Difference between revisions of "Chilled Acetone with IPA and Naphtha"

From DMT-Nexus Wiki
Jump to: navigation, search
(β†’β€ŽMaterials πŸ›’)
(β†’β€ŽPaste 🌡)
Line 39: Line 39:
  
 
== Paste 🌡 ==
 
== Paste 🌡 ==
βˆ’
There are two options to make the alkaline paste using lime or lie. The lime paste is fast and convenient. The lie paste takes longer to make, but breaks down more plant matter<ref>Saponification[https://en.m.wikipedia.org/wiki/Saponification]</ref> making it robust to cactus variability (recommended for whole cacti).
+
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 fridge overnight to cool.
βˆ’
 
+
βˆ’
 
+
βˆ’
*'''Lime paste''': Mix ice cold water, lime, and cactus in french press for at least 10 minutes to a smooth cold paste (Fig. 2).
+
βˆ’
 
+
βˆ’
 
+
βˆ’
*'''Lie paste''': Mix water, cactus paste, and lie for at least 10 minutes to a coagulated paste. Rest overnight to react and saponify. Add CaCl2, starting with 40g (anhydrous) and up to 80g (hexahydrate) to a uniform sandy paste. Leave in fridge overnight to cool.
+
 
   
 
   
  

Revision as of 15:38, 17 June 2021

CIELO

Introduction πŸ™

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 πŸ›’

  • French press (or similar ensemble)
  • 200g water
  • 20g of lime
  • 100g dry cactus powder (outer skin or whole plant)†
  • 100g of anhydrous CaCl2
  • 1qt ethyl acetate (also sold as "MEK substitute")
  • Coffee filters, support basket, and funnel
  • Quart jar
  • 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].


IMG 20210608 223040865 copy 800x600.jpg
Fig. 1: Over the counter materials (french press and lime options).

Process πŸ“œ

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 fridge overnight to cool.


IMG 20210603 183405358 copy 800x600.jpg
Fig. 2: Cactus alkaline paste.

Extract πŸ‘¨πŸΎβ€πŸ”¬

Cover cold paste with freezer chilled ethyl acetate (~0F), mix for 60s, and filter into quart jar. Repeat until quart jar is full (~5 total pulls).


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


IMG 20210601 122315740 copy 600x800.jpg
Fig. 3: Ethyl acetate extract.

Crystalize ✨

Extracts with more plant material need more citric acid. Experimental guidelines:


  • Outer skin lie paste: 1/4 tsp
  • Outer skin lime paste: 1/2 tsp
  • Whole cactus lie paste: 1 tsp
  • Whole cactus lime paste: 1 Tbsp (product can be sticky).


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).


IMG 20210609 064813073 copy 800x600 1.jpg
Fig. 4: Crystals in ethyl acetate (macro lens image).

Collect πŸ’–

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].


IMG 20210603 130102387 copy 600x800 copy 800x600.jpg
Fig. 5: Final mescaline citrate crystals.


Mass spectrometry (MS) results from solaris analytical[6] indicate the product is very clean mescaline (Fig. 6).


Cactus-extract copy 800x600 1.jpg
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.

Reclaim Solvent πŸ’š

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 πŸ”¬

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:


NaOH + CaCl2β‡’ Ca(OH)2 + 2NaCl


It is important to add enough CaCl2 to react with NaOH and reduce the pH, minimizing any ethyl acetate breakdown.

Extract πŸ‘¨πŸΎβ€πŸ”¬

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):


3Mes(↑) + H3Cit(↑) β‡’ 3(MesH)Cit(↓)


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 πŸ’–

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.

References πŸ—οΈ

  1. ↑ Ethyl acetate safety[1]
  2. ↑ Lie safety[2]
  3. ↑ Citric acid safety[3]
  4. ↑ Fresh cacti process[4]
  5. ↑ Cactus analysis thread[5]
  6. ↑ Solaris analytical service[6]
  7. ↑ On reusing non polar solvent[7]
  8. ↑ Ethyl acetate approach[8]