Final mescaline citrate crystals. Appearance will vary.</center>

Mass spectrometry (MS) results from solaris analytical<ref>Solaris analytical service[https://www.solarisanalytical.com/]</ref> indicate the product is very clean mescaline (Fig. 6).

[[File: Cactus-extract copy 800x600_1.jpg|center]]''<center>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. </center>

== Reclaim Solvent 💚==
Reusing solvents is encouraged<ref>On reusing non polar solvent[https://www.dmt-nexus.me/forum/default.aspx?g=posts&t=31398]</ref> 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.

= 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 magnetic stirrer running. 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.<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 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. 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).

= 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<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,

'''<span style="color: Orange"> <div style="text-align: center;">Chlorophyll + 2OH<sup>-</sup> ⇒ Chlorophyllin<sup>--</sup> + Phytol + Ethanol</div></span>'''

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 👨🏾‍🔬==
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):

'''<span style="color: Orange"> <div style="text-align: center;">3Mes<sub>(↑)</sub> + H3Cit<sub>(↑)</sub> ⇒ 3(MesH)Cit<sub>(↓)</sub></div></span>'''

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>).

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<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 💖==

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 🗝️=
<references/>

CIELO

2021-07-05T22:23:57Z

Shroombee: /* Equipment🏺 */

= Introduction 🙏=
'''CIELO''' stands for '''C'''rystals '''I'''n '''E'''thyl-acetate '''L'''eisurely '''O'''ver-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<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.

=Materials🛒=

==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 for pulling cactus with ethyl acetate (or optionally use a French press which is highly recommended)
*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)

[[File:IMG 20210608 223040865 copy 800x600.jpg|center]]
<center>''Fig. 1: Over the counter materials.</center>

= 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 <ref>69ron's Limonene TEK[https://wiki.dmt-nexus.me/69ron%27s_D-Limonene_Mescaline_Extraction]</ref>.

'''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]]
<center>''Fig. 2: Cactus lime paste. Appearance can vary.</center>

== 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.

'''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. This minimizes plant material in the extract to hell with crystalization. While colder extract could lower 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 ✨==
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 "drop 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.

[[File:IMG 20210311 144419793 (1) copy 800x600.jpg|center]]<center>''Fig. 4: Crystals in ethyl acetate. Appearance will vary.</center>

== 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<ref>Cactus analysis thread[https://www.dmt-nexus.me/forum/default.aspx?g=posts&t=71353]</ref>. 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<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]]
<center>''Fig. 5: Final mescaline citrate crystals. Appearance will vary.</center>

Mass spectrometry (MS) results from solaris analytical<ref>Solaris analytical service[https://www.solarisanalytical.com/]</ref> indicate the product is very clean mescaline (Fig. 6).

[[File: Cactus-extract copy 800x600_1.jpg|center]]''<center>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. </center>

== Reclaim Solvent 💚==
Reusing solvents is encouraged<ref>On reusing non polar solvent[https://www.dmt-nexus.me/forum/default.aspx?g=posts&t=31398]</ref> 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.

= 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 magnetic stirrer running. 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.<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 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. 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).

= 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<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,

'''<span style="color: Orange"> <div style="text-align: center;">Chlorophyll + 2OH<sup>-</sup> ⇒ Chlorophyllin<sup>--</sup> + Phytol + Ethanol</div></span>'''

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 👨🏾‍🔬==
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):

'''<span style="color: Orange"> <div style="text-align: center;">3Mes<sub>(↑)</sub> + H3Cit<sub>(↑)</sub> ⇒ 3(MesH)Cit<sub>(↓)</sub></div></span>'''

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>).

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<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 💖==

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 🗝️=
<references/>

CIELO

2021-07-05T22:23:09Z

Shroombee: /* Equipment🏺 */

= Introduction 🙏=
'''CIELO''' stands for '''C'''rystals '''I'''n '''E'''thyl-acetate '''L'''eisurely '''O'''ver-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<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.

=Materials🛒=

==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 for pulling cactus with ethyl acetate (or use a French press - see below)
*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)

[[File:IMG 20210608 223040865 copy 800x600.jpg|center]]
<center>''Fig. 1: Over the counter materials.</center>

= 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 <ref>69ron's Limonene TEK[https://wiki.dmt-nexus.me/69ron%27s_D-Limonene_Mescaline_Extraction]</ref>.

'''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]]
<center>''Fig. 2: Cactus lime paste. Appearance can vary.</center>

== 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.

'''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. This minimizes plant material in the extract to hell with crystalization. While colder extract could lower 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 ✨==
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 "drop 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.

[[File:IMG 20210311 144419793 (1) copy 800x600.jpg|center]]<center>''Fig. 4: Crystals in ethyl acetate. Appearance will vary.</center>

== 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<ref>Cactus analysis thread[https://www.dmt-nexus.me/forum/default.aspx?g=posts&t=71353]</ref>. 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<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]]
<center>''Fig. 5: Final mescaline citrate crystals. Appearance will vary.</center>

Mass spectrometry (MS) results from solaris analytical<ref>Solaris analytical service[https://www.solarisanalytical.com/]</ref> indicate the product is very clean mescaline (Fig. 6).

[[File: Cactus-extract copy 800x600_1.jpg|center]]''<center>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. </center>

== Reclaim Solvent 💚==
Reusing solvents is encouraged<ref>On reusing non polar solvent[https://www.dmt-nexus.me/forum/default.aspx?g=posts&t=31398]</ref> 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.

= 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 magnetic stirrer running. 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.<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 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. 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).

= 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<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,

'''<span style="color: Orange"> <div style="text-align: center;">Chlorophyll + 2OH<sup>-</sup> ⇒ Chlorophyllin<sup>--</sup> + Phytol + Ethanol</div></span>'''

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 👨🏾‍🔬==
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):

'''<span style="color: Orange"> <div style="text-align: center;">3Mes<sub>(↑)</sub> + H3Cit<sub>(↑)</sub> ⇒ 3(MesH)Cit<sub>(↓)</sub></div></span>'''

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>).

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<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 💖==

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 🗝️=
<references/>

CIELO

2021-07-04T04:19:19Z

Shroombee:

= Introduction 🙏=
'''CIELO''' stands for '''C'''rystals '''I'''n '''E'''thyl-acetate '''L'''eisurely '''O'''ver-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<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.

= Materials 🛒=
*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)

[[File:IMG 20210608 223040865 copy 800x600.jpg|center]]
<center>''Fig. 1: Over the counter materials.</center>

= 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 <ref>69ron's Limonene TEK[https://wiki.dmt-nexus.me/69ron%27s_D-Limonene_Mescaline_Extraction]</ref>.

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]]
<center>''Fig. 2: Cactus lime paste. Appearance can vary.</center>

== 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 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.

[[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 ✨==
'''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.

''Note:'' Citric acid is relatively soluble in ethyl acetate (50mg/g). A common question when mescaline citrate precipitates is how does one know that citric acid is not what is precipitating? The answer is simply that citric acid does not precipitate and stays in solution because it is bellow its saturation point. The white particles that form from the clouds are mescaline citrate and not citric acid.

[[File:IMG 20210311 144419793 (1) copy 800x600.jpg|center]]<center>''Fig. 4: Crystals in ethyl acetate. Appearance will vary.</center>

== 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<ref>Cactus analysis thread[https://www.dmt-nexus.me/forum/default.aspx?g=posts&t=71353]</ref>. 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<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]]
<center>''Fig. 5: Final mescaline citrate crystals. Appearance will vary.</center>

Mass spectrometry (MS) results from solaris analytical<ref>Solaris analytical service[https://www.solarisanalytical.com/]</ref> indicate the product is very clean mescaline (Fig. 6).

[[File: Cactus-extract copy 800x600_1.jpg|center]]''<center>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. </center>

== Reclaim Solvent 💚==
Reusing solvents is encouraged<ref>On reusing non polar solvent[https://www.dmt-nexus.me/forum/default.aspx?g=posts&t=31398]</ref> 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.<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.

= 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<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,

'''<span style="color: Orange"> <div style="text-align: center;">Chlorophyll + 2OH<sup>-</sup> ⇒ Chlorophyllin<sup>--</sup> + Phytol + Ethanol</div></span>'''

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):

'''<span style="color: Orange"> <div style="text-align: center;">3Mes<sub>(↑)</sub> + H3Cit<sub>(↑)</sub> ⇒ 3(MesH)Cit<sub>(↓)</sub></div></span>'''

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>).

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<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 💖==

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 🗝️=
<references/>

CIELO

2021-07-04T04:18:59Z

Shroombee: /* Safety ⛑️ */

= Introduction 🙏=
'''CIELO''' stands for '''C'''rystals '''I'''n '''E'''thyl-acetate '''L'''eisurely '''O'''ver-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<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.

= Materials 🛒=
*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)

[[File:IMG 20210608 223040865 copy 800x600.jpg|center]]
<center>''Fig. 1: Over the counter materials.</center>

= 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 <ref>69ron's Limonene TEK[https://wiki.dmt-nexus.me/69ron%27s_D-Limonene_Mescaline_Extraction]</ref>.

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]]
<center>''Fig. 2: Cactus lime paste. Appearance can vary.</center>

== 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 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.

[[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 ✨==
'''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.

''Note:'' Citric acid is relatively soluble in ethyl acetate (50mg/g). A common question when mescaline citrate precipitates is how does one know that citric acid is not what is precipitating? The answer is simply that citric acid does not precipitate and stays in solution because it is bellow its saturation point. The white particles that form from the clouds are mescaline citrate and not citric acid.

[[File:IMG 20210311 144419793 (1) copy 800x600.jpg|center]]<center>''Fig. 4: Crystals in ethyl acetate. Appearance will vary.</center>

== 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<ref>Cactus analysis thread[https://www.dmt-nexus.me/forum/default.aspx?g=posts&t=71353]</ref>. 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<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]]
<center>''Fig. 5: Final mescaline citrate crystals. Appearance will vary.</center>

Mass spectrometry (MS) results from solaris analytical<ref>Solaris analytical service[https://www.solarisanalytical.com/]</ref> indicate the product is very clean mescaline (Fig. 6).

[[File: Cactus-extract copy 800x600_1.jpg|center]]''<center>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. </center>

== Reclaim Solvent 💚==
Reusing solvents is encouraged<ref>On reusing non polar solvent[https://www.dmt-nexus.me/forum/default.aspx?g=posts&t=31398]</ref> 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.<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.

= 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<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,

'''<span style="color: Orange"> <div style="text-align: center;">Chlorophyll + 2OH<sup>-</sup> ⇒ Chlorophyllin<sup>--</sup> + Phytol + Ethanol</div></span>'''

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):

'''<span style="color: Orange"> <div style="text-align: center;">3Mes<sub>(↑)</sub> + H3Cit<sub>(↑)</sub> ⇒ 3(MesH)Cit<sub>(↓)</sub></div></span>'''

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>).

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<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 💖==

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 🗝️=
<references/>

CIELO

2021-07-04T04:18:14Z

Shroombee:

= Introduction 🙏=
'''CIELO''' stands for '''C'''rystals '''I'''n '''E'''thyl-acetate '''L'''eisurely '''O'''ver-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<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 procedure 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 🛒=
*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)

[[File:IMG 20210608 223040865 copy 800x600.jpg|center]]
<center>''Fig. 1: Over the counter materials.</center>

= 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 <ref>69ron's Limonene TEK[https://wiki.dmt-nexus.me/69ron%27s_D-Limonene_Mescaline_Extraction]</ref>.

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]]
<center>''Fig. 2: Cactus lime paste. Appearance can vary.</center>

== 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 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.

[[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 ✨==
'''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.

''Note:'' Citric acid is relatively soluble in ethyl acetate (50mg/g). A common question when mescaline citrate precipitates is how does one know that citric acid is not what is precipitating? The answer is simply that citric acid does not precipitate and stays in solution because it is bellow its saturation point. The white particles that form from the clouds are mescaline citrate and not citric acid.

[[File:IMG 20210311 144419793 (1) copy 800x600.jpg|center]]<center>''Fig. 4: Crystals in ethyl acetate. Appearance will vary.</center>

== 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<ref>Cactus analysis thread[https://www.dmt-nexus.me/forum/default.aspx?g=posts&t=71353]</ref>. 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<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]]
<center>''Fig. 5: Final mescaline citrate crystals. Appearance will vary.</center>

Mass spectrometry (MS) results from solaris analytical<ref>Solaris analytical service[https://www.solarisanalytical.com/]</ref> indicate the product is very clean mescaline (Fig. 6).

[[File: Cactus-extract copy 800x600_1.jpg|center]]''<center>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. </center>

== Reclaim Solvent 💚==
Reusing solvents is encouraged<ref>On reusing non polar solvent[https://www.dmt-nexus.me/forum/default.aspx?g=posts&t=31398]</ref> 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.<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.

= 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<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,

'''<span style="color: Orange"> <div style="text-align: center;">Chlorophyll + 2OH<sup>-</sup> ⇒ Chlorophyllin<sup>--</sup> + Phytol + Ethanol</div></span>'''

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):

'''<span style="color: Orange"> <div style="text-align: center;">3Mes<sub>(↑)</sub> + H3Cit<sub>(↑)</sub> ⇒ 3(MesH)Cit<sub>(↓)</sub></div></span>'''

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>).

