Chilled Acetone with IPA and Naphtha

CIELO

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 in this collaborative effort: someblackguy, Benzyme, shroombee, Metta-Morpheus, Downwardsfromzero, Kash, grollum, Mindlusion, Doubledog, Dreamer042, Loveall, and others.

Materials 🛒

• Mescaline Extraction:
  • French press
  • 300g ice cold water
  • 25g lime
  • 100g dry cactus powder
  • Quart of freezer chilled (~0F) ethyl acetate
  • Coffee filter, support basket, and funnel
  • Large jar (~64 oz)
  • 5g of citric acid if using outer cactus skin or 20g if using whole cactus
  • ~4oz of room temperature ethyl acetate

• Solvent Reclaim:
  • Washing soda saturated water
  • Separatory funnel or glass turkey baster

Fig. 1: Materials used (french press option shown).

Process 📜

Make Alkaline Paste 🌵

Mix ice cold water and lime in a french press. Stir in cactus powder for a few minutes to a smooth paste (Fig. 2).

Fig. 2: Alkaline cactus paste.

Pull Alkaline Paste 👩‍🔬

Cover paste with freezer chilled ethyl acetate (~0 F), mix thoroughly for for 60 seconds, and filter to a large jar (~64 oz). Pull 5 more times stirring thoroughly for 60 seconds each time.

Inspect extract for droplets or particles. If present, decant/filter to remove them. Extract needs to be clean (see Fig. 3).

Fig. 3: Ethyl acetate extract.

Crystalize Extract 🧪

Drop (do not stir) citric acid into extract forming clouds (Fig. 4) which crash as mescaline citrate crystals after a few hours (Fig. 5). Allow crystalization to complete (~12 hours).

Fig 5.: Mescaline citrate crystals precipitating in the extract (side view of baking dish).

Collect Crystals ✨

Swirl and filter crystalized extract to catch crystals in a coffee filter. Rinse jar with a small amount of fresh ethyl acetate twice to remove off color and catch any remaining crystals in the filter. Dry crystals to the final product (Fig. 6). Note: if any crystals stubbornly remain on the jar walls, dissolve them in hot water, dry in a shallow dish, and scrape.

Yield is dependent on cactus material and usually between 0.2% to 2% with ~1% being common.

Fig. 6: Collected mescaline citrate crystals.

Mass spectrometry (MS) results from solaris analytical indicate the product is very clean mescaline (Fig. 7).

Fig. 7: 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.

Reclaim Solvent 💚

Reusing solvents is encouraged at the DMT nexus.

Wash spent extract with sodium carbonate saturated water shaking vigorously (emulsions do not form). Citric acid removal is complete when 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 of completely drying (with heat or drying agent), or adding NaCl to increase the ionic strength.

Pull 👨🏾‍🔬

It is also possible to obtain good results with 3 minute room temperature pulls (30s of stirring and 150s of rest), but the results may not be as consistent compared to chilled ethyl acetate (60s of stirring). This is thought to be because of increased plant contaminants in the warmer pull at room temperature making crystallization more difficult.

Long room temperature pulls made the paste congeal and resulted in lower yield. Heating during the pull did not improve yields. Generally, longer times or higher temperatures make the crystalization more difficult without yield improvements and a persistent tan color can contaminate the product.

Extract 🧪

Chemically drying the extract with a drying agent such as anhydrous MgSO4 before salting had no yield benefit. In one example, drying the extract with CaCl2 resulted in a more difficult crystalization and a 40% yield loss. In general, any water content in ethyl acetate directly from the pulls is already in a good range experimentally.

Droplets or debris not decanted/filtered before adding citric acid can result in crystalization issues. It is very important to verify the extract is clean as mentioned in the main TEK.

Crystalization ✨

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):

3Mes_(↑) + H3Cit_(↑) ⇒ 3(MesH)Cit_(↓)

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 ).

Mescaline citrate grows as needles in ethyl acetate (Fig. 4) that can be up to several mm long. Reused ethyl acetate, warmer pulls, longer pulls, higher citric acid concentration, agitation, and colder temperatures tend to make the needles smaller. Very small needles can look like a powder. Potency does not seem affected by the crystallization appearance, and a powdery precipitate is not an problem unless it becomes difficult to decant/filter.

After the main TEK's room temperature 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 only ice crystals.

Other dry organic acids could work. Fumaric, Malic, Tartaric, Ascorbic, Succinic, etc can be tested in future investigations.

Disclaimer 🤷‍♂️

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. There could be ways to improve this process.