The latest Modified EZ-Tek method (Jan 2025).
I keep refining the technique as I find improvements to this simple method, no extra steps, truly a EZ-tek.
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Starting with 250gms funneled into an 2000ml ERL, Pre-Mix 50gms of Sodium Hydroxide (100% LYE - Caution: Caustic!!) into a liter of water. This should make a sludgy solution. If it’s too thick, (and it probably will be) add up to 350ml of water. Total volume in big ERL should now be ~1600ml. (This level is important to note so that you are aware of how much solvent to extract, you should be coming back to this level once the solvent separates in later steps. Use a Sharpie to mark this level.)
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Monitor while bringing ERL up to 120° (This heating step is OPTIONAL. Dimitri’s melting point is 115°) and stirring at a moderate speed for 45 min to 1 hour.
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Turn off the heat and allow the temp to drop to under 100°. (or remain at room temp, if no heat was used in the previous step.)
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Add naphtha in an amount equal to what will be held in your crystallization vessel (I like to use 2 jars with very flat sides. Allow 100ml+ per expected gram of yield). Next, stopper the ERL and shake vigorously for 30 to 60 seconds, ensuring a good mix. Next, allow to settle for ~1 hour or until the solvent separates 95-100%.
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// A frequently encountered issue at this stage is emulsification. To break it you must make the sludge heavier. Add salt and remix. It may take a large amount, I recommend popcorn salt because of the quick water solubility due to the ultra-fine grains. Agitate or stir gently to finalize the separation. Patience, because it STILL takes time.
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Important secret step for a 1-pull full extraction. Repeat the previous shake/wait steps three times in a row. You could go four times. (If you want pure white crystals, pull and precipitate 1 time with fresh naphtha, then repeat the shake/wait 2-3 more times for the final extraction.)
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Some people will use a siphon tube or vacuum pump and filter paper to extract the solvent from the sludge cleanly and put it in your crystallization jars. However you manage to isolate the solvent, there will ALWAYS be a tiny loss. Remember, you’re trying to get all of the solvent out as cleanly as you possibly can, and leave every bit of that 1600ml of sludge behind. You may have to use alternate glassware to pour them back and forth to reduce sludge and leave the solvent behind. This can be tedious, think about effort vs impact on yield and stop at some point.
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Seal the jars and Freeze precipitate for 8 to 12 hours. It is best to isolate it and avoid movement, allowing for the possibility of larger crystal formation. During the initial stages of freeze precipitation, the solvent will become extremely cloudy, and at the end of the precipitation will be clear again (and typically stained yellow).
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If for some reason you have in ended up with contamination ( sludge ), don’t sweat. Wait for it to dry completely then dump the crystals and contamination into filter paper and rinse with water. Dimitri is not water soluble and this will wash the sludge away and leave it with perfectly clean crystals.
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If you didn’t do the 3+ shake/wait steps, you’ll need to repeat them 2-3 times to complete the final extraction. Hope you get all your solvent back AND 2% yield!
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Quickly and carefully pour off the solvent, being careful not to transfer out any floating crystals. Some people like to use filter paper during this step.
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Be sure to do the previous step as quickly as possible and replace the lid - keep each frozen crystallization vessel sealed to reduce water contamination through condensation.
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Once the crystallization jar reaches room temperature reopen it and drain off the last drops of the naphtha. Allow the crystals to dry for 1.5 hrs in a well-ventilated place. Try not to scrape too early. It should be allowed to dry completely before packaging. Add a silica gel bag to keep it dry.
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