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<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 💖==

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 🗝️=
<references/>

CIELO

2021-07-04T04:17:57Z

Shroombee:

= Introduction 🙏=
'''CIELO''' stands for '''C'''rystals '''I'''n '''E'''thyl-acetate '''L'''eisurely '''O'''ver-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<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 procedure 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 🛒=
*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)

[[File:IMG 20210608 223040865 copy 800x600.jpg|center]]
<center>''Fig. 1: Over the counter materials.</center>

= 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 <ref>69ron's Limonene TEK[https://wiki.dmt-nexus.me/69ron%27s_D-Limonene_Mescaline_Extraction]</ref>.

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]]
<center>''Fig. 2: Cactus lime paste. Appearance can vary.</center>

== 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 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.

[[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 ✨==
'''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.

''Note:'' Citric acid is relatively soluble in ethyl acetate (50mg/g). A common question when mescaline citrate precipitates is how does one know that citric acid is not what is precipitating? The answer is simply that citric acid does not precipitate and stays in solution because it is bellow its saturation point. The white particles that form from the clouds are mescaline citrate and not citric acid.

[[File:IMG 20210311 144419793 (1) copy 800x600.jpg|center]]<center>''Fig. 4: Crystals in ethyl acetate. Appearance will vary.</center>

== 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<ref>Cactus analysis thread[https://www.dmt-nexus.me/forum/default.aspx?g=posts&t=71353]</ref>. 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<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]]
<center>''Fig. 5: Final mescaline citrate crystals. Appearance will vary.</center>

Mass spectrometry (MS) results from solaris analytical<ref>Solaris analytical service[https://www.solarisanalytical.com/]</ref> indicate the product is very clean mescaline (Fig. 6).

[[File: Cactus-extract copy 800x600_1.jpg|center]]''<center>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. </center>

== Reclaim Solvent 💚==
Reusing solvents is encouraged<ref>On reusing non polar solvent[https://www.dmt-nexus.me/forum/default.aspx?g=posts&t=31398]</ref> 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.<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.

= 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<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,

'''<span style="color: Orange"> <div style="text-align: center;">Chlorophyll + 2OH<sup>-</sup> ⇒ Chlorophyllin<sup>--</sup> + Phytol + Ethanol</div></span>'''

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):

'''<span style="color: Orange"> <div style="text-align: center;">3Mes<sub>(↑)</sub> + H3Cit<sub>(↑)</sub> ⇒ 3(MesH)Cit<sub>(↓)</sub></div></span>'''

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>).

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<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 💖==

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 🗝️=
<references/>

CIELO

2021-07-04T04:17:01Z

Shroombee: /* Safety ⛑️ */

= Introduction 🙏=
'''CIELO''' stands for '''C'''rystals '''I'''n '''E'''thyl-acetate '''L'''eisurely '''O'''ver-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<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 procedure 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 🛒=
*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)

[[File:IMG 20210608 223040865 copy 800x600.jpg|center]]
<center>''Fig. 1: Over the counter materials.</center>

= 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 <ref>69ron's Limonene TEK[https://wiki.dmt-nexus.me/69ron%27s_D-Limonene_Mescaline_Extraction]</ref>.

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]]
<center>''Fig. 2: Cactus lime paste. Appearance can vary.</center>

== 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 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.

[[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 ✨==
'''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.

''Note:'' Citric acid is relatively soluble in ethyl acetate (50mg/g). A common question when mescaline citrate precipitates is how does one know that citric acid is not what is precipitating? The answer is simply that citric acid does not precipitate and stays in solution because it is bellow its saturation point. The white particles that form from the clouds are mescaline citrate and not citric acid.

[[File:IMG 20210311 144419793 (1) copy 800x600.jpg|center]]<center>''Fig. 4: Crystals in ethyl acetate. Appearance will vary.</center>

== 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<ref>Cactus analysis thread[https://www.dmt-nexus.me/forum/default.aspx?g=posts&t=71353]</ref>. 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<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]]
<center>''Fig. 5: Final mescaline citrate crystals. Appearance will vary.</center>

Mass spectrometry (MS) results from solaris analytical<ref>Solaris analytical service[https://www.solarisanalytical.com/]</ref> indicate the product is very clean mescaline (Fig. 6).

[[File: Cactus-extract copy 800x600_1.jpg|center]]''<center>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. </center>

== Reclaim Solvent 💚==
Reusing solvents is encouraged<ref>On reusing non polar solvent[https://www.dmt-nexus.me/forum/default.aspx?g=posts&t=31398]</ref> 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.<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.

= 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<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,

'''<span style="color: Orange"> <div style="text-align: center;">Chlorophyll + 2OH<sup>-</sup> ⇒ Chlorophyllin<sup>--</sup> + Phytol + Ethanol</div></span>'''

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):

'''<span style="color: Orange"> <div style="text-align: center;">3Mes<sub>(↑)</sub> + H3Cit<sub>(↑)</sub> ⇒ 3(MesH)Cit<sub>(↓)</sub></div></span>'''

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>).

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<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 💖==

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 🗝️=
<references/>

CIELO

2021-07-04T04:14:07Z

Shroombee: /* Frequently Asked Questions */

= Introduction 🙏=
'''CIELO''' stands for '''C'''rystals '''I'''n '''E'''thyl-acetate '''L'''eisurely '''O'''ver-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<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.

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

= Materials 🛒=
*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)

[[File:IMG 20210608 223040865 copy 800x600.jpg|center]]
<center>''Fig. 1: Over the counter materials.</center>

= 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 <ref>69ron's Limonene TEK[https://wiki.dmt-nexus.me/69ron%27s_D-Limonene_Mescaline_Extraction]</ref>.

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]]
<center>''Fig. 2: Cactus lime paste. Appearance can vary.</center>

== 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 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.

[[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 ✨==
'''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.

''Note:'' Citric acid is relatively soluble in ethyl acetate (50mg/g). A common question when mescaline citrate precipitates is how does one know that citric acid is not what is precipitating? The answer is simply that citric acid does not precipitate and stays in solution because it is bellow its saturation point. The white particles that form from the clouds are mescaline citrate and not citric acid.

[[File:IMG 20210311 144419793 (1) copy 800x600.jpg|center]]<center>''Fig. 4: Crystals in ethyl acetate. Appearance will vary.</center>

== 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<ref>Cactus analysis thread[https://www.dmt-nexus.me/forum/default.aspx?g=posts&t=71353]</ref>. 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<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]]
<center>''Fig. 5: Final mescaline citrate crystals. Appearance will vary.</center>

Mass spectrometry (MS) results from solaris analytical<ref>Solaris analytical service[https://www.solarisanalytical.com/]</ref> indicate the product is very clean mescaline (Fig. 6).

[[File: Cactus-extract copy 800x600_1.jpg|center]]''<center>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. </center>

== Reclaim Solvent 💚==
Reusing solvents is encouraged<ref>On reusing non polar solvent[https://www.dmt-nexus.me/forum/default.aspx?g=posts&t=31398]</ref> 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.<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.

= 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<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,

'''<span style="color: Orange"> <div style="text-align: center;">Chlorophyll + 2OH<sup>-</sup> ⇒ Chlorophyllin<sup>--</sup> + Phytol + Ethanol</div></span>'''

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):

'''<span style="color: Orange"> <div style="text-align: center;">3Mes<sub>(↑)</sub> + H3Cit<sub>(↑)</sub> ⇒ 3(MesH)Cit<sub>(↓)</sub></div></span>'''

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>).

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<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 💖==

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 🗝️=
<references/>

CIELO

2021-07-04T04:12:24Z

Shroombee: /* Frequently Asked Questions */

= Introduction 🙏=
'''CIELO''' stands for '''C'''rystals '''I'''n '''E'''thyl-acetate '''L'''eisurely '''O'''ver-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<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.

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

= Materials 🛒=
*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)

[[File:IMG 20210608 223040865 copy 800x600.jpg|center]]
<center>''Fig. 1: Over the counter materials.</center>

= 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 <ref>69ron's Limonene TEK[https://wiki.dmt-nexus.me/69ron%27s_D-Limonene_Mescaline_Extraction]</ref>.

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]]
<center>''Fig. 2: Cactus lime paste. Appearance can vary.</center>

== 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 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.

[[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 ✨==
'''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.

''Note:'' Citric acid is relatively soluble in ethyl acetate (50mg/g). A common question when mescaline citrate precipitates is how does one know that citric acid is not what is precipitating? The answer is simply that citric acid does not precipitate and stays in solution because it is bellow its saturation point. The white particles that form from the clouds are mescaline citrate and not citric acid.

[[File:IMG 20210311 144419793 (1) copy 800x600.jpg|center]]<center>''Fig. 4: Crystals in ethyl acetate. Appearance will vary.</center>

== 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<ref>Cactus analysis thread[https://www.dmt-nexus.me/forum/default.aspx?g=posts&t=71353]</ref>. 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<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]]
<center>''Fig. 5: Final mescaline citrate crystals. Appearance will vary.</center>

Mass spectrometry (MS) results from solaris analytical<ref>Solaris analytical service[https://www.solarisanalytical.com/]</ref> indicate the product is very clean mescaline (Fig. 6).

[[File: Cactus-extract copy 800x600_1.jpg|center]]''<center>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. </center>

== Reclaim Solvent 💚==
Reusing solvents is encouraged<ref>On reusing non polar solvent[https://www.dmt-nexus.me/forum/default.aspx?g=posts&t=31398]</ref> 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 8-10 minutes incorporating milky water with cactus, 6x3 minute pulls, and 15 mg/gram citric acid). 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.

= 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<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,

'''<span style="color: Orange"> <div style="text-align: center;">Chlorophyll + 2OH<sup>-</sup> ⇒ Chlorophyllin<sup>--</sup> + Phytol + Ethanol</div></span>'''

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):

'''<span style="color: Orange"> <div style="text-align: center;">3Mes<sub>(↑)</sub> + H3Cit<sub>(↑)</sub> ⇒ 3(MesH)Cit<sub>(↓)</sub></div></span>'''

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>).

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<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 💖==

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 🗝️=
<references/>

CIELO

2021-07-04T04:11:49Z

Shroombee: /* Frequently Asked Questions */

= Introduction 🙏=
'''CIELO''' stands for '''C'''rystals '''I'''n '''E'''thyl-acetate '''L'''eisurely '''O'''ver-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<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.

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

= Materials 🛒=
*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)

[[File:IMG 20210608 223040865 copy 800x600.jpg|center]]
<center>''Fig. 1: Over the counter materials.</center>

= 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 <ref>69ron's Limonene TEK[https://wiki.dmt-nexus.me/69ron%27s_D-Limonene_Mescaline_Extraction]</ref>.

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]]
<center>''Fig. 2: Cactus lime paste. Appearance can vary.</center>

== 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 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.

[[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 ✨==
'''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.

''Note:'' Citric acid is relatively soluble in ethyl acetate (50mg/g). A common question when mescaline citrate precipitates is how does one know that citric acid is not what is precipitating? The answer is simply that citric acid does not precipitate and stays in solution because it is bellow its saturation point. The white particles that form from the clouds are mescaline citrate and not citric acid.

[[File:IMG 20210311 144419793 (1) copy 800x600.jpg|center]]<center>''Fig. 4: Crystals in ethyl acetate. Appearance will vary.</center>

== 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<ref>Cactus analysis thread[https://www.dmt-nexus.me/forum/default.aspx?g=posts&t=71353]</ref>. 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<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]]
<center>''Fig. 5: Final mescaline citrate crystals. Appearance will vary.</center>

Mass spectrometry (MS) results from solaris analytical<ref>Solaris analytical service[https://www.solarisanalytical.com/]</ref> indicate the product is very clean mescaline (Fig. 6).

[[File: Cactus-extract copy 800x600_1.jpg|center]]''<center>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. </center>

== Reclaim Solvent 💚==
Reusing solvents is encouraged<ref>On reusing non polar solvent[https://www.dmt-nexus.me/forum/default.aspx?g=posts&t=31398]</ref> 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 8-10 minutes incorporating milky water with cactus, 6x3 minute pulls, and 15 mg/gram citric acid). 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.

= 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<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,

'''<span style="color: Orange"> <div style="text-align: center;">Chlorophyll + 2OH<sup>-</sup> ⇒ Chlorophyllin<sup>--</sup> + Phytol + Ethanol</div></span>'''

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):

'''<span style="color: Orange"> <div style="text-align: center;">3Mes<sub>(↑)</sub> + H3Cit<sub>(↑)</sub> ⇒ 3(MesH)Cit<sub>(↓)</sub></div></span>'''

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>).

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<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 💖==

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 🗝️=
<references/>

CIELO

2021-07-04T04:10:16Z

Shroombee: /* Crystalize ✨ */

= Introduction 🙏=
'''CIELO''' stands for '''C'''rystals '''I'''n '''E'''thyl-acetate '''L'''eisurely '''O'''ver-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<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.

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

= Materials 🛒=
*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)

[[File:IMG 20210608 223040865 copy 800x600.jpg|center]]
<center>''Fig. 1: Over the counter materials.</center>

= 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 <ref>69ron's Limonene TEK[https://wiki.dmt-nexus.me/69ron%27s_D-Limonene_Mescaline_Extraction]</ref>.

