Difference between revisions of "Washing Spice"

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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]

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 converted to sodium carbonate. Dissolve product in an NPS of preference. 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 promptly, and evaporate the solvent until concentrated/saturated and freeze precipitate.

{{[b]Xtechre's Spice Washing Techre; Ver 1.0.[/b]

This technique can be used on Freebase DMT that has been acquired by either A/B, STB or a freebasing of DMT salts such as DMT fumarates.

  #[color=red]1.[/color] Add drop wise to DMT Naphtha at room temperature, agitating until all DMT is dissolved. This may take some work at room temp, so a kitchen knife may help to stir/break up the DMT, then decant away from any remaining undissolved impurity's. [i]Depending on how dirty the product was initially, some visually detectable impurity's may remain undissolved. These impurity's depend on the starting material, in the case of DMT yielded from FASW this may be excess fumaric acid (just one example).[/i] This is your Non Polar Phase.
        
  #[color=orange]2.[/color] Roughly measure the volume of DMT solution prepared in Step 1... and quadruple it. This is the volume of water you will add a pinch of sodium carbonate to. Literally a pinch. For a gram of DMT this pinch will be small. For 10 grams it might be a little bigger... it really doesn't take much. This is your Aqueous basic phase.

  #[color=yellow]3.[/color] Mix the DMT solution (Non Polar Phase) with the Sodium Carbonate solution (Aqueous Basic Phase) with vigor for 3.333 seconds and firmly place upon the table, watch the two layers become visible and separate them mechanically as fast as possible using whatever baster/glass syringe/decanting technique you have mastered in the DMT extraction earlier. Separating these layers (technically phases) quickly is the key here other wise you will experience loss of DMT into the basic aqueous phase.

  #[color=green]4.[/color] Wash the jar used in the step above, then take the DMT solvent solution you just separated, add it back to the jar and wash it exactly the same as step 3 BUT using clean water with no base added. Do this a total of twice.

  #[color=blue]5.[/color] Taking the DMT solvent solution and evaporate it to a volume of 50% or less (till it go's milky when blown upon... this is to make it saturated so that the DMT can precipitate out efficiently when you... put it  in the freezer.}}

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]

NOTE 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. Add a small amount of water in slight excess of completely submerging the product. Stir mixture to dissolve the active fumarate component. Decant solution off, leaving solids behind. 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. 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