Difference between revisions of "Washing Spice"

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====='''Alkaline Solution Washing of Inactive Impurities'''=====
 
====='''Alkaline Solution Washing of Inactive 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.  Some of these impurities may be active ([[DMT N-Oxide]], most notably) while others may not.
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{{Procedure|Washing Spice|
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# 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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#* ''sodium bicarbonate can [[#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.
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# Remove the top NPS layer, and proceed to recrystallization procedure of preference.
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}}
  
 
====='''Solvent Washing and Isolation of Active Impurities'''=====
 
====='''Solvent Washing and Isolation of Active Impurities'''=====
  
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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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Removal of active impurities generally relies strictly on differences of their solubility or insolubility in specific solvents.  Most notably, [[Jungle Spice]] may be removed from DMT using particular solvents such as naphtha or heptane.
  
 
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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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{{:Conversion of Sodium Bicarbonate into Sodium Carbonate}}
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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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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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== Reference ==
 
== Reference ==

Revision as of 06:23, 27 January 2010

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 Inactive 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. Some of these impurities may be active (DMT N-Oxide, most notably) while others may not.

Washing Spice Cog.png
  1. 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.
  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.
  4. Remove the top NPS layer, and proceed to recrystallization procedure of preference.


Solvent Washing and Isolation of Active Impurities

Removal of active impurities generally relies strictly on differences of their solubility or insolubility in specific solvents. Most notably, Jungle Spice may be removed from DMT using particular solvents such as naphtha or heptane.


Conversion of Sodium Bicarbonate into Sodium Carbonate Cog.png
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
  1. Weigh your sodium bicarbonate, and put it onto a non-aluminum pan or oven-safe dish.
  2. 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.
  3. 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 Information.png
This can also be done on a stove top/oven ring in a pot and take around 10 minutes to completely dehydrate


Reference

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