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]]
<center>''Fig. 2: Cactus lime paste. Appearance can vary.</center>

== 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 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.

[[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 ✨==
'''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.

''Note:'' Citric acid is relatively soluble in ethyl acetate (50mg/g). A common question when mescaline citrate precipitates is how does one know that citric acid is not what is precipitating? The answer is simply that citric acid does not precipitate and stays in solution because it is bellow its saturation point. The white particles that form from the clouds are mescaline citrate and not citric acid.

[[File:IMG 20210311 144419793 (1) copy 800x600.jpg|center]]<center>''Fig. 4: Crystals in ethyl acetate. Appearance will vary.</center>

== 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<ref>Cactus analysis thread[https://www.dmt-nexus.me/forum/default.aspx?g=posts&t=71353]</ref>. 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<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]]
<center>''Fig. 5: Final mescaline citrate crystals. Appearance will vary.</center>

Mass spectrometry (MS) results from solaris analytical<ref>Solaris analytical service[https://www.solarisanalytical.com/]</ref> indicate the product is very clean mescaline (Fig. 6).

[[File: Cactus-extract copy 800x600_1.jpg|center]]''<center>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. </center>

== Reclaim Solvent 💚==
Reusing solvents is encouraged<ref>On reusing non polar solvent[https://www.dmt-nexus.me/forum/default.aspx?g=posts&t=31398]</ref> 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 8-10 minutes incorporating milky water with cactus, 6x3 minute pulls, and 15 mg/gram citric acid). 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?

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.

= 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<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,

'''<span style="color: Orange"> <div style="text-align: center;">Chlorophyll + 2OH<sup>-</sup> ⇒ Chlorophyllin<sup>--</sup> + Phytol + Ethanol</div></span>'''

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):

'''<span style="color: Orange"> <div style="text-align: center;">3Mes<sub>(↑)</sub> + H3Cit<sub>(↑)</sub> ⇒ 3(MesH)Cit<sub>(↓)</sub></div></span>'''

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>).

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<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 💖==

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 🗝️=
<references/>

CIELO

2021-07-04T04:02:54Z

Shroombee: /* Crystalize ✨ */

= Introduction 🙏=
'''CIELO''' stands for '''C'''rystals '''I'''n '''E'''thyl-acetate '''L'''eisurely '''O'''ver-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<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.

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

= Materials 🛒=
*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)

[[File:IMG 20210608 223040865 copy 800x600.jpg|center]]
<center>''Fig. 1: Over the counter materials.</center>

= 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 <ref>69ron's Limonene TEK[https://wiki.dmt-nexus.me/69ron%27s_D-Limonene_Mescaline_Extraction]</ref>.

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]]
<center>''Fig. 2: Cactus lime paste. Appearance can vary.</center>

== 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 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.

[[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 ✨==
'''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 15 grams of citric acid (approximately 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.

''Note:'' Citric acid is relatively soluble in ethyl acetate (50mg/g). A common question when mescaline citrate precipitates is how does one know that citric acid is not what is precipitating? The answer is simply that citric acid does not precipitate and stays in solution because it is bellow its saturation point. The white particles that form from the clouds are mescaline citrate and not citric acid.

[[File:IMG 20210311 144419793 (1) copy 800x600.jpg|center]]<center>''Fig. 4: Crystals in ethyl acetate. Appearance will vary.</center>

== 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<ref>Cactus analysis thread[https://www.dmt-nexus.me/forum/default.aspx?g=posts&t=71353]</ref>. 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<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]]
<center>''Fig. 5: Final mescaline citrate crystals. Appearance will vary.</center>

Mass spectrometry (MS) results from solaris analytical<ref>Solaris analytical service[https://www.solarisanalytical.com/]</ref> indicate the product is very clean mescaline (Fig. 6).

[[File: Cactus-extract copy 800x600_1.jpg|center]]''<center>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. </center>

== Reclaim Solvent 💚==
Reusing solvents is encouraged<ref>On reusing non polar solvent[https://www.dmt-nexus.me/forum/default.aspx?g=posts&t=31398]</ref> 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 8-10 minutes incorporating milky water with cactus, 6x3 minute pulls, and 15 mg/gram citric acid). 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?

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.

= 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<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,

'''<span style="color: Orange"> <div style="text-align: center;">Chlorophyll + 2OH<sup>-</sup> ⇒ Chlorophyllin<sup>--</sup> + Phytol + Ethanol</div></span>'''

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):

'''<span style="color: Orange"> <div style="text-align: center;">3Mes<sub>(↑)</sub> + H3Cit<sub>(↑)</sub> ⇒ 3(MesH)Cit<sub>(↓)</sub></div></span>'''

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>).

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<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 💖==

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 🗝️=
<references/>

CIELO

2021-07-04T03:57:28Z

Shroombee: /* Crystalize ✨ */

= Introduction 🙏=
'''CIELO''' stands for '''C'''rystals '''I'''n '''E'''thyl-acetate '''L'''eisurely '''O'''ver-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<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.

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

= Materials 🛒=
*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)

[[File:IMG 20210608 223040865 copy 800x600.jpg|center]]
<center>''Fig. 1: Over the counter materials.</center>

= 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 <ref>69ron's Limonene TEK[https://wiki.dmt-nexus.me/69ron%27s_D-Limonene_Mescaline_Extraction]</ref>.

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]]
<center>''Fig. 2: Cactus lime paste. Appearance can vary.</center>

== 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 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.

[[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 ✨==
''Slow crystalization option:'' Drop citric acid 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:'' Use 15g of citric acid and continuous magnetic stirring (or continuous shaking) to both dissolve citric acid quickly 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.

''Note:'' Citric acid is relatively soluble in ethyl acetate (50mg/g). A common question when mescaline citrate precipitates is how does one know that citric acid is not what is precipitating? The answer is simply that citric acid does not precipitate and stays in solution because it is bellow its saturation point. The white particles that form from the clouds are mescaline citrate and not citric acid.

[[File:IMG 20210311 144419793 (1) copy 800x600.jpg|center]]<center>''Fig. 4: Crystals in ethyl acetate. Appearance will vary.</center>

== 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<ref>Cactus analysis thread[https://www.dmt-nexus.me/forum/default.aspx?g=posts&t=71353]</ref>. 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<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]]
<center>''Fig. 5: Final mescaline citrate crystals. Appearance will vary.</center>

Mass spectrometry (MS) results from solaris analytical<ref>Solaris analytical service[https://www.solarisanalytical.com/]</ref> indicate the product is very clean mescaline (Fig. 6).

[[File: Cactus-extract copy 800x600_1.jpg|center]]''<center>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. </center>

== Reclaim Solvent 💚==
Reusing solvents is encouraged<ref>On reusing non polar solvent[https://www.dmt-nexus.me/forum/default.aspx?g=posts&t=31398]</ref> 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 8-10 minutes incorporating milky water with cactus, 6x3 minute pulls, and 15 mg/gram citric acid). 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?

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.

= 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<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,

'''<span style="color: Orange"> <div style="text-align: center;">Chlorophyll + 2OH<sup>-</sup> ⇒ Chlorophyllin<sup>--</sup> + Phytol + Ethanol</div></span>'''

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):

'''<span style="color: Orange"> <div style="text-align: center;">3Mes<sub>(↑)</sub> + H3Cit<sub>(↑)</sub> ⇒ 3(MesH)Cit<sub>(↓)</sub></div></span>'''

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>).

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<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 💖==

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 🗝️=
<references/>

CIELO

2021-07-04T03:54:31Z

Shroombee: /* Extract 👨🏾‍🔬 */

= Introduction 🙏=
'''CIELO''' stands for '''C'''rystals '''I'''n '''E'''thyl-acetate '''L'''eisurely '''O'''ver-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<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.

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

= Materials 🛒=
*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)

[[File:IMG 20210608 223040865 copy 800x600.jpg|center]]
<center>''Fig. 1: Over the counter materials.</center>

= 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 <ref>69ron's Limonene TEK[https://wiki.dmt-nexus.me/69ron%27s_D-Limonene_Mescaline_Extraction]</ref>.

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]]
<center>''Fig. 2: Cactus lime paste. Appearance can vary.</center>

== 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 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.

[[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 ✨==
Drop citric acid 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: Use 15g of citric acid and continuous magnetic stirring (or continuous shaking) to both dissolve citric acid quickly 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.

''Note:'' Citric acid is relatively soluble in ethyl acetate (50mg/g). A common question when mescaline citrate precipitates is how does one know that citric acid is not what is precipitating? The answer is simply that citric acid does not precipitate and stays in solution because it is bellow its saturation point. The white particles that form from the clouds are mescaline citrate and not citric acid.

[[File:IMG 20210311 144419793 (1) copy 800x600.jpg|center]]<center>''Fig. 4: Crystals in ethyl acetate. Appearance will vary.</center>

== 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<ref>Cactus analysis thread[https://www.dmt-nexus.me/forum/default.aspx?g=posts&t=71353]</ref>. 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<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]]
<center>''Fig. 5: Final mescaline citrate crystals. Appearance will vary.</center>

Mass spectrometry (MS) results from solaris analytical<ref>Solaris analytical service[https://www.solarisanalytical.com/]</ref> indicate the product is very clean mescaline (Fig. 6).

[[File: Cactus-extract copy 800x600_1.jpg|center]]''<center>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. </center>

== Reclaim Solvent 💚==
Reusing solvents is encouraged<ref>On reusing non polar solvent[https://www.dmt-nexus.me/forum/default.aspx?g=posts&t=31398]</ref> 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 8-10 minutes incorporating milky water with cactus, 6x3 minute pulls, and 15 mg/gram citric acid). 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?

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.

= 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<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,

'''<span style="color: Orange"> <div style="text-align: center;">Chlorophyll + 2OH<sup>-</sup> ⇒ Chlorophyllin<sup>--</sup> + Phytol + Ethanol</div></span>'''

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):

'''<span style="color: Orange"> <div style="text-align: center;">3Mes<sub>(↑)</sub> + H3Cit<sub>(↑)</sub> ⇒ 3(MesH)Cit<sub>(↓)</sub></div></span>'''

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>).

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<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 💖==

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 🗝️=
<references/>

CIELO

2021-07-04T03:51:14Z

Shroombee: /* Extract 👨🏾‍🔬 */

= Introduction 🙏=
'''CIELO''' stands for '''C'''rystals '''I'''n '''E'''thyl-acetate '''L'''eisurely '''O'''ver-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<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.

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

= Materials 🛒=
*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)

[[File:IMG 20210608 223040865 copy 800x600.jpg|center]]
<center>''Fig. 1: Over the counter materials.</center>

= 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 <ref>69ron's Limonene TEK[https://wiki.dmt-nexus.me/69ron%27s_D-Limonene_Mescaline_Extraction]</ref>.

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]]
<center>''Fig. 2: Cactus lime paste. Appearance can vary.</center>

== 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 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. '''Extract needs to be clean''' (see Fig. 3). To be sure extract is clean, one extra pass through a fresh coffee filter after settling is recommended.

[[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 ✨==
Drop citric acid 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: Use 15g of citric acid and continuous magnetic stirring (or continuous shaking) to both dissolve citric acid quickly 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.

''Note:'' Citric acid is relatively soluble in ethyl acetate (50mg/g). A common question when mescaline citrate precipitates is how does one know that citric acid is not what is precipitating? The answer is simply that citric acid does not precipitate and stays in solution because it is bellow its saturation point. The white particles that form from the clouds are mescaline citrate and not citric acid.

[[File:IMG 20210311 144419793 (1) copy 800x600.jpg|center]]<center>''Fig. 4: Crystals in ethyl acetate. Appearance will vary.</center>

== 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<ref>Cactus analysis thread[https://www.dmt-nexus.me/forum/default.aspx?g=posts&t=71353]</ref>. 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<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]]
<center>''Fig. 5: Final mescaline citrate crystals. Appearance will vary.</center>

Mass spectrometry (MS) results from solaris analytical<ref>Solaris analytical service[https://www.solarisanalytical.com/]</ref> indicate the product is very clean mescaline (Fig. 6).

[[File: Cactus-extract copy 800x600_1.jpg|center]]''<center>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. </center>

== Reclaim Solvent 💚==
Reusing solvents is encouraged<ref>On reusing non polar solvent[https://www.dmt-nexus.me/forum/default.aspx?g=posts&t=31398]</ref> 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 8-10 minutes incorporating milky water with cactus, 6x3 minute pulls, and 15 mg/gram citric acid). 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?

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.

= 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<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,

'''<span style="color: Orange"> <div style="text-align: center;">Chlorophyll + 2OH<sup>-</sup> ⇒ Chlorophyllin<sup>--</sup> + Phytol + Ethanol</div></span>'''

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):

'''<span style="color: Orange"> <div style="text-align: center;">3Mes<sub>(↑)</sub> + H3Cit<sub>(↑)</sub> ⇒ 3(MesH)Cit<sub>(↓)</sub></div></span>'''

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>).

