12-21-03 05:52
No 478128
I've read the chapters on recrystallization in Zubrick, watched the video clip from the University of Hong Kong on recrystallization, and also read the posts on recrystallization, and this is what I was able to compile. I'm confident that this is a fairly accurate procedure, but if there are inconsistencies, then please make comments. Please note the inline questions, and also a question at the end.
Equipment required
600ml beaker
250ml filter flask
Isopropyl Alcohol (91%)
Acetone
Buchner funnel with vacuum filtration set up (500ml filter flask)
Watch glass
1)Add IPA to a clean 600ml beaker (say 400ml) and place this beaker on a hot plate and bring the IPA to a seady boil.
2)Add impure crystals to a clean 250ml filter flask. Remove the boiling IPA from the hot plate and add IPA slowly to the filter flask containing the impure crystals. Add just enough IPA to dissolve the crystals. Place the beaker containing the IPA back on the hot plate.
3)Place the flask containing the dissolved crystals on a hot plate and boil for 2-3 minutes (?, not sure about the boiling duration). If neccessary, add a small amount of boiling IPA to the flask if all crystals do not appear to be dissolved.
4)Remove the flask containing the dissolved crystals from the hot plate, place the watch glass over the mouth of the flask and allow the flask to completely cool.
5)Once the flask has cooled, vacuum filter the crystals with a buchner funnel. Wash the filter cake with acetone. Remove crystals and allow to dry under a lamp.
Zubrick mentions that if the dissolved crystal solution appears only slightly colored, then the use of activated charcoal is not needed. The chemist in the Chinese video uses activated charcoal, and it was obvious why he choose to since the dissolved crystal solution in the video looked dirty. Is the use of charcoal neccessary in the recrystallization of MDMA.HCl? Is this charcoal the same kind that you would use to grill some burgers on a Sunday afternoon? It's just carbon, right?
If charcoal is used, then you would actually need to filter the dissolved crystal solution twice. The first filtration is to remove the charcoal, and this must be performed in a beaker with a filter flask submerged in boiling water, same as the video describes. The second filtration is the same as step 5) from above.
(Daddy)
12-21-03 09:19
No 478139
3. Use an erlenmeyer filled with icewater, and hold it close above the container with the boiling IPA with the dissolved crystals in it. That way, if you hold it a bit tilded, the hot IPA vapours will condense on it's outside, and the fluid will roll off into a small beaker you keep under it.
When the small beaker has collected about 20% of the evaporated IPA, then you take the boiling IPA container off the hotplate. So you have now a superconcentrated solution in IPA, and let it now cool down. The time needed for this concluded when you read on the small beaker that about 20% of the motherload IPA was evaporated.
""Is the use of charcoal neccessary in the recrystallization of MDMA.HCl? Is this charcoal the same kind that you would use to grill some burgers on a Sunday afternoon? It's just carbon, right?""
Depends on the acumulated impurities, mostly roughly appraised by the color by a cook.
No, it's definitely ACTIVATED carbon, like also used in aquarium filters, thus obtainable in 1 liter sacks in aquarium shops, if you want it OTC.
The rest of the procedure is pretty well like you described, however to obtain the highest purity, you should repeat it another time, so 2x recrystallization. It depends also on the quantity of your to be recristalized crystals, the less, the more difficult to gain purity with more recrystalizations. LT/
WISDOMwillWIN
(Newbee)
12-22-03 02:10
No 478296
Thanks for the reply,
Using an erlenmyer flask filled with ice water is a good method to gauge the amount of evaporating IPA.
If I choose to use charcoal, then in Step 3) after the dissolved crystals have been boiling for a few minutes, remove the flask from the hot plate and add a small amount of charcoal, then place the flask back on the hot and allow it to continue boiling until 20% of the IPA has evaporated, after which the flask can be removed from the hot plate and filtered immediately in a beaker set up with a filtering flask partly submerged in boiling water, just like the video, right? The filtrate is collected and allowed to cool slowly (place the watch glass over the filter). Then, vacuum filter using a buchner funnel (step 5) and procede as usual
Looks ok?
PS: Does activated charcoal have a brand name in aquarium stores, or just wask for it name?
(Hive Addict)
12-22-03 10:22
No 478373
Add your charcoal before concentrating boil a minute then filter off and concentrate... The activated carbon is labeled as fish tank aquarium filter granules. Or activated carbon filter. It should have a pic on teh front or open the box flap it shuld look like little porous black rocks. The size of CaCl2 or chunky epsoms or usially slightly larger..
All stores carry different brands usually. Aqua tech is brand at wally world here. Just go to the super wally place or pet store and ask someone for activated carbon for recharging a filter.