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

Revision as of 17:18, 24 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.

Aqueous akaline cacti 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 dried over MgSO4. Finally, mescaline salt is precipitated with citric acid, rinsed, and recovered.

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.

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 dry cactus power and lime in a mason jar until homogeneous. Slowly add the dry mix to a jar with the 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 liquify 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. 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. This can sometimes occur in the later pulls, especially when using new/dry solvent.

3 Dry

Add dry MgSO4 to the ethyl afetate 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 powder into the extract without stirring. Leasurely cover and let the citric acid slowly dissolve by diffusion. Clouds form and settle as citrate xtals. After a day or so, solution will be clear again with no citric acid grains left and full of beautiful xtals.

Stirring after adding citric acid won't cause any major issues, but xtals will be smaller. Conversely, adding only 50mg of citric acid on the first day forms seed xtals, from which larger xtals could grow 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 (salting is complete) to red (excess citric acid). Orange is the target, but no issues are known if over acidifying as the excess the citric simply remains in solution (as long as solvent is not over saturated with a large amount of citric acid).

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 in jar and filter with fresh dry ethyl acetate until yellow color is removed to personal cosmetic satisfaction. Scrape up and combine xtals, and leave them uncovered to evaporate residual solvent, this is the final product.

Mass spec results are current pending. Howpefully 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). 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