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<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 💖==

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 🗝️=
<references/>

CIELO

2021-07-04T03:44:08Z

Shroombee: /* Paste 🌵 */

CIELO

2021-07-04T03:38:53Z

Shroombee: /* Equipment */

CIELO

2021-07-04T03:36:53Z

Shroombee: /* Paste 🌵 */

CIELO

2021-07-04T03:34:30Z

Shroombee:

CIELO

2021-03-12T22:58:17Z

Shroombee: /* Experiment #2 */

{{ShowInfo|[[Image:Note_error.png]]|'''Note:'''|This page is a workplace for an experimental process. It is intended to summarize information from ongoing discussions in the forum. Feel free to update this page with any observations or comments. Wiki changes are reversible so you can't break anything - be bold. This page is not currently linked to the main wiki and will remain as such until the process is independently verified by others.}}

= Introduction =

'''CIELO''' stands for '''C'''rystals '''I'''n '''E'''thyl-acetate '''L'''eisurely '''O'''TC (Over The Counter).

In this TEK, aqueous alkaline cactus paste is extracted with ethyl acetate. The extract is salted with citric acid to precipitate mescaline citrate crystals directly in the solvent.

== Materials ==

* Quart jars with LDPE or PP plastic lids (e.g. below)
* Food scale
* 300g water
* 25g Ca(OH)2 (lime)
* 100g powdered dry cacti
* ~ 1000g ethyl acetate ("MEK substitute")
* Coffee filters
* pH paper
* Citric acid
* Shallow baking dish
* Scraping tool (e.g. razor blade)

[[File:Plastics.png|center]]

== Safety ==

Review ethyl acetate's safety information<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 check the manufacture's MSDS to verify you have pure ethyl acetate.

Each adult individual needs to find and review any other relevant safety information throughly and make their own personal decision on proceeding.

== Process ==

=== Paste ===

Mix water and lime. Add cactus powder and mix to a homogeneous paste for a few minutes.

[[File:Screenshot_20210311-161134.png|center]]

=== Pull ===

Add ~ 200g of ethyl acetate to the paste. Extract by mixing very gently for 30 seconds followed by 10 minutes of settling. Decant to a second jar. If needed, a coffee filter covering the mouth of the jar and secured with a metal screw ring will keep the paste in the first jar (tear off excess filter paper and poke a breathing hole on one side).

It is important to never shake or stir quickly to minimize the ammount of solvent binding to the paste.

Pull three more times. Progress can be monitored with pH paper (green color indicates free base presence). Paste will change during the pulls and can become gunky.

Combined pulls will give ~a quart of deep green extract (see image below up against a window with horizontal blinds). Optionally, more pulls can be done into a different jar for a modest yield improvement.

[[File:Screenshot_20210311-161548.png| center]]

=== Salt ===

Dissolve ~500mg (~1/8 tsp) of citric acid into the extract making it cloudy. Test with pH paper, salting is complete when pH paper is acidic with excess acid in solution. If needed, add more citric acid in small increments of ~100mg until salting is complete.

Move extract to fridge for 12-72h. White xtals should form towards the bottom of the jar.

[[File:Screenshot_20210311-162001.png|center]]

If there are issues with chrystalization, it should still be possible to recover any product present with water pulls followed by evaporation and ethyl acetate washes.

=== Finish ===

Decant ethyl acetate into a storage jar for reuse, using a filter to catch any loose crystals. Rinse crystals with fresh ethyl acetate at least once or until green color is removed to personal cosmetic satisfaction. Dissolve crystals in minimal warm water and passively evaporate undisturbed in a shallow baking dish. Finally, scrape up the resulting long crystal needles.

Mass spectrometry (MS) results from solaris analytical<ref>Solaris analytical service[https://www.solarisanalytical.com/]</ref> indicate the product is very clean mescaline after only two ethyl acetate rinses with some minor discoloration remaining. See MS spectrum below, peak near 210.5 is mescaline. Peaks at and 193.6, 178.4, and 162.0 are believed to be mescaline with amine/methyl/methoxy groups cleaved to generate the lower mass mescaline spectrum in multiples of ~16 au (16.9, 32.1, and 48.5 respectively). The small peak at 239.5 is not attributed to mescaline.

[[File: Screenshot_20210310-062431.png|center]]

== Lab Notes ==

The pulls appear to be very efficient, extracting mescaline within minutes. The similarity between the solvent's ethoxy group and mescaline's methoxy groups could contribute to the solubility.

It is possible to chemically dry the extract with a drying agent such as anhydrous MgSO4 before salting. However, no clear yield benefit was observed by performing this step. Surprisingly, solutions carefully dried with anhydrous CaCl2 followed by K2CO3 had difficulty crystalizing, indicating that a some water is desirable for crystalization. This points to the precipitate from this TEK maybe being hydrate salt. Regardless of the reason, the water content in ethyl acetate directly from the pulls is in a good range experimentally.

During salting, every 10mg of citric acid ('''CitH3''') reacts with enough free base mescaline ('''Mes''') to precipitate up to 43mg of mescaline citrate (or slightly more if a hydrate form is precipitating):

'''<span style="color: Orange"> <div style="text-align: center;">3Mes<sub>(↑)</sub> + CitH3<sub>(↑)</sub> ⇒ 3(MesH)Cit<sub>(↓)</sub></div></span>'''

250mg of citric acid are enough for the typical cactus (up to 1% yield). However, and outlier like the legendary Ogun would need ~1100mg of citric acid for a 4.7% yield.

Over acidifying helps precipitate crystals better. This is a simple lab observation, compatible with Le Chatelier's principle. There is room for excess citric acid in solution since several grams can dissolve in a quart of ethyl acetate even when chilled. The vast majority of excess acid is poured off after salting, and any traces removed when washing the crystals.

Other solid organic acids could work. Fumaric acid was tested and gave wispy tiny crystals (not ideal). Malic was tested and slowly crystalized from a dry solution. Tartaric could not crystalize well from dry a dried extract, but began to crystalize with some water added (similar to citric acid). There are many other solid organic acids soluble in ethyl acetate that can be tested (ascorbic, succinic, etc).

It is possible that some of the assumptions and conclusions in these lab notes are incorrect or incomplete. The process was tested in several ways, but the search was not exhaustive<ref>Ethyl acetate approach[https://www.dmt-nexus.me/forum/default.aspx?g=posts&t=96262]</ref>. There could be ways to improve this process.

== References ==
<references/>

== Appendix: Shroombee's Notes ==

=== Experiment #2 ===

'''March 12, 2021'''

'''8:45 am''' Weighed out 100 grams cactus chips (will use 50 grams for this experiment and the other 50 grams in a followup experiment).

'''8:48 am''' Ground cactus chips to very fine powder in Vitamix for 2 minutes, eventually hitting highest speed.

'''8:50 am''' Weighed out 12.5 grams lime, 153.1 grams purified water, 50.5 grams finely ground cactus powder.

'''8:58 am''' Mixed water and lime together in a stainless steel mixing bowl to make a milky water. Gradually added cactus powder, incorporating powder into milky water. Cactus gets to a fluffy texture and then transitions to being a little more clumpy. Finished mixing at 9:05 am.

'''9:11 am''' Added 99.8 grams ethyl acetate to the cactus for pull #1. Mixed gently for 30 seconds.

'''In retrospect, do not mix at all. Just push the cactus around a little so the ethyl acetate can run through the cactus.''' Solvent quickly turns green.

'''9:23 am''' After letting the cactus and ethyl acetate sit for 10 minutes, decanted the ethyl acetate into a beaker with a metal coffee filter sitting inside the top of the beaker (works well). Beaker plus filter beforehand was 342.3 grams. After decanting solvent into it, 372.8 grams.

'''Solvent recovery for pull #1 = 30.5 grams (out of 99.8 grams added).''' For next experiment, see if not mixing at all will reduce the amount of solvent that the cactus absorbs. A drop of solvent on pH paper turns the paper dark green (not blackish green though).

'''9:28 am''' Added 110.1 grams fresh ethyl acetate to cactus for pull #2. Very gently pushing the cactus for about 10 seconds, just to get the solvent to run through the cactus. The ethyl acetate quickly turns green.

'''9:31 am''' Moved pull #1 to a mason jar. Mason jar beforehand is 426.8 grams. After is 456.6 grams. 29.8 grams solvent moved from beaker to mason jar.

'''9:38 am''' After 10 minutes sitting with the cactus, decanted pull #2 into the beaker. Beaker is 342.3 grams before, 447.9 grams after.

'''Solvent recovery for pull #2 = 105.6 grams (out of 110.1 grams added).''' pH paper is medium dark green.

'''9:45 am''' Added 103.3 grams fresh ethyl acetate to the cactus for pull #3. Almost no manipulation of the cactus at this point. Solvent quickly gets green color.

'''9:46 am''' Moved pull #2 to the mason jar (combining with pull #1). Mason jar beforehand is 456.4 grams. After is 560.4 grams. 104.0 grams solvent moved from beaker to mason jar. Interesting at 9:31 am the mason jar weighed 456.6 grams. 15 minutes later it weighs 456.4 grams. Is this evaporation of ethyl acetate or error in the scale? Scale supposed to be accurate to 0.1 grams.

'''9:55 am''' After 10 minutes sitting with the cactus, decanted pull #3 into the beaker. Beaker is 342.5 grams before, 450.3 grams after.

'''Solvent recovery for pull #3 = 107.8 grams (out of 103.3 grams added).''' We got back the amount we added for pull #3, plus a few more grams. The paste is starting to stick to itself, making it easy to decant and pour solvent out of the mixing bowl by holding the paste back with a strainer/skimmer ladle. pH paper is light green.

'''10:00 am''' Added 103.9 grams fresh ethyl acetate to the cactus for pull #4. As with pull #3, almost no manipulation of the cactus. Just pushing the cactus under the solvent. Solvent picks up green color.

'''10:08 am''' Moved pull #3 to the mason jar (combining with pull #1 and pull #2). Mason jar beforehand is 560.2. After is 667.0 grams. 106.8 grams solvent moved from beaker to mason jar. As before, mason jar seems to have lost 0.2 grams of solvent. The solvent in the mason jar is a beautiful emerald green.

'''10:10 am''' After 10 minutes sitting with the cactus, decanted pull #4 into the beaker. Beaker is 342.7 grams before, 444.7 grams after.

'''Solvent recovery for pull #4 = 102.0 grams (out of 103.9 grams added).''' pH paper is faint green. After drying, the paper barely has any greenish tint.

'''10:16 am''' Added 104.0 grams fresh ethyl acetate to the cactus for pull #5. Almost no manipulation of the cactus. Solvent picks up a light green tint.

'''10:20 am''' Moved pull #4 to the mason jar (combining with pull #1-3). Mason jar beforehand is 666.9 grams. After is 767.8 grams. 100.9 grams solvent moved from beaker to mason jar. Mason jar lost 0.1 grams solvent since 10:08 am.

'''10:26 am''' After 10 minutes sitting with the cactus, decanted pull #5 into the beaker. Beaker is 342.5 grams before, 446.0 grams after.

'''Solvent recovery for pull #5 = 103.5 grams (out of 104.0 grams added).''' pH paper has no materially significant color change. After drying, the paper shows no color change. This pull is NOT being combined with pulls #1-4 since it does not appear to have any freebase mescaline. Will consider what technique to use to see if there is any mescaline to be obtained from this pull.

'''Total solvent added = 99.8 + 110.1 + 103.3 + 103.9 + 104.0 = 521.1 grams. Total solvent recovered = 30.5 + 105.6 + 107.8 + 102.0 + 103.5 = 449.4 grams. Lost 71.7 grams solvent to the cactus (almost all in pull #1).'''

'''10:46 am''' Washed and dried the metal coffee filter. Then added a paper filter into the metal filter. Ran pulls #1-4 through the metal+paper filter and into a new mason jar. Ran pull #5 through the metal+paper filter and into a separate mason jar. The purpose of filtering again is that I noticed a few bits of cactus material got into the combined decanted solvent. I don't know how that occurred since the metal filter is a fine mesh filter. In any case, now we have filtered solvent.

'''10:52 am''' Added 254 grams of citric acid to the combined pulls mason jar. Clouds form in the solvent. Stirred gently with a spoon. pH paper comes out yellow.

'''10:56 am''' Put a stainless steel lid with silicone liner on the mason jar. Put mason jar into the frig to wait for crystals.

'''1:45 pm''' Mason jar is in the frig. Solvent is opaque. No crystals yet.

=== Experiment #1 ===

'''March 9, 2021'''

'''6:42 pm'''

100 grams Peruvian Torch chips

298 grams purified water

Blended cactus chips in the Vitamix dry container so it becomes a fine powder.

'''6:58 pm'''
Mixed cactus powder and water in a plastic mixing bowl rather than a mason jar because it seems easier. Product is a fluffy texture, olive green color. There is no excess water.

The bowl plus cactus plus silicone mixing spoon weighs 826.5 grams. Microwave on high for 30 seconds, mix, then weigh. This is pretty easy. I wouldn't want to do this in a mason jar. The cactus does not bubble and there is no issue at 30 seconds with anything bubbling over. Weight after each 30 second cycle:

825.6 grams

823.9 grams

820.2 grams

816.0 grams

808.7 grams

800.7 grams

791.3 grams

783.2 grams

775.8 grams

765.8 grams

DONE

After a couple of the microwaving cycles, the cactus lost its fluffiness and became like light bread dough, not sticking much to the bowl.

