Difference between revisions of "Chilled Acetone with IPA and Naphtha"
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| − | Longer pull times or higher temperatures result in (1) | + | Longer pull times or higher temperatures result in more (1) off colors, (2) difficult crystalization, (3) absorbed solvent, and (4) tendency for paste to congeal. These negatives come with no yield improvement. |
Revision as of 03:10, 9 June 2021
Contents
Introduction 🙏
CIELO stands for Crystals In Ethyl-acetate Leisurely Over-the-counter.
In this technique (TEK), cold alkaline cactus paste (Fig. 2) is extracted with chilled ethyl acetate (Fig. 3). Mescaline citrate is precipitated with citric acid (Fig. 4-5) and collected (Fig. 6).
Thanks to everyone who contributed: someblackguy, Benzyme, shroombee, Metta-Morpheus, Downwardsfromzero, Kash, grollum, Mindlusion, Doubledog, Dreamer042, Loveall, and others.
Materials 🛒
- French press (or similar ensemble)
- 300g ice cold water
- 25g lime
- 100g dry cactus powder
- Quart freezer chilled (~0F) ethyl acetate
- Coffee filter, support basket, and funnel
- Quart jar
- 5g of citric acid
- 4oz of room temperature ethyl acetate
- Washing soda (for solvent reclaim)
Process 📜
Paste 🌵
Mix ice cold water, lime, and cactus in french press for a few minutes to a smooth paste (Fig. 2).
Extract 👨🏾🔬
Cover cold paste with chilled ethyl acetate (~0F), mix for for 20 seconds, squeeze with french press, mix for 20 seconds, squeeze again, and mix for 20 more seconds. Filter into quart jar. Repeat until jar is full (~5x).
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, forming clouds (Fig. 4). After a few hours mescaline citrate crystals form (Fig. 5). Allow crystalization to complete undisturbed (~12 hours).
Collect 💖
Catch crystals in a coffee filter. Rinse jar/filter with room temperature ethyl acetate a couple times and dry (Fig. 6).
If some crystals stubbornly remain on the jar walls, dissolve them in hot water, dry in a shallow dish, and scrape.
Yield depends on the cactus and is usually between 0.2% to 2% with ~1% being most common[1].
Mass spectrometry (MS) results from solaris analytical[2] indicate the product is very clean mescaline (Fig. 7).
Reclaim Solvent 💚
Reusing solvents is encouraged[3] at the DMT nexus.
Wash spent extract with sodium carbonate saturated water shaking vigorously (emulsions do not form). Citric acid removal is complete when CO2 bubbling stops. Remove water layer. Freeze and filter out ice crystals. Store for reuse.
Appendix: Development Notes 🔬
Paste 🌵
No improvements were seen with longer basing time, microwaving, partially or completely drying (heat or drying agent), or increasing the ionic strength.
Extract 👨🏾🔬
Longer pull times or higher temperatures result in more (1) off colors, (2) difficult crystalization, (3) absorbed solvent, and (4) tendency for paste to congeal. These negatives come with no yield improvement.
Chemically drying the extract before salting had no crystallization or yield benefit.
Droplets or debris not decanted/filtered before adding citric acid will result in crystalization issues. It is very important to verify the extract is clean.
Crystalize ✨
During crystallization, 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):
The TEK calls for more citric acid than would be needed for titration because 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 recommends ~5mg/g but 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 [4]).
Several factors can make crystals smaller: Reusing ethyl acetate, warmer pulls, longer pulls, higher citric acid concentration, and mechanical agitation. Very small needles 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 over a filter gave better results than decanting washes from a jar. The filter paper wicked away the off colors forming a ring. More than two washes do not seem necessary. Unlike the pulls, warmer ethyl acetate is an advantage because the goal is to dissolve away plant matter.
The jar wash should be done immediately. If any straggler crystals dry they can become stuck to the jar walls.
