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

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(4 Salt)
(2 Pull)
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Add ~ 400g of ethyl acetate (fill the jar about 3/4 full). Extract for a few hours shaking vigorously every once in a while*. Decant solvent into second jar. About ~ 150g of solvent will remain in the paste (the pulls are still very efficient despite this). Pull two more times with ~250g ethyl acetate (simply aim to fill the jar to ~3/4 like before). Combined pulls will give about ~750g (~0.9 quarts) of a clear yellow extract. Optionally, more pulls can be done for modest yield improvements.
 
Add ~ 400g of ethyl acetate (fill the jar about 3/4 full). Extract for a few hours shaking vigorously every once in a while*. Decant solvent into second jar. About ~ 150g of solvent will remain in the paste (the pulls are still very efficient despite this). Pull two more times with ~250g ethyl acetate (simply aim to fill the jar to ~3/4 like before). Combined pulls will give about ~750g (~0.9 quarts) of a clear yellow extract. Optionally, more pulls can be done for modest yield improvements.
  
'''*Troubleshooting:'''
+
 
 +
""'''*Troubleshooting:'''
  
 
It is important to get the paste consistentcy right. If it is too watery, ethyl acetate will be completely absorbed by the paste and not separate. If it is too dry, it will be hard to mix and the pull won't be as efficient. Plant material is variable and practice helps gets the proper paste consistency. Fortunately, it is possible to make adjustments:
 
It is important to get the paste consistentcy right. If it is too watery, ethyl acetate will be completely absorbed by the paste and not separate. If it is too dry, it will be hard to mix and the pull won't be as efficient. Plant material is variable and practice helps gets the proper paste consistency. Fortunately, it is possible to make adjustments:
Line 59: Line 60:
 
'''- Too watery:''' Adding lime will break up the blob and cloudy release solvent. The cloudiness clears up over time.
 
'''- Too watery:''' Adding lime will break up the blob and cloudy release solvent. The cloudiness clears up over time.
  
'''- Too dry:''' Simply add water a few ml at a time until paste is easy to mix. Sometimes this is needed in the later pulls.
+
'''- Too dry:''' Simply add water a few ml at a time until paste is easy to mix. Sometimes this is needed in the later pulls.""
  
 
=== 3 Dry ===  
 
=== 3 Dry ===  

Revision as of 19:44, 25 February 2021

Blind placeholder for CIELO (Chrystals In Ethyl-acetate Leisurely OTC). Information has not been verified.

Introduction

In the CIELO approach, Crystals are formed directly In Ethyl-acetate Leisurely using OTC (over the counter) materials.


The process is simple: aqueous cactus matter is broken down with microwave radiation, saturated with NaCl, made alkaline, and extracted with ethyl acetate. The extract is dried over MgSO4 and salted with citric acid to precipitate mescaline citrate.

Materials

- Three quart jars with leak-proof ethyl-acetate resistant lids

- Food scale to measure weights

- 100g powdered dry cacti

- 80g Ca(OH)2 (lime)

- 300g water

- Microwave

- 80g NaCl (plain table salt)

- 1L ethyl acetate (sometimes labeled "MEK substitute")

- pH paper strips

- 20g MgSO4 (oven dehydrated epson salt)

- Coffee filters

- 300mg of Citric acid (~1/16 of a tsp)

- Xtal scraping tool (e.g. razor blade)

Safety

Ethyl acetate is a natural product in small amounts in some foods and fermented beverages. It is volatile and the smell can be strong. Fume accumulation can be a concern, so work in a well ventilated area and keep lids on as much as possible. The fumes smell sweet and usually dissipate quickly. Read the safety information here, and check your manufacture's MSDS to verify you have ethyl acetate without additives such as methanol. Test all plastic you are planning to use with ethyl acetate and make sure it does not degrade. NEVER pour ethyl acetate down the drain. Not only is solvent in the water an environmental issue, but ethyl acetate can damage PVC pipes. Do not have an open flame anywhere near ethyl acetate. After searching for and reviewing the safety information it is up to you to make an adult personal decision on using ethyl acetate.


These are only good-faith safety tips. They do not guarantee safety. Each adult individual needs to make their personal decisions on how/if to use over the counter chemicals.

Process

1 Paste

Slowly add cactus powder to water while stirring to form a homogeneous paste. Microwave at medium power (~500W) in short 2-5 minute bursts monitoring closely to not boil over and stirring between irradiations. Initial paste will liquefy as the plant matter breaks down and then become a paste again after ~100g of water evaporates. Mix in NaCl (paste will become more runny) and cool. Finally, add Ca(OH)2 to thicken the paste and convert mescaline from salt to free base. The ideal paste is both stiff and easy to stir. If needed, adjust consistency by adding more brine (runnier) or lime (stiffer).

2 Pull

Add ~ 400g of ethyl acetate (fill the jar about 3/4 full). Extract for a few hours shaking vigorously every once in a while*. Decant solvent into second jar. About ~ 150g of solvent will remain in the paste (the pulls are still very efficient despite this). Pull two more times with ~250g ethyl acetate (simply aim to fill the jar to ~3/4 like before). Combined pulls will give about ~750g (~0.9 quarts) of a clear yellow extract. Optionally, more pulls can be done for modest yield improvements.


""*Troubleshooting:

It is important to get the paste consistentcy right. If it is too watery, ethyl acetate will be completely absorbed by the paste and not separate. If it is too dry, it will be hard to mix and the pull won't be as efficient. Plant material is variable and practice helps gets the proper paste consistency. Fortunately, it is possible to make adjustments:

- Too watery: Adding lime will break up the blob and cloudy release solvent. The cloudiness clears up over time.

- Too dry: Simply add water a few ml at a time until paste is easy to mix. Sometimes this is needed in the later pulls.""

3 Dry

Add anhydrous MgSO4 to the ethyl acetate extract and swirl well. After at least an hour filter to a new jar. Rinse MgSO4 with ~25ml of fresh ethyl acetate and combine that with the dried extract.

4 Salt

Gently drop citric acid into the extract without stirring. Clouds slowly form as the citric acid dissolves by diffusion. After a few hours the clouds settle as beautiful citrate xtals**.

Progress in this step can be monitored by cloud formation: salting is finished when no new clouds form after adding more citric acid. Alternatively, pH paper can be used: salting is finished when pH paper color goes from green to orange/red.

No issues are known if over acidifying as long as solvent is not oversaturated and the citric acid can go into solution.

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

3Mes(↑) + CitH3(↑) ⇒ 3(MesH)Cit(↓)

Other dry organic acids (fumaric, malic, oxalic, succinic, ascorbic, lactic, tartaric, etc) may also precipitate mescaline salt. These salts may have different crystal qualities compared to mescaline citrate. In one example, fumaric acid gave a wispy precipitate that was difficult to work with and not reccomended.

**Stirring after adding citric acid won't cause any major issues, xtals will be smaller but form more quickly.

5 Finish

Pour off ethyl acetate into a storage container (solvent can be washed with brine and reused). Use a coffee filter to help pick up any loose xtals. Rinse xtals with fresh dry ethyl acetate until yellow color is removed to personal cosmetic satisfaction. Scrape up xtals, and leave them uncovered to evaporate all residual solvent, this is the final product.


Mass spec results are current pending. Hopefully they will show the product is mescaline citrate within measurement sensitivity (already >98% pure) even when not completely white after two rinses. Yields are highly dependent on starting cacti powder and can vary from 0.1% to 5% (0.5% to 1% being common).

References