'''7:25 pm''' Begin slowly mixing in 25 grams pickling lime. Started with the plastic bowl but switched to a ceramic bowl after a minute, not knowing how the plastic would react to the base. Bowl appears fine after washing it out.

'''7:39 pm''' I'm using a fork to try to get the lime mixed evenly. I figure my Kitchenaid stand mixer will be easier so I break that out.

'''7:45 pm''' Letting the Kitchenaid stir the cactus for me. Much easier!

'''7:53 pm''' Added 25 grams calcium chloride. Before adding, the cactus paste was fluffy and stuck to the sides of the stainless steel bowl. After adding the calcium chloride, the cactus became like clumpy sand and hardly stuck to the sides of the bowl.

'''7:58 pm''' Stopped mixing.

'''8:05 pm''' Transferred cactus to a wide mouth quart mason jar and added 220 ml of ethyl acetate (weighing 199.9 grams). The ethyl acetate came up to approximately 540 ml on the side of the mason jar. After shaking, the cactus looked like fluffy beach sand.

'''8:28 pm''' Shake for a minute.

'''9:00 pm''' Shake for a minute.

'''9:22 pm''' No shaking, I notice the ethyl acetate is light green.

'''10:30 pm''' Shake for a minute. The cactus is starting to get a little stickier, leaving streaks on the glass.

'''11:00 pm''' Ethyl acetate comes up to exactly 500 ml on the side of the mason jar. Versus ~540 ml at 8:05 pm when the ethyl acetate was first added. '''What accounts for this 40 ml difference?'''

'''12:00 am''' Shake for a minute.

'''1:06 am''' Weighed mason jar with cactus: 1001.4 grams.

'''March 10, 2021'''

'''7:57 am''' Weighed mason jar with cactus: 1001.1 grams.

Ready to decant ethyl acetate. Large pyrex beaker with metal coffee filter weighs 342.3 grams. Ethyl acetate is a medium, emerald green. Definitely not light green and not yellow.

Using a small ladle to decant, which gets most of the ethyl acetate with no plant matter. Beaker weighs 427.2 grams meaning we recovered 84.9 grams of ethyl acetate. Not too good.

I transferred the cactus to a french press to see if I could recover more ethyl acetate. The sticky paste does not compress and I recovered an additional ~6 grams ethyl acetate. '''French press is obviously not worth the effort!'''

'''8:21 am''' Done with decanting, transferring, french pressing, weighing, et cetera. Total recovery for this pull is 90.6 grams ethyl acetate.

'''8:23 am''' Added 90.7 grams of fresh ethyl acetate to the mason jar. Stirred ethyl acetate into the sticky cactus, did not shake. Ethyl acetate is already changing to green color.

'''8:33 am''' Photo of pH paper. Paper is dark green. pH 10 or 11? Also tested using the 4 color pH strips. More difficult to judge the pH with these.

'''8:34 am''' Photo of recovered ethyl acetate showing it is an emerald green color.

'''8:45 am''' Poured 10 ml of ethyl acetate into a small beaker. Added 13 mg of citric acid. Lower half of the beaker turned milky, cloudy. Checked pH and it's basically the same as the rest of the solvent. So the small amount of citric acid didn't change the pH much. I used a disposable pipette and pulled from the top of the solvent, so perhaps the top layer didn't have a chance to react yet.

'''8:49 am''' Photo showing cloudy 10 ml in small beaker.

'''8:50 am''' Poured the 10 ml and the rest of the solvent into a mini Pyrex baking dish, using the larger volume of solvent to rinse out of the small beaker. I probably should have left the solvent in a mason jar or beaker rather than adding to the baking dish. Added 95 mg of citric acid. Stirred a little because I wanted to get a more accurate pH. pH was about 7. Added an additional 61 mg citric acid. pH went to about 6. Total citric acid added to the 90.6 grams ethyl acetate is 169 mg. Even after rinsing with the main solvent, the bottom of the small beaker has some spots that look like something crystalizing. I don't know if it's just sticky citric acid or ???

'''9:07 am''' Photo of 3 pH test strips.

'''3:42 pm''' Moving the dish to the freezer. Solvent is clear (and has been clear for at least a few hours). Initially I thought there were droplets on the bottom of the dish (around 11:00 am). Then tried to scrape at them with a knife and not seeing any movement, I figured they were a reflection from the surface because I noticed some tiny droplets on the surface if I caught the light at the right angle. Then as I tipped the dish at 3:42pm to move it into the freezer, I now see the droplets really are at the bottom of the dish. Sort of an oily substance. There are no crystals.

'''8:00 pm''' Retrieving pull #2. Beaker plus metal coffee filter weigh 342.3 grams. Weighs 407.5 grams after decanting. Recovered 65.2 grams. Looks like the cactus sucked up more solvent even though I didn't shake. pH is basic, although the pH paper is not as dark green as pull #1.

'''8:09 pm''' Removed a few tablespoons of sticky slimy cactus and put it into a separate bowl. Mixed in 5.4 grams of calcium chloride (which is a lot relative to the amount of cactus). Even waiting more than 30 minutes, no additional solvent is released. The cactus is drier though, more clumpy, and lost some gooey sliminess.

'''8:27 pm''' Since only 65.2 grams of solvent was retrieved, I decided adding this amount of fresh solvent for pull #3 would be too inefficient. I added 197.6 grams fresh ethyl acetate and stirred for 1-2 minutes. Solvent turned a light green fairly quickly.

'''8:38 pm''' Added 49 mg citric acid to the recovered solvent. Bottom of jar got milky. Tested pH with 3 strips. (1) Took a solvent sample towards the bottom of the jar at the clouds: pH about 5. (2) Solvent sample at the surface: pH about 7. (3) Swirled the jar around then took a solvent sample. pH about 6.

'''8:45 pm''' Put jar into freezer.

CIELO

2021-03-12T21:47:31Z

Shroombee: /* Appendix: Shroombee's Notes */

{{ShowInfo|[[Image:Note_error.png]]|'''Note:'''|This page is a workplace for an experimental process. It is intended to summarize information from ongoing discussions in the forum. Feel free to update this page with any observations or comments. Wiki changes are reversible so you can't break anything - be bold. This page is not currently linked to the main wiki and will remain as such until the process is independently verified by others.}}

= Introduction =

'''CIELO''' stands for '''C'''rystals '''I'''n '''E'''thyl-acetate '''L'''eisurely '''O'''TC (Over The Counter).

In this TEK, aqueous alkaline cactus paste is extracted with ethyl acetate. The extract is salted with citric acid to precipitate mescaline citrate crystals directly in the solvent.

== Materials ==

* Quart jars with LDPE or PP plastic lids (e.g. below)
* Food scale
* 300g water
* 25g Ca(OH)2 (lime)
* 100g powdered dry cacti
* ~ 1000g ethyl acetate ("MEK substitute")
* Coffee filters
* pH paper
* Citric acid
* Shallow baking dish
* Scraping tool (e.g. razor blade)

[[File:Plastics.png|center]]

== Safety ==

Review ethyl acetate's safety information<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 check the manufacture's MSDS to verify you have pure ethyl acetate.

Each adult individual needs to find and review any other relevant safety information throughly and make their own personal decision on proceeding.

== Process ==

=== Paste ===

Mix water and lime. Add cactus powder and mix to a homogeneous paste for a few minutes.

[[File:Screenshot_20210311-161134.png|center]]

=== Pull ===

Add ~ 200g of ethyl acetate to the paste. Extract by mixing very gently for 30 seconds followed by 10 minutes of settling. Decant to a second jar. If needed, a coffee filter covering the mouth of the jar and secured with a metal screw ring will keep the paste in the first jar (tear off excess filter paper and poke a breathing hole on one side).

It is important to never shake or stir quickly to minimize the ammount of solvent binding to the paste.

Pull three more times. Progress can be monitored with pH paper (green color indicates free base presence). Paste will change during the pulls and can become gunky.

Combined pulls will give ~a quart of deep green extract (see image below up against a window with horizontal blinds). Optionally, more pulls can be done into a different jar for a modest yield improvement.

[[File:Screenshot_20210311-161548.png| center]]

=== Salt ===

Dissolve ~500mg (~1/8 tsp) of citric acid into the extract making it cloudy. Test with pH paper, salting is complete when pH paper is acidic with excess acid in solution. If needed, add more citric acid in small increments of ~100mg until salting is complete.

Move extract to fridge for 12-72h. White xtals should form towards the bottom of the jar.

[[File:Screenshot_20210311-162001.png|center]]

If there are issues with chrystalization, it should still be possible to recover any product present with water pulls followed by evaporation and ethyl acetate washes.

=== Finish ===

Decant ethyl acetate into a storage jar for reuse, using a filter to catch any loose crystals. Rinse crystals with fresh ethyl acetate at least once or until green color is removed to personal cosmetic satisfaction. Dissolve crystals in minimal warm water and passively evaporate undisturbed in a shallow baking dish. Finally, scrape up the resulting long crystal needles.

Mass spectrometry (MS) results from solaris analytical<ref>Solaris analytical service[https://www.solarisanalytical.com/]</ref> indicate the product is very clean mescaline after only two ethyl acetate rinses with some minor discoloration remaining. See MS spectrum below, peak near 210.5 is mescaline. Peaks at and 193.6, 178.4, and 162.0 are believed to be mescaline with amine/methyl/methoxy groups cleaved to generate the lower mass mescaline spectrum in multiples of ~16 au (16.9, 32.1, and 48.5 respectively). The small peak at 239.5 is not attributed to mescaline.

[[File: Screenshot_20210310-062431.png|center]]

== Lab Notes ==

The pulls appear to be very efficient, extracting mescaline within minutes. The similarity between the solvent's ethoxy group and mescaline's methoxy groups could contribute to the solubility.

It is possible to chemically dry the extract with a drying agent such as anhydrous MgSO4 before salting. However, no clear yield benefit was observed by performing this step. Surprisingly, solutions carefully dried with anhydrous CaCl2 followed by K2CO3 had difficulty crystalizing, indicating that a some water is desirable for crystalization. This points to the precipitate from this TEK maybe being hydrate salt. Regardless of the reason, the water content in ethyl acetate directly from the pulls is in a good range experimentally.

During salting, every 10mg of citric acid ('''CitH3''') reacts with enough free base mescaline ('''Mes''') to precipitate up to 43mg of mescaline citrate (or slightly more if a hydrate form is precipitating):

'''<span style="color: Orange"> <div style="text-align: center;">3Mes<sub>(↑)</sub> + CitH3<sub>(↑)</sub> ⇒ 3(MesH)Cit<sub>(↓)</sub></div></span>'''

250mg of citric acid are enough for the typical cactus (up to 1% yield). However, and outlier like the legendary Ogun would need ~1100mg of citric acid for a 4.7% yield.

Over acidifying helps precipitate crystals better. This is a simple lab observation, compatible with Le Chatelier's principle. There is room for excess citric acid in solution since several grams can dissolve in a quart of ethyl acetate even when chilled. The vast majority of excess acid is poured off after salting, and any traces removed when washing the crystals.

Other solid organic acids could work. Fumaric acid was tested and gave wispy tiny crystals (not ideal). Malic was tested and slowly crystalized from a dry solution. Tartaric could not crystalize well from dry a dried extract, but began to crystalize with some water added (similar to citric acid). There are many other solid organic acids soluble in ethyl acetate that can be tested (ascorbic, succinic, etc).

It is possible that some of the assumptions and conclusions in these lab notes are incorrect or incomplete. The process was tested in several ways, but the search was not exhaustive<ref>Ethyl acetate approach[https://www.dmt-nexus.me/forum/default.aspx?g=posts&t=96262]</ref>. There could be ways to improve this process.

== References ==
<references/>

== Appendix: Shroombee's Notes ==

=== Experiment #2 ===

'''March 12, 2021'''

'''8:45 am''' Weighed out 100 grams cactus chips (will use 50 grams for this experiment and the other 50 grams in a followup experiment).

'''8:48 am''' Ground cactus chips to very fine powder in Vitamix for 2 minutes, eventually hitting highest speed.

'''8:50 am''' Weighed out 12.5 grams lime, 153.1 grams purified water, 50.5 grams finely ground cactus powder.

'''8:58 am''' Mixed water and lime together in a stainless steel mixing bowl to make a milky water. Gradually added cactus powder, incorporating powder into milky water. Cactus gets to a fluffy texture and then transitions to being a little more clumpy. Finished mixing at 9:05 am.

'''9:11 am''' Added 99.8 grams ethyl acetate to the cactus for pull #1. Mixed gently for 30 seconds.

'''In retrospect, do not mix at all. Just push the cactus around a little so the ethyl acetate can run through the cactus.''' Solvent quickly turns green.

'''9:23 am''' After letting the cactus and ethyl acetate sit for 10 minutes, decanted the ethyl acetate into a beaker with a metal coffee filter sitting inside the top of the beaker (works well). Beaker plus filter beforehand was 342.3 grams. After decanting solvent into it, 372.8 grams.

