Difference between revisions of "Washing Spice"

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The purpose of washing is to disperse impurities off of the product or out of a solution containing the product and into an intermediate solvent.
 
The purpose of washing is to disperse impurities off of the product or out of a solution containing the product and into an intermediate solvent.
  
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====='''Alkaline Solution Washing of Inactive Impurities'''=====
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===== Alkaline Solution Washing of Impurities =====
  
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Most of the impurities that plague yields tend to be quite soluble in both alkaline aqueous solutions and non-polar solvents.  To remove these impurities, an imbalance in equilibrium must be created between these two types of solutions, causing the impurities to disperse into a disposable solution from the solution containing the product.
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Most of the impurities that plague yields tend to be quite soluble in both alkaline aqueous solutions and non-polar solvents.  To remove these impurities, an imbalance in equilibrium must be created between these two types of solutions, causing the impurities to disperse into a disposable solution from the solution containing the product.  This procedure is commonly used for purifying product from extractions that utilize naphtha or heptane to obtain a whiter product.
  
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====='''Solvent Washing and Isolation of Active Impurities'''=====
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{{Procedure|Washing Spice of Oxidization and Inactive Impurities Using Alkaline Solution<ref>[[Acolon 5's Spice Washing Tek]]</ref>|
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# Create a solution of warm water with a weak base such as sodium bicarbonate (baking soda) or sodium carbonate (washing soda) to render an alkaline solution using a pinch of base.
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#* ''sodium bicarbonate can be [[Conversion of Sodium Bicarbonate into Sodium Carbonate|converted to sodium carbonate]].''
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# Dissolve product in an [[NPS]] of preference.
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# Add alkaline solution to the NPS at a ratio of about 1:4 and mix thoroughly for a short time (5-10 seconds).
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# Remove and collect the top NPS layer promptly, and evaporate the solvent until concentrated/saturated and freeze precipitate.
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}}
  
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Active impurities require a slightly different method of isolation for purification and generally rely strictly on differences of their solubility or insolubility in specific solvents.  Often, reactions are required in order to create these differences, as the products tend to exhibit very similar properties.
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===== Solvent Washing and Isolation of Impurities =====
  
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<noinclude>
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Some product may contain undesirable active or inactive impurities with solubility properties differing greatly from the more desirable components.
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# Get a glass and put a teaspoon of baking soda (or 1/4 teaspoon of sodium carbonate) in it. Fill with about 100&ndash;150mL luke warm/room temperature water. Stir, stir, stir. It will not all dissolved, but we are making a saturated solution so that is fine. Let all soilds settle.
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# Dissolve freeze preciptated spice in enough warm naphtha that is does not cloud upon cooling. Less is better, but use enough to prevent precipitation. I use 1/2 pint canning jars for this. For 1g of spice I would use 200mL of warm naphtha or bestine.
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# Take a baster/syring/nasal aspirator and suck up some of the saturated baking soda water &hellip; do not get any solid baking soda in the baster.
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# Add until the volume of baking soda (or sodium carbonate) solution is about 1/4 the volume of naphtha.
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# Swirl around for about a minute, do not heat. You can shake.
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# After swirling I usually take my nasal aspirator (I like it better than a syringe or a turkey baster) and suck up some of the naphtha layer and squirt it into the baking soda layer &hellip; not sure if it helps or not, but it is what I always do. It just mixes it up a little better and it separates pretty quickly.
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# Remove naphtha layer (top layer!) save and recrystalize normally (freeze or room temp, your choice)
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# Trash baking soda layer (bottom layer!), or add more naphtha and attempt to recover any lost yield (I've tried without success, just not enough spice in there).
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I imagine that this would work with naphtha just pulled from the basified mimosa juice (uncrystalized) &hellip; however, I like to freeze precipitate first. It seems to get a much cleaner product.
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{{:Purification of Spice Fumarate Product}}
  
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With the method I have outline above I have taken yellow oily freeze precipitated spice that badly burns the tongue and turned it into clear spice that no longer burns (just a little bitter). My best batches of spice were made using this technique.
 
