- By G.Patton
Some side extraction products. Just recrystallize this.
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Solvents:
Heptane
Equipment:
Filter papers, Beakers, Water bath, Pipette
1. Find a suitable solvent for the recrystallization;
2. Dissolve the impure solid in a minimum volume of hot solvent;
3. Remove any insoluble impurities by filtration;
4. Slowly cool the hot solution to crystallize the desired compound from the solution.
Finding a suitable solvent
The first consideration in purifying a solid by recrystallization is to find a suitable solvent. A good recrystallization solvent should fit the following criteria:
1. The compound should be very soluble at the boiling point of the solvent and only sparingly soluble in the solvent at room temperature.
2. The unwanted impurities should be insoluble in the hot solvent.
A good recrystallization solvent for DMT is heptane. DMT is not very soluble in it at room temperature but quite soluble as we add heat. Most common spice impurities, however, are not very soluble in it at all and can thus be separated via simple decanting.
Dissolve solid into hot solvent
Prepare a waterbath and heat the heptane in their own beaker until boiling. Add heated solvent dropwise into the beaker containing the extract. The heptane will go cloudy almost immediately and take on a yellow color as the DMT goes into solution. Keep adding boiling hot solvent until further addition or agitation causes no more DMT to dissolve.
Your beaker should now contain yellowish-tinged heptane with an orange-brown blob of oil and undissolved solids at the bottom of the vessel. Carefully filter the solution into another beaker, careful to leave the impurities behind. Repeat dropwise addition of heated solvent and filtration to ensure no DMT is left behind.
Decolorize with carbon
Now that we have dealt with insoluble impurities, our solution is see-through but tinged yellow. This discoloration is due to the presence of high-molecular-weight reaction by-products which may have been formed during the extraction process. A simple wash with activated carbon will get rid of coloring compounds. (Activated carbon is extremely efficient at absorbing impurities due to its large surface area.)
1. Add excess solvent and activated carbon, and boil the solution for a few minutes. The colored impurities will adsorb onto the surface of activated charcoal.
2. Remove the charcoal with absorbed impurities by filtration. Your solvent should now be almost clear. If the yellow color persists, repeat the charcoal wash carefully.
Note: Very little activated carbon is needed to remove the colored impurities from a solution. You must be careful in your use of decolorizing carbon: if too much is used, it can adsorb the desired compound from the solution as well as the colored impurities.
Crystallization
After the solution has been filtered cover the flask containing the hot filtrate and set it aside undisturbed to cool slowly to room temperature. As the solution cools, the solubility of the dissolved compound will decrease and the solid will begin to crystallize from the solution. Once the solution reaches room temperature, move it into the refridgerator, and finally into the freezer to freeze precipitate most of the DMT.
The slower your solution cools, the cleaner and larger your crystals will be.
#DMT_recrystallization #DMT #recrystallization
- By G.Patton
DMT recrystallization
Solvents:
Heptane
Equipment:
Filter papers, Beakers, Water bath, Pipette
1. Find a suitable solvent for the recrystallization;
2. Dissolve the impure solid in a minimum volume of hot solvent;
3. Remove any insoluble impurities by filtration;
4. Slowly cool the hot solution to crystallize the desired compound from the solution.
Finding a suitable solvent
The first consideration in purifying a solid by recrystallization is to find a suitable solvent. A good recrystallization solvent should fit the following criteria:
1. The compound should be very soluble at the boiling point of the solvent and only sparingly soluble in the solvent at room temperature.
2. The unwanted impurities should be insoluble in the hot solvent.
A good recrystallization solvent for DMT is heptane. DMT is not very soluble in it at room temperature but quite soluble as we add heat. Most common spice impurities, however, are not very soluble in it at all and can thus be separated via simple decanting.
Dissolve solid into hot solvent
Prepare a waterbath and heat the heptane in their own beaker until boiling. Add heated solvent dropwise into the beaker containing the extract. The heptane will go cloudy almost immediately and take on a yellow color as the DMT goes into solution. Keep adding boiling hot solvent until further addition or agitation causes no more DMT to dissolve.
Your beaker should now contain yellowish-tinged heptane with an orange-brown blob of oil and undissolved solids at the bottom of the vessel. Carefully filter the solution into another beaker, careful to leave the impurities behind. Repeat dropwise addition of heated solvent and filtration to ensure no DMT is left behind.
Decolorize with carbon
Now that we have dealt with insoluble impurities, our solution is see-through but tinged yellow. This discoloration is due to the presence of high-molecular-weight reaction by-products which may have been formed during the extraction process. A simple wash with activated carbon will get rid of coloring compounds. (Activated carbon is extremely efficient at absorbing impurities due to its large surface area.)
1. Add excess solvent and activated carbon, and boil the solution for a few minutes. The colored impurities will adsorb onto the surface of activated charcoal.
2. Remove the charcoal with absorbed impurities by filtration. Your solvent should now be almost clear. If the yellow color persists, repeat the charcoal wash carefully.
Note: Very little activated carbon is needed to remove the colored impurities from a solution. You must be careful in your use of decolorizing carbon: if too much is used, it can adsorb the desired compound from the solution as well as the colored impurities.
Crystallization
After the solution has been filtered cover the flask containing the hot filtrate and set it aside undisturbed to cool slowly to room temperature. As the solution cools, the solubility of the dissolved compound will decrease and the solid will begin to crystallize from the solution. Once the solution reaches room temperature, move it into the refridgerator, and finally into the freezer to freeze precipitate most of the DMT.
The slower your solution cools, the cleaner and larger your crystals will be.
#DMT_recrystallization #DMT #recrystallization
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