'''Solvent recovery for pull #1 = 30.5 grams (out of 99.8 grams added).''' For next experiment, see if not mixing at all will reduce the amount of solvent that the cactus absorbs. A drop of solvent on pH paper turns the paper dark green (not blackish green though).

'''9:28 am''' Added 110.1 grams fresh ethyl acetate to cactus for pull #2. Very gently pushing the cactus for about 10 seconds, just to get the solvent to run through the cactus. The ethyl acetate quickly turns green.

'''9:31 am''' Moved pull #1 to a mason jar. Mason jar beforehand is 426.8 grams. After is 456.6 grams. 29.8 grams solvent moved from beaker to mason jar.

'''9:38 am''' After 10 minutes sitting with the cactus, decanted pull #2 into the beaker. Beaker is 342.3 grams before, 447.9 grams after.

'''Solvent recovery for pull #2 = 105.6 grams (out of 110.1 grams added).''' pH paper is medium dark green.

'''9:45 am''' Added 103.3 grams fresh ethyl acetate to the cactus for pull #3. Almost no manipulation of the cactus at this point. Solvent quickly gets green color.

'''9:46 am''' Moved pull #2 to the mason jar (combining with pull #1). Mason jar beforehand is 456.4 grams. After is 560.4 grams. 104.0 grams solvent moved from beaker to mason jar. Interesting at 9:31 am the mason jar weighed 456.6 grams. 15 minutes later it weighs 456.4 grams. Is this evaporation of ethyl acetate or error in the scale? Scale supposed to be accurate to 0.1 grams.

'''9:55 am''' After 10 minutes sitting with the cactus, decanted pull #3 into the beaker. Beaker is 342.5 grams before, 450.3 grams after.

'''Solvent recovery for pull #3 = 107.8 grams (out of 103.3 grams added).''' We got back the amount we added for pull #3, plus a few more grams. The paste is starting to stick to itself, making it easy to decant and pour solvent out of the mixing bowl by holding the paste back with a strainer/skimmer ladle. pH paper is light green.

'''10:00 am''' Added 103.9 grams fresh ethyl acetate to the cactus for pull #4. As with pull #3, almost no manipulation of the cactus. Just pushing the cactus under the solvent. Solvent picks up green color.

'''10:08 am''' Moved pull #3 to the mason jar (combining with pull #1 and pull #2). Mason jar beforehand is 560.2. After is 667.0 grams. 106.8 grams solvent moved from beaker to mason jar. As before, mason jar seems to have lost 0.2 grams of solvent. The solvent in the mason jar is a beautiful emerald green.

'''10:10 am''' After 10 minutes sitting with the cactus, decanted pull #4 into the beaker. Beaker is 342.7 grams before, 444.7 grams after.

'''Solvent recovery for pull #4 = 102.0 grams (out of 103.9 grams added).''' pH paper is faint green. After drying, the paper barely has any greenish tint.

'''10:16 am''' Added 104.0 grams fresh ethyl acetate to the cactus for pull #5. Almost no manipulation of the cactus. Solvent picks up a light green tint.

'''10:20 am''' Moved pull #4 to the mason jar (combining with pull #1-3). Mason jar beforehand is 666.9 grams. After is 767.8 grams. 100.9 grams solvent moved from beaker to mason jar. Mason jar lost 0.1 grams solvent since 10:08 am.

'''10:26 am''' After 10 minutes sitting with the cactus, decanted pull #5 into the beaker. Beaker is 342.5 grams before, 446.0 grams after.

'''Solvent recovery for pull #5 = 103.5 grams (out of 104.0 grams added).''' pH paper has no materially significant color change (indicating neutral pH). After drying, the paper shows no color change. This pull is NOT being combined with pulls #1-4 since it does not appear to have any freebase mescaline. Will consider what technique to use to see if there is any mescaline to be obtained from this pull.

'''Total solvent added = 99.8 + 110.1 + 103.3 + 103.9 + 104.0 = 521.1 grams. Total solvent recovered = 30.5 + 105.6 + 107.8 + 102.0 + 103.5 = 449.4 grams. Lost 71.7 grams solvent to the cactus (almost all in pull #1).'''

'''10:46 am''' Washed and dried the metal coffee filter. Then added a paper filter into the metal filter. Ran pulls #1-4 through the metal+paper filter and into a new mason jar. Ran pull #5 through the metal+paper filter and into a separate mason jar. The purpose of filtering again is that I noticed a few bits of cactus material got into the combined decanted solvent. I don't know how that occurred since the metal filter is a fine mesh filter. In any case, now we have filtered solvent.

'''10:52 am''' Added 254 grams of citric acid to the combined pulls mason jar. Clouds form in the solvent. Stirred gently with a spoon. pH paper comes out yellow (neutral pH).

'''10:56 am''' Put a stainless steel lid with silicone liner on the mason jar. Put mason jar into the frig to wait for crystals.

'''1:45 pm''' Mason jar is in the frig. Solvent is opaque. No crystals yet.

=== Experiment #1 ===

'''March 9, 2021'''

'''6:42 pm'''

100 grams Peruvian Torch chips

298 grams purified water

Blended cactus chips in the Vitamix dry container so it becomes a fine powder.

'''6:58 pm'''
Mixed cactus powder and water in a plastic mixing bowl rather than a mason jar because it seems easier. Product is a fluffy texture, olive green color. There is no excess water.

The bowl plus cactus plus silicone mixing spoon weighs 826.5 grams. Microwave on high for 30 seconds, mix, then weigh. This is pretty easy. I wouldn't want to do this in a mason jar. The cactus does not bubble and there is no issue at 30 seconds with anything bubbling over. Weight after each 30 second cycle:

825.6 grams

823.9 grams

820.2 grams

816.0 grams

808.7 grams

800.7 grams

791.3 grams

783.2 grams

775.8 grams

765.8 grams

DONE

After a couple of the microwaving cycles, the cactus lost its fluffiness and became like light bread dough, not sticking much to the bowl.

'''7:25 pm''' Begin slowly mixing in 25 grams pickling lime. Started with the plastic bowl but switched to a ceramic bowl after a minute, not knowing how the plastic would react to the base. Bowl appears fine after washing it out.

'''7:39 pm''' I'm using a fork to try to get the lime mixed evenly. I figure my Kitchenaid stand mixer will be easier so I break that out.

'''7:45 pm''' Letting the Kitchenaid stir the cactus for me. Much easier!

'''7:53 pm''' Added 25 grams calcium chloride. Before adding, the cactus paste was fluffy and stuck to the sides of the stainless steel bowl. After adding the calcium chloride, the cactus became like clumpy sand and hardly stuck to the sides of the bowl.

'''7:58 pm''' Stopped mixing.

'''8:05 pm''' Transferred cactus to a wide mouth quart mason jar and added 220 ml of ethyl acetate (weighing 199.9 grams). The ethyl acetate came up to approximately 540 ml on the side of the mason jar. After shaking, the cactus looked like fluffy beach sand.

'''8:28 pm''' Shake for a minute.

'''9:00 pm''' Shake for a minute.

'''9:22 pm''' No shaking, I notice the ethyl acetate is light green.

'''10:30 pm''' Shake for a minute. The cactus is starting to get a little stickier, leaving streaks on the glass.

'''11:00 pm''' Ethyl acetate comes up to exactly 500 ml on the side of the mason jar. Versus ~540 ml at 8:05 pm when the ethyl acetate was first added. '''What accounts for this 40 ml difference?'''

'''12:00 am''' Shake for a minute.

'''1:06 am''' Weighed mason jar with cactus: 1001.4 grams.

'''March 10, 2021'''

'''7:57 am''' Weighed mason jar with cactus: 1001.1 grams.

Ready to decant ethyl acetate. Large pyrex beaker with metal coffee filter weighs 342.3 grams. Ethyl acetate is a medium, emerald green. Definitely not light green and not yellow.

Using a small ladle to decant, which gets most of the ethyl acetate with no plant matter. Beaker weighs 427.2 grams meaning we recovered 84.9 grams of ethyl acetate. Not too good.

I transferred the cactus to a french press to see if I could recover more ethyl acetate. The sticky paste does not compress and I recovered an additional ~6 grams ethyl acetate. '''French press is obviously not worth the effort!'''

'''8:21 am''' Done with decanting, transferring, french pressing, weighing, et cetera. Total recovery for this pull is 90.6 grams ethyl acetate.

'''8:23 am''' Added 90.7 grams of fresh ethyl acetate to the mason jar. Stirred ethyl acetate into the sticky cactus, did not shake. Ethyl acetate is already changing to green color.

'''8:33 am''' Photo of pH paper. Paper is dark green. pH 10 or 11? Also tested using the 4 color pH strips. More difficult to judge the pH with these.

'''8:34 am''' Photo of recovered ethyl acetate showing it is an emerald green color.

'''8:45 am''' Poured 10 ml of ethyl acetate into a small beaker. Added 13 mg of citric acid. Lower half of the beaker turned milky, cloudy. Checked pH and it's basically the same as the rest of the solvent. So the small amount of citric acid didn't change the pH much. I used a disposable pipette and pulled from the top of the solvent, so perhaps the top layer didn't have a chance to react yet.

'''8:49 am''' Photo showing cloudy 10 ml in small beaker.

'''8:50 am''' Poured the 10 ml and the rest of the solvent into a mini Pyrex baking dish, using the larger volume of solvent to rinse out of the small beaker. I probably should have left the solvent in a mason jar or beaker rather than adding to the baking dish. Added 95 mg of citric acid. Stirred a little because I wanted to get a more accurate pH. pH was about 7. Added an additional 61 mg citric acid. pH went to about 6. Total citric acid added to the 90.6 grams ethyl acetate is 169 mg. Even after rinsing with the main solvent, the bottom of the small beaker has some spots that look like something crystalizing. I don't know if it's just sticky citric acid or ???

'''9:07 am''' Photo of 3 pH test strips.

'''3:42 pm''' Moving the dish to the freezer. Solvent is clear (and has been clear for at least a few hours). Initially I thought there were droplets on the bottom of the dish (around 11:00 am). Then tried to scrape at them with a knife and not seeing any movement, I figured they were a reflection from the surface because I noticed some tiny droplets on the surface if I caught the light at the right angle. Then as I tipped the dish at 3:42pm to move it into the freezer, I now see the droplets really are at the bottom of the dish. Sort of an oily substance. There are no crystals.

'''8:00 pm''' Retrieving pull #2. Beaker plus metal coffee filter weigh 342.3 grams. Weighs 407.5 grams after decanting. Recovered 65.2 grams. Looks like the cactus sucked up more solvent even though I didn't shake. pH is basic, although the pH paper is not as dark green as pull #1.

'''8:09 pm''' Removed a few tablespoons of sticky slimy cactus and put it into a separate bowl. Mixed in 5.4 grams of calcium chloride (which is a lot relative to the amount of cactus). Even waiting more than 30 minutes, no additional solvent is released. The cactus is drier though, more clumpy, and lost some gooey sliminess.

'''8:27 pm''' Since only 65.2 grams of solvent was retrieved, I decided adding this amount of fresh solvent for pull #3 would be too inefficient. I added 197.6 grams fresh ethyl acetate and stirred for 1-2 minutes. Solvent turned a light green fairly quickly.

'''8:38 pm''' Added 49 mg citric acid to the recovered solvent. Bottom of jar got milky. Tested pH with 3 strips. (1) Took a solvent sample towards the bottom of the jar at the clouds: pH about 5. (2) Solvent sample at the surface: pH about 7. (3) Swirled the jar around then took a solvent sample. pH about 6.

'''8:45 pm''' Put jar into freezer.

CIELO

2021-03-11T07:19:46Z

Shroombee: /* Experiment #1 */

{{ShowInfo|[[Image:Note_error.png]]|'''Note:'''|This page is a workplace for an experimental process. It is intended to summarize information from ongoing discussions in the forum. Feel free to update this page with any observations or comments. Wiki changes are reversible so you can't break anything - be bold. This page is not currently linked to the main wiki and will remain as such until the process is independently verified by others.}}

= Introduction =

'''CIELO''' stands for '''C'''rystals '''I'''n '''E'''thyl-acetate '''L'''eisurely '''O'''TC (Over The Counter).

In this TEK, aqueous cactus paste is broken down with microwave radiation, basified with lime, made clumpy with CaCl2, and extracted with ethyl acetate. The extract is salted with citric acid to precipitate mescaline citrate crystals directly in the solvent.

== Materials ==

* Quart jars with LDPE or PP plastic lids (e.g. below)
* Food scale
* 300g water
* 100g powdered dry cacti
* Microwave
* 25g Ca(OH)2 (lime)
* 25g anhydrous CaCl2
* ~ 1000g ethyl acetate ("MEK substitute")
* pH paper
* Citric acid
* Filter (optional)
* Shallow baking dish
* Scraping tool (e.g. razor blade)

[[File:Plastics.png|center]]

== Safety ==

Review ethyl acetate's safety information<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 check the manufacture's MSDS to verify you have pure ethyl acetate.

Each adult individual needs to find and review any other relevant safety information throughly and make their own personal decision on proceeding.

