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

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== Introduction ==
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CIELO (Chrystals In Ethyl-acetate Leisurely OTC)
  
This TEK uses freezer chilled acetone<ref>Sphere's chilled acetone process [https://www.dmt-nexus.me/forum/resource.ashx?a=52872]</ref> to extract salvinorin while minimizing the extraction of other plant material. The dry residue is washed with naphtha and then recrystallized from boiling 99% IPA<ref>99% IPA recrystallization process [https://www.designer-drug.com/pte/12.162.180.114/dcd/chemistry/salvinorin.extraction.html]</ref> with a naphtha co-solvent addition<ref>Naphtha addition to recrystalization[https://www.dmt-nexus.me/forum/default.aspx?g=posts&m=1084864#post1084864]</ref>.
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Introduction
  
==Safety==
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In the CIELO approach, Crystals are formed directly In Ethyl-acetate Leisurely using OTC (over the counter) materials.
  
Do not proceed unless you are familiar with handling acetone, 99% IPA, and naphtha. If you are not familiar with these chemicals, learn about their safety and make your personal adult decision on using them or not.
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An alkaline cacti water paste is treated in the microwave to break down plant material and convert mescaline to the free base form (M). Water in the paste is saturated with salt (NaCl), extracted with ethyl acetate, and the extract dryed over MgSO4. Finally, mescaline salt is precipitated by adding citric acid to the extract.
  
Salvinorin is a powerful substance. Proper dose and a sitter in a controlled environment are important (involuntary movement has been reported)<ref>Sagewisdom caution[http://www.sagewisdom.org/caution.html]</ref>.
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Material:
  
Following these suggestions does not guarantee safety. Proceed at your personal adult discretion.
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- Three quart jars with leak-proof ethyl-acetate-resistant lid
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- Food scale to measure weights
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- 100g powdered dry cacti
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- 80g Ca(OH)2 (lime)
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- 300g water
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- Microwave
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- 80g NaCl (plain table salt)
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- 750ml ethyl acetate (sometimes labeled "MEK substitute")
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- pH paper strips
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- 20g MgSO4 (oven dehydrated epson salt)
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- Coffee filters
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- 300mg of Citric acid (~1/16 of a tsp)
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- Xtal scraping tool (e.g. razor blade)
  
== Steps ==
 
  
=== Step 1 ===
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Safety:
Place ~100g of dry salvia leaves in a quart mason jar. Leaves do not need to be ground, but some pushing/compressing will be needed to make them fit. Cool leaves and jar in the refrigerator before the next step.
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=== Step 2 ===
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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.
Add about 1/3 of a quart of freezer chilled acetone and cover with an acetone resistant lid such as the type pictured below:
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[[File:AcetoneResitantLid.png|center]]
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The alkaline microwave process is smelly. Be aware of this, especially in close quarters where other people may notice the smell. Extending this step over time can lower the smell intensity, but it will still be present.
  
Shake for 60s. Uncover and use metal canning jar ring to screw on a coffee filter, tear off excess filter paper beyond the ring, and pour acetone into new quart jar (a small puncture hole may be needed at the top of the filter for air flow if filter becomes fully wet). Repeat this extraction two more times to obtain about 3/4 of a quart of extract (some acetone is left behind on the leaves).
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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.
  
