Ethyl Acetate Approach Harmala

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Introduction

This Tek was inspired by Loveall's Cielo Tek, with the aim of cutting out manske steps to aid in yields and substantially quicken the process while maintaining purity. The quickest run has been 2.5hours with decent yields and purity.

Thanks to everyone who has contributed to this process: Loveall, Benzyme, _Trip_, and others.

This Tek is still a work in progress however lab and test results have been confirmed and are very promising for a quick Tek. Feel free to contribute. Photo's to follow soon.


Safety

Review ethyl acetate[1] and citric acid[2] safety information. Verify solvent MSDS, plastic compatibility, and clean evaporation.

This TEK is food safe if food grade materials are used.


Following this advice does not guarantee safety. It is up to each adult individual to make their own personal decisions.


Consumables

  • 300ml water/ 600-800ml of distilled water (tap water works fine too)
  • 25g Ca(OH)
  • 100g of Syrian Rue seeds
  • 1lt ethyl acetate (sometimes sold as "MEK substitute")
  • 10-15g of citric acid
  • Sodium Carbonate
  • 1lt Jar

Equipment

  • Blender
  • French press
  • Kitchen scale
  • Coffee filters, support basket, and funnel Or lab filter and vacuum pump.
  • 1lt mason glass jars with lids
  • Fridge
  • Milligram scale
  • Microwave


Detailed Process

Base Water

-Add 300ml of water to 25g of calcium hydroxide and mix to form 'base water'. Alternatively one can use sodium carbonate (this may negate the need for filtering later). Note: Sodium Carbonate has not been fully tested start to finish.

Powder

-Get 100g of rue seeds and grind them up, mix with 'base water'. A glass bender is quickest.

Microwave

-Microwave the rue/base mix until 2/3rd's of the water content is steamed off (use kitchen scales to measure this). As a guide a 750 watt microwave at 5-7min bursts should work fine. Mix between bursts. Several burst will be required. This may be like the Cielo Tek and require more water to facilitate efficient pulls, thus may need to be fine tuned. And like the Cielo tek may not need microwaving. However for now those ratios and the microwave step should work fine.

Water Bath

-Prepare a warm water bath with boiling water and warm 1lt of EA. No open flames. (This step helps yields).

Pulling

-Place ground up water-base/ rue seed mix in a french press. Using the french press conduct 6 pulls with the 1lt of warm EA. So 6x 160ml pulls approx (keep in mind rue seeds will absorb a little bit of EA). Carefully decant into 1lt jar(6x warm pulls at 1-2 mins each). Decant from the french press after each pull. Keep rue base mix and fresh EA in the warm water bath to improve yield (obviously in their respective containers).

Recovery/ Filter

-Approx just over 800ml of EA should be recovered and then filtered (filtering may not be necessary if one has used sodium carbonate as a base). Lab filter is recommended, coffee filters should work too.


Salting

-Add 15g of citirc acid to the combined EA pulls and shake for 5-10mins (red/orange/yellow oil should form very fast). Orange/red goo forms at the base of the jar and the rest of the jar gets covered with sticky yellow goo (making it easy to decant). (This goo should crystalize if left for 24hours+. This is not necessary though, the goo makes decanting easy so one can decant right away).

Decant & Reclaim

-Decant EA (this can be cleaned and reused next extraction). One can also add a little bit of EA to the citrate stuck to the jar to clean it up a little bit but it is not necessary. Again decant this EA.

Dissolve Goo

-After the tiny amount of EA still left in the jar evaporates, add 600-850ml of warm water to the citrate goo, it will dissolve fairly quickly. (Ratio it down if using less seeds). The more water the more sodium carbonate may be needed depending on yield but the more water used gives a cleaner product (in appearance anyway). This may need to be dialed in. See "further investigation" notes below.

Base

-Base slowly with sodium carbonate (you can shake up the jar to get excess sodium carbonate to dissolve once the acid is neutralized). Add enough sodium carbonate until the harmala starts to crash out then add a little bit more.

Crash & Filter

-Harmala will crash out quickly. Some of the FB harmala will float to the top, this needs to be left to cool. (Sticking the jar in a freezer appears to speed up the process and harmala crashes as it cools. The floating harmala should settle. This should not take long).

Once it has finished crashing out filter and dry the product.

No need to leave this overnight, if left for too long (say 24hrs+) some impurities appear to crash out. The final product in this step should crash out quick and should/ can be filtered within a hour or 2 (often quicker). As a rule of thumb I wait for the floating harmala to settle to the bottom. This rarely exceeds the 2 hour mark, again usually a lot quicker. Once filtered and dried you have the final product. (Keep the sodium carbonated water after filtering, more harmala may crash out overnight. It usually appears more impure by color though)


Well done this should have been a quick and easy run. 3.7% is usually the minimum percentage pulled on first run. The process can be repeated on spent material and re-pulled with hot EA to get over 5%.



Convert FB Harmala to Citrate Harmala for Pharmahuasca

Initially the citric acid crashes out a goo. However, once clean FB Haramla is obtained one can dissolve it in hot EA (with the help of a few shakes of the jar) and then add citirc acid at about 20mg per ml of EA. This should give you nice clean yellowish harmala citrate crystals. They may be slightly sticky.

Lab Analysis

A1.jpg

Above is harmala lab analysis results. Figure A is the traditional 3x Manske, figure B & C are from the EA approach (B & C were conducted with slightly different variations). Figure B is the standard EA approach TEK as written above.



Further investigations

-Sodium Carbonate should be usable as a base for this Tek but it's yet to be confirmed.

-Chemical drying solvent after pulls does not change the end result/ purity.

-A mini A/B at the end for clean up does not appear to change end result/ purity.

-Other acids are yet to be tested. Fumaric acid was briefly test and should work.

-Microwave route may be unnecessary as eventually discovered with the Cielo Tek.

-Dissolving the goo in more water appears to give a purer looking product but may not crash out as easily, using too little amount of water gives a very impure looking product. The ideal ratio is yet to be worked out.

Reuse

Reusing solvents is encouraged[3] at the DMT nexus.


Wash spent extract with sodium carbonate saturated water (35% by weight). About 1/5 of the solvent volume as saturated water is enough. Shake vigorously (emulsions do not form). CO2 bubbles may be visible during citric acid neutralization. Keep an eye on any bubbles and release any pressure buildup regularly. Neutralization can be optionally verified with pH paper. Rest washed solution until clear (up to a day or more).


Remove the water layer with a pipette or separatory funnel. Freezing the solvent and filtering the ice slush that forms with a metal strainer is also an option. Finally, decant off any excess solid sodium carbonate/citrate. CaCl2 (sold as deicer, calcium hardener for pools and sometimes is the only ingredient in moisture absorbers tubs) can be used to ensure there is no water still left in the EA.

References

Ethyl Acetate Safety[1] Citric Acid Safety [2]
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