== Process ==

=== Paste ===

Mix water and cactus powder in a a quart jar. Microwave in short bursts, interrupting the irradiation so the paste does not swell over the rim. This can get to be only a few seconds, so patience is required. Stir frequently and keep track of evaporation with a food scale. Paste color will change from green to tan. Once ~55g of water evaporate microwaving is complete.

Mix in lime until homogeneous and then mix in CaCl2 until paste breaks up into spongy clumps.

With a little practice this step can be done in under an hour, but it does require some elbow grease. See image below from initial green water paste and final clumpy tan paste.

[[File: Screenshot_20210310-053131.png|center]]

=== Pull ===

Add ~ 200g of ethyl acetate to the paste making the jar ~3/4 full and seal with proper lid. Extract for at least 20 minutes regularly shaking every once in a while. Allow to rest and settle for at least 15 minutes and decant to a second jar.

Pull three more times. Progress can be monitored with pH paper (green color indicates free base presence - see middle of image bellow). Paste will change during the pulls and become gunky. When working with a gunky paste, stir, don't shake.

Combined pulls will give ~a quart of clear yellow extract (see image below). Optionally, more pulls can be done into a different jar for a modest yield improvement.

[[File: Screenshot_20210310-060210.png | center]]

=== Salt ===

Drop ~250mg (~1/16 tsp) of citric acid into the extract making it cloudy and let it passively dissolve and react (12 to 48h) in the fridge until clear with crystals on the jar surfaces. Test with pH paper, salting is complete when pH paper is acidic. If needed, add more citric acid in small increments of ~100mg.

Finish crystalization in the freezer to maximize yield.

If there are issues with xtalization, it should still be possible to recover any product present with water pulls followed by evaporation and ethyl acetate washes.

=== Finish ===

Decant ethyl acetate into a storage jar for reuse, using a filter to catch any loose crystals. Rinse crysals with fresh ethyl acetate at least once or until yellow color is removed to personal cosmetic satisfaction. Dissolve crystals in minimal warm water and passively evaporate undisturbed in a shallow baking dish. Finally, scrape up the resulting long crystal needles.

Mass spectrometry (MS) results from solaris analytical<ref>Solaris analytical service[https://www.solarisanalytical.com/]</ref> indicate the product is very clean mescaline after only two ethyl acetate rinses with some minor discoloration remaining. See MS spectrum below, peak near 210.5 is mescaline. Peaks at and 193.6, 178.4, and 162.0 are believed to be mescaline with amine/methyl/methoxy groups cleaved to generate the lower mass mescaline spectrum in multiples of ~16 au (16.9, 32.1, and 48.5 respectively). The small peak at 239.5 is not attributed to mescaline.

[[File: Screenshot_20210310-062431.png|center]]

== Lab Notes ==

The microwave radiation breaks down the plant matter potentially helping free mescaline from the biological matrix. CaCl2 improves the paste texture and helps keep water out of the solvent. CaCl2 can lower the pH by making Ca(OH)2 less soluble, however pH paper indicates paste is still alkaline. Overall, the resulting plant paste seems to give give efficient and clean pulls that are ready to to crash the mescaline salt. Different paste process order, skipping the microwave, using NaCl instead of CaCl2, or using acetone instead of ethyl acetate, could work too, but may have lower yields, produce a less workable paste, or carry unwanted plant matter that interferes with crystalization or ends up in the product.

Allowing 8 hours rest before decanting gives the pull enough time for ethyl acetate, water, and cactus/Ca(OH)2/CaCl2 time to settle and reach liquid-liquid equilibrium.

It is possible to chemically dry the extract with a drying agent such as anhydrous MgSO4. However, no clear yield benefit was observed by performing this step. Surprisingly, solutions carefully dried with anhydrous CaCl2 followed by K2CO3 had difficulty crystalizing after salting, indicating that a some water is desirable for crystalization. This points to the precipitate from this TEK maybe being hydrate salt. Regardless of the reason, the small water content in ethyl acetate directly from the pulls is in a good range experimentally.

During salting, every 10mg of citric acid ('''CitH3''') reacts with enough free base mescaline ('''Mes''') to precipitate up to 43mg of mescaline citrate (or slightly more if a hydrate form is precipitating):

'''<span style="color: Orange"> <div style="text-align: center;">3Mes<sub>(↑)</sub> + CitH3<sub>(↑)</sub> ⇒ 3(MesH)Cit<sub>(↓)</sub></div></span>'''

250mg of citric acid are enough for the typical cactus (up to 1% yield). However, and outlier like the legendary Ogun would need ~1100mg of citric acid for a 4.7% yield.

Over acidifying is not a big concern. There is room for excess citric acid in solution since several grams can dissolve in a quart of ethyl acetate even when chilled. The vast majority of excess acid would be poured off after salting, and any traces removed when washing the crystals.

Other solid organic acids could work. Fumaric acid was tested and gave wispy tiny crystals (not ideal). Malic was tested and slowly crystalized from a dry solution. Tartaric could not crystalize well from dry a dried extract, but began to crystalize with some water added (similar to citric acid). There are many other solid organic acids soluble in ethyl acetate that can be tested (ascorbic, succinic, etc).

It is possible that some of the assumptions and conclusions in these lab notes are incorrect or incomplete. The process was simply tuned for good yields, but the search was not exhaustive<ref>Ethyl acetate approach[https://www.dmt-nexus.me/forum/default.aspx?g=posts&t=96262]</ref>. There could be ways to improve this process.

== References ==
<references/>

== Shroombee's Notes ==

=== Experiment #1 ===

'''March 9, 2021'''

'''6:42 pm'''

100 grams Peruvian Torch chips

298 grams purified water

Blended cactus chips in the Vitamix dry container so it becomes a fine powder.

'''6:58 pm'''
Mixed cactus powder and water in a plastic mixing bowl rather than a mason jar because it seems easier. Product is a fluffy texture, olive green color. There is no excess water.

The bowl plus cactus plus silicone mixing spoon weighs 826.5 grams. Microwave on high for 30 seconds, mix, then weigh. This is pretty easy. I wouldn't want to do this in a mason jar. The cactus does not bubble and there is no issue at 30 seconds with anything bubbling over. Weight after each 30 second cycle:

825.6 grams

823.9 grams

820.2 grams

816.0 grams

808.7 grams

800.7 grams

791.3 grams

783.2 grams

775.8 grams

765.8 grams

DONE

After a couple of the microwaving cycles, the cactus lost its fluffiness and became like light bread dough, not sticking much to the bowl.

'''7:25 pm''' Begin slowly mixing in 25 grams pickling lime. Started with the plastic bowl but switched to a ceramic bowl after a minute, not knowing how the plastic would react to the base. Bowl appears fine after washing it out.

'''7:39 pm''' I'm using a fork to try to get the lime mixed evenly. I figure my Kitchenaid stand mixer will be easier so I break that out.

'''7:45 pm''' Letting the Kitchenaid stir the cactus for me. Much easier!

'''7:53 pm''' Added 25 grams calcium chloride. Before adding, the cactus paste was fluffy and stuck to the sides of the stainless steel bowl. After adding the calcium chloride, the cactus became like clumpy sand and hardly stuck to the sides of the bowl.

'''7:58 pm''' Stopped mixing.

'''8:05 pm''' Transferred cactus to a wide mouth quart mason jar and added 220 ml of ethyl acetate (weighing 199.9 grams). The ethyl acetate came up to approximately 540 ml on the side of the mason jar. After shaking, the cactus looked like fluffy beach sand.

'''8:28 pm''' Shake for a minute.

'''9:00 pm''' Shake for a minute.

'''9:22 pm''' No shaking, I notice the ethyl acetate is light green.

'''10:30 pm''' Shake for a minute. The cactus is starting to get a little stickier, leaving streaks on the glass.

'''11:00 pm''' Ethyl acetate comes up to exactly 500 ml on the side of the mason jar. Versus ~540 ml at 8:05 pm when the ethyl acetate was first added. '''What accounts for this 40 ml difference?'''

'''12:00 am''' Shake for a minute.

'''1:06 am''' Weighed mason jar with cactus: 1001.4 grams.

'''March 10, 2021'''

'''7:57 am''' Weighed mason jar with cactus: 1001.1 grams.

Ready to decant ethyl acetate. Large pyrex beaker with metal coffee filter weighs 342.3 grams. Ethyl acetate is a medium, emerald green. Definitely not light green and not yellow.

Using a small ladle to decant, which gets most of the ethyl acetate with no plant matter. Beaker weighs 427.2 grams meaning we recovered 84.9 grams of ethyl acetate. Not too good.

I transferred the cactus to a french press to see if I could recover more ethyl acetate. The sticky paste does not compress and I recovered an additional ~6 grams ethyl acetate. '''French press is obviously not worth the effort!'''

'''8:21 am''' Done with decanting, transferring, french pressing, weighing, et cetera. Total recovery for this pull is 90.6 grams ethyl acetate.

'''8:23 am''' Added 90.7 grams of fresh ethyl acetate to the mason jar. Stirred ethyl acetate into the sticky cactus, did not shake. Ethyl acetate is already changing to green color.

'''8:33 am''' Photo of pH paper. Paper is dark green. pH 10 or 11? Also tested using the 4 color pH strips. More difficult to judge the pH with these.

'''8:34 am''' Photo of recovered ethyl acetate showing it is an emerald green color.

'''8:45 am''' Poured 10 ml of ethyl acetate into a small beaker. Added 13 mg of citric acid. Lower half of the beaker turned milky, cloudy. Checked pH and it's basically the same as the rest of the solvent. So the small amount of citric acid didn't change the pH much. I used a disposable pipette and pulled from the top of the solvent, so perhaps the top layer didn't have a chance to react yet.

'''8:49 am''' Photo showing cloudy 10 ml in small beaker.

'''8:50 am''' Poured the 10 ml and the rest of the solvent into a mini Pyrex baking dish, using the larger volume of solvent to rinse out of the small beaker. I probably should have left the solvent in a mason jar or beaker rather than adding to the baking dish. Added 95 mg of citric acid. Stirred a little because I wanted to get a more accurate pH. pH was about 7. Added an additional 61 mg citric acid. pH went to about 6. Total citric acid added to the 90.6 grams ethyl acetate is 169 mg. Even after rinsing with the main solvent, the bottom of the small beaker has some spots that look like something crystalizing. I don't know if it's just sticky citric acid or ???

'''9:07 am''' Photo of 3 pH test strips.

'''3:42 pm''' Moving the dish to the freezer. Solvent is clear (and has been clear for at least a few hours). Initially I thought there were droplets on the bottom of the dish (around 11:00 am). Then tried to scrape at them with a knife and not seeing any movement, I figured they were a reflection from the surface because I noticed some tiny droplets on the surface if I caught the light at the right angle. Then as I tipped the dish at 3:42pm to move it into the freezer, I now see the droplets really are at the bottom of the dish. Sort of an oily substance. There are no crystals.

'''8:00 pm''' Retrieving pull #2. Beaker plus metal coffee filter weigh 342.3 grams. Weighs 407.5 grams after decanting. Recovered 65.2 grams. Looks like the cactus sucked up more solvent even though I didn't shake. pH is basic, although the pH paper is not as dark green as pull #1.

'''8:09 pm''' Removed a few tablespoons of sticky slimy cactus and put it into a separate bowl. Mixed in 5.4 grams of calcium chloride (which is a lot relative to the amount of cactus). Even waiting more than 30 minutes, no additional solvent is released. The cactus is drier though, more clumpy, and lost some gooey sliminess.

'''8:27 pm''' Since only 65.2 grams of solvent was retrieved, I decided adding this amount of fresh solvent for pull #3 would be too inefficient. I added 197.6 grams fresh ethyl acetate and stirred for 1-2 minutes. Solvent turned a light green fairly quickly.

'''8:38 pm''' Added 49 mg citric acid to the recovered solvent. Bottom of jar got milky. Tested pH with 3 strips. (1) Took a solvent sample towards the bottom of the jar at the clouds: pH about 5. (2) Solvent sample at the surface: pH about 7. (3) Swirled the jar around then took a solvent sample. pH about 6.

'''8:45 pm''' Put jar into freezer.

CIELO

2021-03-11T06:52:16Z

Shroombee: /* Experiment #1 */

{{ShowInfo|[[Image:Note_error.png]]|'''Note:'''|This page is a workplace for an experimental process. It is intended to summarize information from ongoing discussions in the forum. Feel free to update this page with any observations or comments. Wiki changes are reversible so you can't break anything - be bold. This page is not currently linked to the main wiki and will remain as such until the process is independently verified by others.}}

= Introduction =

'''CIELO''' stands for '''C'''rystals '''I'''n '''E'''thyl-acetate '''L'''eisurely '''O'''TC (Over The Counter).

In this TEK, aqueous cactus paste is broken down with microwave radiation, basified with lime, made clumpy with CaCl2, and extracted with ethyl acetate. The extract is salted with citric acid to precipitate mescaline citrate crystals directly in the solvent.

== Materials ==

* Quart jars with LDPE or PP plastic lids (e.g. below)
* Food scale
* 300g water
* 100g powdered dry cacti
* Microwave
* 25g Ca(OH)2 (lime)
* 25g anhydrous CaCl2
* ~ 1000g ethyl acetate ("MEK substitute")
* pH paper
* Citric acid
* Filter (optional)
* Shallow baking dish
* Scraping tool (e.g. razor blade)

[[File:Plastics.png|center]]

== Safety ==

Review ethyl acetate's safety information<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 check the manufacture's MSDS to verify you have pure ethyl acetate.