=== Step 3 ===
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Process:
Place extract with acetone resistant lid in freezer until sediment stops forming (~overnight). Decant to shallow glass baking dish leaving solids behind.
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=== Step 4 ===
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1) Base: Shake cactus power and lime in a mason jar until homogeneous. Slowly add the dry mix to a jar with water while stirring to form a homogeneous paste. Microwave at low power (~400W) in short 2-5 minute bursts. Watch closely to not boil over, stirring between irradiations.  Initial paste will liquidy and then become a paste again. Monitor progress with a food scale, targeting for ~200g of water remaining and a firm paste consistentcy. Finally, mix in NaCl salt to saturate remaining water (this also makes the paste more runny), cover, and cool to room temperature. The ideal paste is sticky yet easy to stir: it allows mixing with the solvent in the next step while being easy to decant.
Evaporate acetone in a well ventilated area. It is recommended to avoid direct sunlight. Some water will be absorbed and a fan can speed evaporation towards the end when mostly water remains. Scrape up green powdery residue and transfer it to a small mason jar.
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=== Step 5 ===
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2) Pull: Add ~ 320g 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. Stirring can help loosen up solvent, but about ~ 120g of solvent will remain binded to the paste (the pulls are still very efficient despite this). Pull three more times with ~200g ethyl acetate (simply aim to fill the jar to ~3/4 like before). Combined pulls will give about ~800g of a clear yellow extract. Use pH paper to monitor extraction: green color indicates mescaline presence. By the fourth pull there should be very little visible green on the pH paper (if any).
Wash powder with naphtha. Allow time to settle and ensure naphtha is clear before decanting to not lose any product. Repeat until solvent is no longer a deep green (light green is OK). Allow napthata to evaporate.
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=== Step 6 ===
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Troubleshooting:
Washed powder will still be green. Dissolve it in warm/boiling 99% IPA leaving any insoluble matter behind. Use a hot water bath to heat up the IPA (do not have flames anywhere near solvents).
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=== Step 7 ===
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It is important to get the paste consistentcy right. This is an important part of the process. If it is too watery, ethyl acetate will be absorbed by the paste and not separate. If it is too dry, it will be hard to mix and pull won't be as efficient. Plant material is variable and learning to get a feel for the paste will make the process more reliable. Fortunately each of these issues can be addressed:
Allow IPA too cool and add an equal volume of naphtha. Place cloudy solution in freezer for several days. White xtals will grow over time, for example:
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[[File:Salvinorin_ReX_small.png|center]]
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- Too watery: Adding lime will break up the blob. The separated ethyl acetate will be cloudy, but that clears up over time.
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- Too dry: Simply add water a few ml at a time until paste is easy to mix with solvent. If paste becomes tougher in the later pulls, add a few ml of water until smooth again.
  
Decant green liquid, rinse with Naphtha, and recover xtals. Typical yield is 0.2% to 0.3% (100g of dry leaf will give ~250mg of white powder). Optionally, dissolve product in acetone and evaporate slowly to yield larger crystals (for cosmetic purposes).
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3) Dry: Add MgSO4 to the ethyl afetatr extract and swirl well. After an hour filter to a new jar. Rinse MgSO4 with ~25ml of fresh ethyl acetate and combine that with the dried extract.
  
== Product Information ==
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4) Salt: Gently drop citric acid powder into the extract. Do not stir, simply leasurely cover and let the citric acid slowly dissolve by diffusion. As the citric acid dissolves, clouds form which over time settle as citrate xtals. After a day or so, solution will be clear again with no citric acid grains left and full of shiny citrate xtals. Notes: Stirring after adding citric acid won't cause any major issues, but xtals will be smaller with the faster dissolution. Conversely, adding 50mg of citric acid on the first day (or less) without stirring and until cloudiness stops forms seed xtals with a chance of getting larger xtals with subsequent citric acid addition(s). As with the pulls, progress in this step can be monitored with pH paper. Color will go from green (alkaline free base present) to orange (neutral) to red (excess citric acid). Orange is the target, but no issues occur if over acidifying as the citric acid simply remains in solution.
This produces a relatively pure powder thought to have ~ 80% of salvinorin A<ref>Endlessness salvinorin extract analysis [https://www.dmt-nexus.me/forum/default.aspx?g=posts&t=31790]</ref>.
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== Dosage ==
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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. Scrape up xtals and (optionally) rinse them with fresh dry ethyl acetate until yellow color is removed to personal cosmetic satisfaction. Leave uncovered to evaporate residual solvent, this is the final product.
One milligram is considered a large dose when vaporized, with 0.2 to 0.5mg being a usual active range. One method of dosing is dissolving salvinorin in acetone (which saturates at about ~23mg/ml<ref>Salvia-Divinorum 2004[https://erowid.org/archive/rhodium/chemistry/salvinorin.extraction.faq76.html]</ref>, equivalent to 29mg/g) and calculating the dosage per drop. A practical way to do this is to pre-weigh the acetone and salvinorin, mix, and then measure the average drop weight of 10 drops or more. For example, if 125mg of salvinorin are dissolved in 5g of acetone a single ~20mg drop will carry ~0.5mg of product. That would be many personal doses in a small ~7ml vial. However, it is not currently understood how well salvinorin keeps in solution over time (cool dark storage place makes sense). Verify that acetone does not evaporate while stored since that would throw off the dosage (eventually, precipitation will also happen).  
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Mass spec results 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). If yield is > 1% or pH paper remains green after salting, add more citric acid to salted ethyl acetate to see if more salts precipitate (300mg of citric acid can make up to ~1.3g of mescaline citrate).  
To administer, simply add the desired dosage by counting drops to your vaporization device, allow the acetone to  
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'''fully''' evaporate, and then vape. High vaping temperatures are not required and it has been reported that 180C e-mesh setting can be sufficient<ref>Salvinorin extract e-mesh report[https://www.dmt-nexus.me/forum/default.aspx?g=posts&t=96145]</ref>.
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== References ==
 
