Difference between revisions of "Chilled Acetone with IPA and Naphtha"
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*Washing soda (for solvent reclaim) | *Washing soda (for solvent reclaim) | ||
Revision as of 17:02, 17 June 2021
Contents
Introduction 🙏
CIELO stands for Crystals In Ethyl-acetate Leisurely Over-the-counter.
In this technique (TEK), cactus alkaline paste (Fig. 2) is extracted with chilled ethyl acetate (Fig. 3). Mescaline citrate is precipitated with citric acid (Fig. 4) and collected (Fig. 5).
Thanks to everyone who contributed to this process: someblackguy, Benzyme, shroombee, Metta-Morpheus, Downwardsfromzero, Kash, grollum, Mindlusion, Doubledog, Dreamer042, Loveall, and others.
Safety ⛑️
Review ethyl acetate[1], lie[2], and citric acid[3] 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 🛒
- French press (or similar ensemble)
- 200g water
- 20g of lie
- 100g dry cactus powder (outer skin or whole plant)†
- 100g of anhydrous CaCl2 (sold as ice melt)
- 1qt ethyl acetate (also sold as "MEK substitute")
- Coffee filters, support basket, and funnel
- Quart jar
- 1/2 tsp Citric acid
- Washing soda (for solvent reclaim)
†Note: If starting with fresh cacti, store the dark for 3 months, slice, dry in oven at lowest heat setting, and grind to a fine powder (keeping spines is ok)[4].
Process 📜
Paste 🌵
Mix water, cactus powder, and lie for at least 10 minutes to a coagulated paste and rest overnight. Add CaCl2 and blend well to a fine moist powder. Leave in freezer overnight (~0F).
Extract 👨🏾🔬
Cover cold paste with freezer chilled ethyl acetate (~0F), mix for 60s, and filter into quart jar. Repeat until quart jar is full (~4x).
Inspect extract for droplets or particles. If present, remove them. Extract needs to be clean (see Fig. 3).
Crystalize ✨
Drop (do not stir) citric acid into extract. Clouds form quickly, slowly followed by mescaline citrate crystals (Fig. 4). Allow crystalization to complete undisturbed (~12 hours).
Note: If using whole cactus more citric acid may be needed to induce crystallization (up to 1 Tbsp).
Collect 💖
Swirl crystalized extract to knock off crystals from walls and dissolve any remaining citric acid granules. Catch floating crystals in a coffee filter. Repeat with a small amount (~1oz) of fresh room temperature ethyl acetate until all crystals are in the filter and off color is washed (~2-3x). Dry and collect from filter (Fig. 5).
Yield depends on the cactus and is usually between 0.2% to 2% with ~1% being common[5].
Mass spectrometry (MS) results from solaris analytical[6] indicate the product is very clean mescaline (Fig. 6).
Reclaim Solvent 💚
Reusing solvents is encouraged[7] at the DMT nexus.
Wash spent extract with sodium carbonate saturated water shaking vigorously (emulsions do not form). Filter any excess calcium carbonate and remove water layer. Freeze and filter out ice crystals. Optionally, remove color over activated carbon over several days an filter. Store for reuse.
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).
Microwaving the lime paste could be a shortcut to break down plant material and a possible alternative for whole cactus. This is currently and open question.
The lie paste is converted to a lime paste with NaCl when CaCl2 is added because the following reaction goes to the right as excess lime precipitates:
It is important to add enough CaCl2 to react with NaOH and reduce the pH, minimizing any ethyl acetate breakdown.
Extract 👨🏾🔬
Longer/warmer pulls resulted in darker extract, smaller crystals, solvent paste absorption, congealing of paste, and no yield benefit.
Chemically drying the extract had no benefits.
An additional long room temperature pull on the TEK's spent paste only yielded 4mg of very small crystals, indicating the chilled pulls are efficient.
Crystalize ✨
During crystallization, every 233mg of citric acid (H3Cit) react with free base mescaline (Mes) to form to 1g of mescaline citrate (or slightly more if a hydrate is precipitating):
Excess citric acid shifts the precipitation reaction to the right (Le Chatelier's principle), helping overcome water and plant material. There is a lot room for excess citric acid in solution since its solubility is 50mg/g in ethyl acetate. The TEK guidelines range from 1.5mg/ml to 20mg/ml, but since cacti and pull techniques can vary, users may find other values work better for their specific situation (in one specific example with whole cactus powder 20mg/g was used [8]).
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. Fumaric, Malic, Tartaric, Ascorbic, Succinic, etc can be tested in future investigations.
Collect 💖
Washing crystals in a filter appears to wick away plant colors and superior to decanting. Unlike the pulls, warmer ethyl acetate is preferred to wash off plant matter.
The quart jar wash should be done immediately. If any straggler crystals dry in the jar they may stick to the wall. To recover from such a situation, dissolve stuck crystals in hot water, dry in a shallow dish, and scrape.