Each adult individual needs to find and review any other relevant safety information throughly and make their own personal decision on proceeding.

== Process ==

=== Paste ===

Mix water and cactus powder in a a quart jar. Microwave in short bursts, interrupting the irradiation so the paste does not swell over the rim. This can get to be only a few seconds, so patience is required. Stir frequently and keep track of evaporation with a food scale. Paste color will change from green to tan. Once ~55g of water evaporate microwaving is complete.

Mix in lime until homogeneous and then mix in CaCl2 until paste breaks up into spongy clumps.

With a little practice this step can be done in under an hour, but it does require some elbow grease. See image below from initial green water paste and final clumpy tan paste.

[[File: Screenshot_20210310-053131.png|center]]

=== Pull ===

Add ~ 200g of ethyl acetate to the paste making the jar ~3/4 full and seal with proper lid. Extract for at least 20 minutes regularly shaking every once in a while. Allow to rest and settle for at least 15 minutes and decant to a second jar.

Pull three more times. Progress can be monitored with pH paper (green color indicates free base presence - see middle of image bellow). Paste will change during the pulls and become gunky. When working with a gunky paste, stir, don't shake.

Combined pulls will give ~a quart of clear yellow extract (see image below). Optionally, more pulls can be done into a different jar for a modest yield improvement.

[[File: Screenshot_20210310-060210.png | center]]

=== Salt ===

Drop ~250mg (~1/16 tsp) of citric acid into the extract making it cloudy and let it passively dissolve and react (12 to 48h) in the fridge until clear with crystals on the jar surfaces. Test with pH paper, salting is complete when pH paper is acidic. If needed, add more citric acid in small increments of ~100mg.

Finish crystalization in the freezer to maximize yield.

If there are issues with xtalization, it should still be possible to recover any product present with water pulls followed by evaporation and ethyl acetate washes.

=== Finish ===

Decant ethyl acetate into a storage jar for reuse, using a filter to catch any loose crystals. Rinse crysals with fresh ethyl acetate at least once or until yellow color is removed to personal cosmetic satisfaction. Dissolve crystals in minimal warm water and passively evaporate undisturbed in a shallow baking dish. Finally, scrape up the resulting long crystal needles.

Mass spectrometry (MS) results from solaris analytical<ref>Solaris analytical service[https://www.solarisanalytical.com/]</ref> indicate the product is very clean mescaline after only two ethyl acetate rinses with some minor discoloration remaining. See MS spectrum below, peak near 210.5 is mescaline. Peaks at and 193.6, 178.4, and 162.0 are believed to be mescaline with amine/methyl/methoxy groups cleaved to generate the lower mass mescaline spectrum in multiples of ~16 au (16.9, 32.1, and 48.5 respectively). The small peak at 239.5 is not attributed to mescaline.

[[File: Screenshot_20210310-062431.png|center]]

== Lab Notes ==

The microwave radiation breaks down the plant matter potentially helping free mescaline from the biological matrix. CaCl2 improves the paste texture and helps keep water out of the solvent. CaCl2 can lower the pH by making Ca(OH)2 less soluble, however pH paper indicates paste is still alkaline. Overall, the resulting plant paste seems to give give efficient and clean pulls that are ready to to crash the mescaline salt. Different paste process order, skipping the microwave, using NaCl instead of CaCl2, or using acetone instead of ethyl acetate, could work too, but may have lower yields, produce a less workable paste, or carry unwanted plant matter that interferes with crystalization or ends up in the product.

Allowing 8 hours rest before decanting gives the pull enough time for ethyl acetate, water, and cactus/Ca(OH)2/CaCl2 time to settle and reach liquid-liquid equilibrium.

It is possible to chemically dry the extract with a drying agent such as anhydrous MgSO4. However, no clear yield benefit was observed by performing this step. Surprisingly, solutions carefully dried with anhydrous CaCl2 followed by K2CO3 had difficulty crystalizing after salting, indicating that a some water is desirable for crystalization. This points to the precipitate from this TEK maybe being hydrate salt. Regardless of the reason, the small water content in ethyl acetate directly from the pulls is in a good range experimentally.

During salting, every 10mg of citric acid ('''CitH3''') reacts with enough free base mescaline ('''Mes''') to precipitate up to 43mg of mescaline citrate (or slightly more if a hydrate form is precipitating):

'''<span style="color: Orange"> <div style="text-align: center;">3Mes<sub>(↑)</sub> + CitH3<sub>(↑)</sub> ⇒ 3(MesH)Cit<sub>(↓)</sub></div></span>'''

250mg of citric acid are enough for the typical cactus (up to 1% yield). However, and outlier like the legendary Ogun would need ~1100mg of citric acid for a 4.7% yield.

Over acidifying is not a big concern. There is room for excess citric acid in solution since several grams can dissolve in a quart of ethyl acetate even when chilled. The vast majority of excess acid would be poured off after salting, and any traces removed when washing the crystals.

Other solid organic acids could work. Fumaric acid was tested and gave wispy tiny crystals (not ideal). Malic was tested and slowly crystalized from a dry solution. Tartaric could not crystalize well from dry a dried extract, but began to crystalize with some water added (similar to citric acid). There are many other solid organic acids soluble in ethyl acetate that can be tested (ascorbic, succinic, etc).

It is possible that some of the assumptions and conclusions in these lab notes are incorrect or incomplete. The process was simply tuned for good yields, but the search was not exhaustive<ref>Ethyl acetate approach[https://www.dmt-nexus.me/forum/default.aspx?g=posts&t=96262]</ref>. There could be ways to improve this process.

== References ==
<references/>

== Shroombee's Notes ==

=== Experiment #1 ===

'''March 9, 2021'''

'''6:42 pm'''

100 grams Peruvian Torch chips

298 grams purified water

Blended cactus chips in the Vitamix dry container so it becomes a fine powder.

'''6:58 pm'''
Mixed cactus powder and water in a plastic mixing bowl rather than a mason jar because it seems easier. Product is a fluffy texture, olive green color. There is no excess water.

The bowl plus cactus plus silicone mixing spoon weighs 826.5 grams. Microwave on high for 30 seconds, mix, then weigh. This is pretty easy. I wouldn't want to do this in a mason jar. The cactus does not bubble and there is no issue at 30 seconds with anything bubbling over. Weight after each 30 second cycle:

825.6 grams

823.9 grams

820.2 grams

816.0 grams

808.7 grams

800.7 grams

791.3 grams

783.2 grams

775.8 grams

765.8 grams

DONE

After a couple of the microwaving cycles, the cactus lost its fluffiness and became like light bread dough, not sticking much to the bowl.

'''7:25 pm''' Begin slowly mixing in 25 grams pickling lime. Started with the plastic bowl but switched to a ceramic bowl after a minute, not knowing how the plastic would react to the base. Bowl appears fine after washing it out.

'''7:39 pm''' I'm using a fork to try to get the lime mixed evenly. I figure my Kitchenaid stand mixer will be easier so I break that out.

'''7:45 pm''' Letting the Kitchenaid stir the cactus for me. Much easier!

'''7:53 pm''' Added 25 grams calcium chloride. Before adding, the cactus paste was fluffy and stuck to the sides of the stainless steel bowl. After adding the calcium chloride, the cactus became like clumpy sand and hardly stuck to the sides of the bowl.

'''7:58 pm''' Stopped mixing.

'''8:05 pm''' Transferred cactus to a wide mouth quart mason jar and added 220 ml of ethyl acetate (weighing 199.9 grams). The ethyl acetate came up to approximately 540 ml on the side of the mason jar. After shaking, the cactus looked like fluffy beach sand.

'''8:28 pm''' Shake for a minute.

'''9:00 pm''' Shake for a minute.

'''9:22 pm''' No shaking, I notice the ethyl acetate is light green.

'''10:30 pm''' Shake for a minute. The cactus is starting to get a little stickier, leaving streaks on the glass.

'''11:00 pm''' Ethyl acetate comes up to exactly 500 ml on the side of the mason jar. Versus ~540 ml at 8:05 pm when the ethyl acetate was first added. '''What accounts for this 40 ml difference?'''

'''12:00 am''' Shake for a minute.

'''1:06 am''' Weighed mason jar with cactus: 1001.4 grams.

'''March 10, 2021'''

'''7:57 am''' Weighed mason jar with cactus: 1001.1 grams.

Ready to decant ethyl acetate. Large pyrex beaker with metal coffee filter weighs 342.3 grams. Ethyl acetate is a medium, emerald green. Definitely not light green and not yellow.

Using a small ladle to decant, which gets most of the ethyl acetate with no plant matter. Beaker weighs 427.2 grams meaning we recovered 84.9 grams of ethyl acetate. Not too good.

I transferred the cactus to a french press to see if I could recover more ethyl acetate. The sticky paste does not compress and I recovered an additional ~6 grams ethyl acetate. '''French press is obviously not worth the effort!'''

'''8:21 am''' Done with decanting, transferring, french pressing, weighing, et cetera. Total recovery for this pull is 90.6 grams ethyl acetate.

'''8:23 am''' Added 90.7 grams of fresh ethyl acetate to the mason jar. Stirred ethyl acetate into the sticky cactus, did not shake. Ethyl acetate is already changing to green color.

'''8:33 am''' Photo of pH paper. Paper is dark green. pH 10 or 11? Also tested using the 4 color pH strips. More difficult to judge the pH with these.

'''8:34 am''' Photo of recovered ethyl acetate showing it is an emerald green color.

'''8:45 am''' Poured 10 ml of ethyl acetate into a small beaker. Added 13 mg of citric acid. Lower half of the beaker turned milky, cloudy. Checked pH and it's basically the same as the rest of the solvent. So the small amount of citric acid didn't change the pH much. I used a disposable pipette and pulled from the top of the solvent, so perhaps the top layer didn't have a chance to react yet.

'''8:49 am''' Photo showing cloudy 10 ml in small beaker.

'''8:50 am''' Poured the 10 ml and the rest of the solvent into a mini Pyrex baking dish, using the larger volume of solvent to rinse out of the small beaker. I probably should have left the solvent in a mason jar or beaker rather than adding to the baking dish. Added 95 mg of citric acid. Stirred a little because I wanted to get a more accurate pH. pH was about 7. Added an additional 61 mg citric acid. pH went to about 6. Total citric acid added to the 90.6 grams ethyl acetate is 169 mg. Even after rinsing with the main solvent, the bottom of the small beaker has some spots that look like something crystalizing. I don't know if it's just sticky citric acid or ???

'''9:07 am''' Photo of 3 pH test strips.

'''3:42 pm''' Moving the dish to the freezer. Solvent is clear (and has been clear for at least a few hours). Initially I thought there were droplets on the bottom of the dish (around 11:00 am). Then tried to scrape at them with a knife and not seeing any movement, I figured they were a reflection from the surface because I noticed some tiny droplets on the surface if I caught the light at the right angle. Then as I tipped the dish at 3:42pm to move it into the freezer, I now see the droplets really are at the bottom of the dish. Sort of an oily substance. There are no crystals.

'''8:00 pm''' Retrieving pull #2. Beaker plus metal coffee filter weigh 342.3 grams. Weighs 407.5 grams after decanting. Recovered 65.2 grams. Looks like the cactus sucked up more solvent even though I didn't shake. pH is basic, although not as dark green as pull #1.

'''8:09 pm''' Removed a few tablespoons of sticky slimy cactus and put it into a separate bowl. Mixed in 5.4 grams of calcium chloride (which is a lot relative to the amount of cactus). Even waiting more than 30 minutes, no additional solvent is released. The cactus is drier though, more clumpy, and lost some gooey sliminess.

'''8:27 pm''' Since only 65.2 grams of solvent was retrieved, I decided adding this amount of fresh solvent for pull #3 would be too inefficient. I added 197.6 grams fresh ethyl acetate and stirred for 1-2 minutes. Solvent turned a light green fairly quickly.

'''8:38 pm''' Added 49 mg citric acid to the recovered solvent. Bottom of jar got milky. Tested pH with 3 strips. (1) Took a solvent sample towards the bottom of the jar at the clouds: pH about 5. (2) Solvent sample at the surface: pH about 7. (3) Swirled the jar around then took a solvent sample. pH about 6.

'''8:45 pm''' Put jar into freezer.

CIELO

2021-03-10T23:48:25Z

Shroombee: /* Experiment #1 */

CIELO

2021-03-10T18:35:48Z

Shroombee: /* Experiment #1, March 9, 2021 */

CIELO

2021-03-10T06:37:38Z

Shroombee: /* Experiment #1, March 9, 2021 */

CIELO

2021-03-10T06:36:27Z

Shroombee: /* Experiment #1, March 9, 2021 */

CIELO

2021-03-10T06:31:44Z

Shroombee: /* Shroombee's Notes */

CIELO

2021-03-10T06:26:15Z

Shroombee: /* Shroombee's Notes */

CIELO

2021-03-10T06:16:36Z

Shroombee: /* Shroombee's Notes */

CIELO

2021-03-10T06:06:32Z

Shroombee: