Difference between revisions of "Dry Technique Extraction"

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Dry Technique Extraction

Note:

This technique is still experimental and may result in variable success if used with MHRB.

Dry techniques (drytek) evolved from and are ideally intended for the implementation of the FASA method of crystallization and serve as the only techniques able to implement acetone as an extraction solvent. Acetone is generally favored for its ability to extract a notably broad range of active products.

Considerations:

The use of dry techniques requires fewer and less toxic materials than the techniques that employ aqueous phases and separatory methods. The materials required are generally of a more household nature. They are most effectively applied to powdered botanical material. Acetone is, however, completely water miscible, so proper drying procedures are of the utmost importance. This technique may or may not require the defatting of botanical materials, depending on the intended method of crystallization. Dry techniques are the youngest of the current extraction techniques though apparently sound in theory and in practice.

Overview of Materials and Methods

Materials Required
Source Material: Powdered DMT-Containing Botanical Material
Solvents: Water Acetone
Reagents/Desiccants: Magnesium Sulfate (Epsom Salt) Household Base: Either Sodium Carbonate (Washing Soda) or Calcium Hydroxide (Pickling Lime) or Sodium Bicarbonate (Baking Soda) Only after Conversion to Sodium Carbonate

Material Considerations:

• Acetone can be purchased at hardware stores but should be confirmed as pure acetone prior to purchase. Note that almost all acetone can contain up to 5% water contamination, depending on time and shelving conditions.
• In order to be utilized for extraction, sodium bicarbonate must undergo conversion to sodium carbonate.
• Lime is often found difficult to decant acetone off of and also difficult to filter out of acetone, whereas sodium carbonate is generally found more agreeable for both.
• Distilled water is preferable, as tap water almost always contains impurities that can potentially tamper with resulting yields.
• With few exceptions, the source material should be completely pulverized to a powder consistency before use, as this technique's choice of reagents are not quite capable of penetrating cell structure.

Methods:

Extractions by dry techniques are characterized by the lack of a traditional aqueous phase in the extraction process, and instead, opting for basification within a paste which is followed by chemically drying the paste with desiccant. The process does not make use of separatory methods, and instead is characterized by it's use of dry-washing, decanting and non-intensive filtering methods. Certain materials must be rendered anhydrous prior to use.

Material Preparation

Rendering Anhydrous Magnesium Sulfate

Spread Epsom Salt (Hydrated Magnesium Sulfate) on an aluminum foil covered pan. Place in the oven on 400°F for about one hour, or until the salt becomes gray and ash-like. Place your now anhydrous magnesium sulfate into a storage container and store away from moisture. If it becomes hydrated again, the process can be repeated. NOTE This can also be done on the stove top/oven ring, however it should be noted that as the Epsom Salt releases water it will stick to the inside of your pot but as it reaches complete dehydration and becomes grey and ash like it will unstick and become a powder.

Rendering Anhydrous Acetone
Pour anhydrous magnesium sulfate directly into the can of acetone. Shake vigorously for an extended amount of time. Allow to settle for one day. Observe the magnesium sulfate at the bottom of the can. if it appears extremely moist, repeat the process. if it appears quite dry, the acetone is ready for use. Store away from moisture and never leave uncapped.

THP Approach to Rendering Anhydrous Acetone
Prepare THP by cutting the bottom off of an HDPE bottle and stuffing cotton balls the neck. Fill THP with anhydrous magnesium sulfate, leaving enough room for an appropriate amount of acetone to fill. Pour acetone through THP until satisfactorily dried. Store acetone away from moisture and never leave uncapped.

Conversion of Sodium Bicarbonate into Sodium Carbonate

Sodium carbonate on left and bicarbonate on right, both in oversaturated solutions. After vs Before the conversion. Sodium carbonate on left and bicarbonate on right. Notice how carbonate is more grainy and bicarbonate more loose/fluffy Weigh your sodium bicarbonate, and put it onto a non-aluminum pan or oven-safe dish. Place in the oven at 400ºF (205ºC) for one hour to one hour and a half to release CO2 and water. Alternatively you can put in a stainless steel (dont use any other material!) pot on the stovetop, 20mins should be enough. Be careful because the powder will be VERY hot, leave it to cool down for a while. The resulting material should have lost around 20% of the original weight. It will be of a slightly less powdery consistency, closer to sugar than flour. If it didnt lose a third of the original weigh, leave it for longer in the oven sodium carbonate feels a bit looser and grainier than bicarbonate, and in an oversaturated solution, sodium bicarbonate will remain powdery while sodium carbonate tends to rock up. NOTE This can also be done on a stove top/oven ring in a pot and take around 10 minutes to completely dehydrate

Extraction Procedure

1. Mix the intended base with the powdered source material at a ratio between 1:2 and 1:1.
   • The product remains in its natural salt form which is generally considered to be quite free from the botanical cell structure in powdered material.
2. Add only enough water to thoroughly moisten the mixture to the consistency of a paste while stirring to ensure the consistency of the mixture.
   • Although this is not generally considered a traditional aqueous phase in that it is not a solution, it is an aqueous phase in that it is excessively hydrated and sufficiently aqueous to facilitate reaction.
3. Allow adequate time to soak in order for reaction to occur.
   • The acid component of salt-form product undergoes reaction with the base, effectively neutralizing the acid and freeing the product in its pure alkaloid form, or freebase.
4. Stir in anhydrous magnesium sulfate until thoroughly dry.
   • The magnesium sulfate acts as a desiccant, and that this is performed in order to prevent water contamination of the acetone.
5. Add an excess of anhydrous acetone and stir thoroughly, allotting adequate time and stirring for thorough dissolution of the product into the acetone.
   • The more contact allotted between the product and the acetone, the greater the saturation.
6. Decant and/or filter acetone and collect, being careful not to allow any particulates into the collection vessel.
   • The bases used should not harm the quality of the product, but may interfere with the accuracy of weight.
7. Repeat steps 5-6 with fresh acetone until material is exhausted to satisfaction, and proceed to the appropriate desired crystallization method.
   • Three washes is generally considered sufficient.

Further Elaboration and Technical Support

Directory of Current Dryteks

Discussing Alternative Spice Extraction Techniques