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The taste and vaporization also seems to be improved.
 
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Total yield loss after washing AND recrystalization from a gram is about 80mgs. I've read some threads about how yellow spice is better/smoother than clear spice. I am not in that group of people. I think that crystal clear/white spice gives the best experience.
 
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Also after final recrystalization I will put my mason jar containg my spice (no solvent, just spice) into a hot water bath and melt it down. I then put it into the freezer for about 10 minutes. The spice that comes out is denser, easier to vaporize, and for some reason more potent. I highly suggest trying the spice meltdown method &hellip; you will be suprised at the results!
 
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# Obtain naptha/spice solution from extraction.
 
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# Freeze until spice precipitates.
 
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# Pull or pour out all naptha from the precipitate and set to dry.
 
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# After the spice is dry, add heptane (heptane can be purchased from most hardware/craft stores in the brand BESTINE).
 
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# Warm the heptane/spice solution slowly in almost boiling water and agitate (the solution should be transparent).
 
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# Freeze.
 
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# After the spice has precipitated, pull or pour the heptane from the solution and set to dry.
 
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# The spice is now ready for use. Spice from the A/B naptha extraction will result in clean pearly white crystals.
 
  
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<noinclude>
  
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== Reference ==
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===== Reference =====
  
 
{{Page_Footer|Enhancement Tek|DMT}}
 
{{Page_Footer|Enhancement Tek|DMT}}
 
<noinclude>
 
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Latest revision as of 22:02, 16 September 2011

Note error.png Note: This page has been transcluded to The Nexian DMT Handbook under the Washing Spice section or other locations within or without the handbook. Please markup in consideration of this. The top section header is to remain in place as a reference for subsequent section headers and to allow easy editing directly from the handbook.

Washing Spice

The purpose of washing is to disperse impurities off of the product or out of a solution containing the product and into an intermediate solvent.

Alkaline Solution Washing of Impurities

Most of the impurities that plague yields tend to be quite soluble in both alkaline aqueous solutions and non-polar solvents. To remove these impurities, an imbalance in equilibrium must be created between these two types of solutions, causing the impurities to disperse into a disposable solution from the solution containing the product. This procedure is commonly used for purifying product from extractions that utilize naphtha or heptane to obtain a whiter product.

Washing Spice of Oxidization and Inactive Impurities Using Alkaline Solution[1] Cog.png
  1. Create a solution of warm water with a weak base such as sodium bicarbonate (baking soda) or sodium carbonate (washing soda) to render an alkaline solution using a pinch of base.
  2. Dissolve product in an NPS of preference.
  3. Add alkaline solution to the NPS at a ratio of about 1:4 and mix thoroughly for a short time (5-10 seconds).
  4. Remove and collect the top NPS layer promptly, and evaporate the solvent until concentrated/saturated and freeze precipitate.


Solvent Washing and Isolation of Impurities

Some product may contain undesirable active or inactive impurities with solubility properties differing greatly from the more desirable components.



Purification of Spice Fumarate Product[2] Cog.png
NOTE Information.png

This procedure is generally performed to remove excess fumaric acid based on it's low solubility in water and to remove residual solvent by dispersing it and allowing it to evaporate more easily and completely. The resulting product is considered to be the most appropriately purified form for oral administration.

  1. Add a small amount of water in slight excess of completely submerging the product.
  2. Stir mixture to dissolve the active fumarate component.
  3. Decant solution off, leaving solids behind.
  4. Repeat process until no more color change is observed in the solution, but perform once more with a minimal amount of water for good measure.
    • the solids remaining should be mainly composed of the excess fumaric acid from the starting material.
  5. Evaporate the solution with or without heat and airflow to achieve purified crystalline fumarate product.
    • reduction of the solution by heat and airflow is generally always beneficial, but slow evaporation in the later stages may result in a more uniform and attractive crystalline product.




Reference
  1. ↑ Acolon 5's Spice Washing Tek
  2. ↑ FASA Alteration of Final Purification
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