== References ==
 
<references/>
 
<references/>

Revision as of 16:50, 24 February 2021

CIELO (Chrystals In Ethyl-acetate Leisurely OTC)

Introduction

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

An alkaline cacti water paste is treated in the microwave to break down plant material and convert mescaline to the free base form (M). Water in the paste is saturated with salt (NaCl), extracted with ethyl acetate, and the extract dryed over MgSO4. Finally, mescaline salt is precipitated by adding citric acid to the extract.

Material:

- Three quart jars with leak-proof ethyl-acetate-resistant lid - Food scale to measure weights - 100g powdered dry cacti - 80g Ca(OH)2 (lime) - 300g water - Microwave - 80g NaCl (plain table salt) - 750ml 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.

The alkaline microwave process is smelly. Be aware of this, especially in close quarters where other people may notice the smell. Extending this step over time can lower the smell intensity, but it will still be present.

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) Base: Shake cactus power and lime in a mason jar until homogeneous. Slowly add the dry mix to a jar with water while stirring to form a homogeneous paste. Microwave at low power (~400W) in short 2-5 minute bursts. Watch closely to not boil over, stirring between irradiations. Initial paste will liquidy and then become a paste again. Monitor progress with a food scale, targeting for ~200g of water remaining and a firm paste consistentcy. Finally, mix in NaCl salt to saturate remaining water (this also makes the paste more runny), cover, and cool to room temperature. The ideal paste is sticky yet easy to stir: it allows mixing with the solvent in the next step while being easy to decant.

2) Pull: Add ~ 320g 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. Stirring can help loosen up solvent, but about ~ 120g of solvent will remain binded to the paste (the pulls are still very efficient despite this). Pull three more times with ~200g ethyl acetate (simply aim to fill the jar to ~3/4 like before). Combined pulls will give about ~800g of a clear yellow extract. Use pH paper to monitor extraction: green color indicates mescaline presence. By the fourth pull there should be very little visible green on the pH paper (if any).

Troubleshooting:

It is important to get the paste consistentcy right. This is an important part of the process. If it is too watery, ethyl acetate will be absorbed by the paste and not separate. If it is too dry, it will be hard to mix and pull won't be as efficient. Plant material is variable and learning to get a feel for the paste will make the process more reliable. Fortunately each of these issues can be addressed:

- Too watery: Adding lime will break up the blob. The separated ethyl acetate will be cloudy, but that clears up over time. - Too dry: Simply add water a few ml at a time until paste is easy to mix with solvent. If paste becomes tougher in the later pulls, add a few ml of water until smooth again.

3) Dry: Add MgSO4 to the ethyl afetatr extract and swirl well. After 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 powder into the extract. Do not stir, simply leasurely cover and let the citric acid slowly dissolve by diffusion. As the citric acid dissolves, clouds form which over time settle as citrate xtals. After a day or so, solution will be clear again with no citric acid grains left and full of shiny citrate xtals. Notes: Stirring after adding citric acid won't cause any major issues, but xtals will be smaller with the faster dissolution. Conversely, adding 50mg of citric acid on the first day (or less) without stirring and until cloudiness stops forms seed xtals with a chance of getting larger xtals with subsequent citric acid addition(s). As with the pulls, progress in this step can be monitored with pH paper. Color will go from green (alkaline free base present) to orange (neutral) to red (excess citric acid). Orange is the target, but no issues occur if over acidifying as the citric acid simply remains in solution.

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. Scrape up xtals and (optionally) rinse them with fresh dry ethyl acetate until yellow color is removed to personal cosmetic satisfaction. Leave uncovered to evaporate residual solvent, this is the final product. Mass spec results 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). If yield is > 1% or pH paper remains green after salting, add more citric acid to salted ethyl acetate to see if more salts precipitate (300mg of citric acid can make up to ~1.3g of mescaline citrate).

References