Revision as of 18:32, 4 March 2021

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.

Introduction

CIELO

CIELO stands for Crystals In Ethyl-acetate Leisurely OTC (Over The Counter).

In this TEK, aqueous lime cactus paste is broken down by microwave radiation, saturated with NaCl, and extracted with ethyl acetate. The extract is chemically dried and salted with citric acid to precipitate mescaline citrate crystals. The materials needed are available over the counter in several countries.

Processing the paste in the microwave to make it ready for extraction is the most laborious part of this TEK. There is also a MgSO4 chemichal dry that may need some practice to perform cleanly to avid fine particles persisting in the extract.

Materials

• Quart jars with lids*
• Food scale
• 25g + 25g lime (Ca(OH)2)
• 300g water
• 100g powdered dry cacti
• Microwave
• 80g plain table salt (NaCl)
• ~ 1000g Ethyl acetate (sometimes labeled "MEK substitute")
• 10g anhydrous Na2CO3
• pH paper (optional)
• Shallow glass baking dish with lid*
• Citric acid

*If lids are plastic, use ethyl acetate resistant LDPE or PP.

Safety

Review ethyl acetate's safety information^[1] and check the manufacture's MSDS to verify you have pure ethyl acetate.

Do not microwave a sealed container. There must be a ventilation path for water vapor to avoid pressure buildup and subsequent cracked jar or explosion.

Microwaving lime cacti paste produces smelly fumes that will be noticed by the people in your surroundings. Lime is a skin irritant and hot lime will be more severe, avoid skin contact.

These are only good-faith suggestions. They do not guarantee safety. Each adult individual needs to review external information throughly and make their personal decision on proceeding.

Process

Paste

Add first 25g of lime to water followed by cactus powder while stirring to form a homogeneous paste. Stir long enough give time for the lime to change the texture if the paste and make it smooth.

Microwave between 300W and 500W in bursts of 5 minutes or less monitoring closely (paste will swell and can escape the jar if not stopped). Loosely cover with a plastic lid initially to partially trap steam until paste liquefies. Continue microwaving without a lid until a total of 100g of water evaporate to give a denser paste (total microwave time is ~40 minutes).

Mix in NaCl (the paste will become runny). Finally, mix in second 25g of lime to stiffen up the paste.

Note:

Could using CaCl2 instead of NaCl be better?? OTC as a de-icer, the anhydrous form would absorb water. Also, the LLE for water/ethyl acetate/CaCl2 could be cleaner than water/ehtyl acetate/NaCl (less water in the solvent and less solvent in the water), but have only found published data for water/ehtyl acetate/NaCl has been found.

The ideal final paste is stiff but not hard to stir. If needed, adjust consistency by adding a little water (runnier) or lime (stiffer).

Pull

Add ~ 300g of ethyl acetate to the paste making the jar ~3/4 full. Stir slowly and thoroughly. Cover with lid and let it sit for a few hours or more**.

Decant solvent into a second jar. About ~100g of solvent will remain in the paste.

Pull three more times with ~200g of ethyl acetate, making the jar ~3/4 full again. Unlike the first pull, all the added solvent can be recovered. The paste may become sandy in later pulls.

Combined pulls will give about ~800g (~a quart) of clear yellow extract. Optionally, more pulls can be done later for a modest yield improvement.

**If solvent separation is poor the starting paste was too wet. Adding lime releases cloudy solvent that clears up over time. Conversely, if paste in hard to mix with the solvent, the paste was too dry (simply add water).

Dry

Dry extract with anhydrous MgSO4 (~2g per 100g of extract) by swirling and settling^[2]. Decant clear solution to shallow glass baking dish.

If settling time is very long or decanting is difficult, using more coarse MgSO4 and/or filtering with a fine filter may be helpful.

Note:

Could using CaCl2 be better/easier? Have also tested Na2CO3 and Na2SO4, so far MgSO4 gives the fastest xtalization in the next step. An extra dry could be tried with K2CO3 also. A good chemichal drying does help with xtalization. However, without drying xtalization can be done in the freezer - perhaps we can simply do that and skip this?

Salt

Gently drop ~250mg (~1/16 tsp) of citric acid into the extract without stirring***. Clouds form as the citric acid diffuses into solution and reacts with free base mescaline. After a few hours at room temperature the clouds settle as beautiful mescaline citrate xtals. If xtals have difficulty forming, move dish to freezer to try to recover the product (this indicates an issue with the process such as incomplete chemichal drying).

Every 10mg of citric acid (CitH₃) reacts with enough free base mescaline (Mes) to precipitate up to 43mg of mescaline citrate:

Salting is complete if no clouds form after adding more citric acid (e.g. ~ 50mg), or optionally if pH paper is neutral/acidic. A few hundred mg of citric acid should be more than enough for the typical cactus (0.5% to 0.8% yield). The legendary Ogun would need 1000mg of citric acid for 4.3% yield.

Over acidifying is not a big concern. There is room for a lot of excess citric acid in solution since several grams can dissolve in a quart of ethyl acetate.

***Stirring won't cause any major issues but xtals will be smaller.

Note:

The micriwave to break down plant matter and a good chemmical dry both sem to help get good quality xtalization at room temp. However, even when those steps are not done (or not done well), xtalization can be forced in the freezer usually. Perhaps this could even enable skipping the microwave step and/or the drying step someday - especially if CaCl2 gives a drier solution while pulling (compared to NaCl).

Note:

Other organic acids could work. Perhaps an anhydrous one could be better (citric acid is monohydrate)? Tested fumaric and got wispy xtals (not ideal). Malic would be interesting (natural salt?). There are many other solid organic salts soluble in ethyl acetate.

Finish

Pour off ethyl acetate into a storage container**** using a coffee filter to help pick up any loose xtals. Optionally, rinse xtals with anhydrous ethyl acetate until yellow color is removed to personal cosmetic satisfaction. Leave xtals uncovered to evaporate all residual solvent, this is the final product.

Mass spectrometry results indicate the product is very clean mescaline (see image below for a sample after two completely white after two rinses that was not completely white yet). Yields are highly dependent on starting cacti powder and can vary from 0.1% to 5% (0.5% to 1% being common).

****Solvent can be washed with brine and reused.

References

1. ↑ Ethyl acetate safety[1]
2. ↑ Solvent drying tips[2]