Difference between revisions of "Washing Spice"

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(Solvent Washing and Isolation of Impurities: transclusion)
(Alkaline Solution Washing of Impurities)
 
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{{Procedure|Washing Spice of Oxidization and Inactive Impurities Using Alkaline Solution<ref>[[Acolon 5's Spice Washing Tek]]</ref>|
 
{{Procedure|Washing Spice of Oxidization and Inactive Impurities Using Alkaline Solution<ref>[[Acolon 5's Spice Washing Tek]]</ref>|
# Saturate 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.
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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.
 
#* ''sodium bicarbonate can be [[Conversion of Sodium Bicarbonate into Sodium Carbonate|converted to sodium carbonate]].''
 
#* ''sodium bicarbonate can be [[Conversion of Sodium Bicarbonate into Sodium Carbonate|converted to sodium carbonate]].''
 
# Dissolve product in an [[NPS]] of preference.
 
# Dissolve product in an [[NPS]] of preference.
# Add alkaline solution to the NPS at a ratio of about 1:4 and mix thoroughly.
+
# Add alkaline solution to the NPS at a ratio of about 1:4 and mix thoroughly for a short time (5-10 seconds).
# Remove and collect the top NPS layer, and proceed to recrystallization procedure of preference.
+
# Remove and collect the top NPS layer promptly, and evaporate the solvent until concentrated/saturated and freeze precipitate.
 
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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