Hi! I'm new here and there's so much to read that I really can't know for certain what has already been discussed, but this is interesting and important so I made a new topic. I posted it here since I don't seem to have the rights to start a new topic in a more suitable place...
By following this procedure you can make NaOH/NaCl solution at home using for example a DC power from your old computer, passive electrodes and table salt (without iodine, I don't know why it'd be a problem though, do you?):
http://en.wikipedia.org/...ess#Laboratory_procedureMy goal is to produce as pure crystals as possible from 2 kg's of acacia.
I've yet to try any tek so I'd need to know the suitable ones where this can be utilized.
What I was planning to do with my acacia without any knowledge about its effectiveness was something like this (I'm assuming that the DMT is totally in its acid form in the beginning and addition of solutions prior the step 8 doesn't change the situation):
1. Prepare NaOH/NaCl solution, and at the same time
2. Mix acacia powder with pure water in a glass jar leaving plenty of room, freeze and thaw it 2-3 times to break the remaining plant structures and speed up the next steps
3. Simmer over night
4. Filter off all solid material and wash it with pure water with half of the original volume in a Buchner funnel, store the solid material in a freezer just in case the final yield is unacceptably low
(5. Distill to concentrate the material, stop when a change in viscosity is seen and double the volume with pure water, the volumes are just my guesses)
6. Add dichloromethane to a warm filtrate solution, pour in to sep funnel, shake and turn vigorously and let the phases separate, discard the bottom phase, add more DCM, repeat until no material sets to the bottom and the DMC-phase seem more or less clear
(7. Distill the DCM for later use, use additional condenser attached to the collection flask to avoid exposure to toxic fumes and use a fan + open window or well ventilated space to minimize the health risk)
8. Add NAOh/NaCl solution until pH reaches 11
(9. Or let pH be 10, pour in to heavy wall round bottom flask, turn on the magnetic stirrer, warm up the solution to 40C but not higher since it would start to corrode the borosilicate glass, and vacuum distill the solution until a change in viscosity is seen)
10. Add pure naphta about half the volume of the original volume (again just my guess), raise the temp near to the boiling point, pour in to sep funnel and mix the phases with circular motion to avoid the formation of emulsion, continue until you become tired, allow the formation of two clear phases, discard the bottom phase
11. Pour in to glass jar (preferably borosilicate), put in to the freezer and let it stay there over night
12. Collect the fluffy stuff somehow from the surface. I don't know the best way but if you don't suggest otherwise, I would try this: Buchner funnel is also stored in the freezer O/N in a minigrip bad to avoid condensation. Before filtration, the filter paper is first wetted with cold naphta. The filtration is carried out as fast as possible
13. 1/4 of naphta (a guess) is distilled off and step 12 is repeated until the pulled crystals change color or appearance (I don't know anything about this, just guessing). Rest of the solution is distilled until only a minimal amount of liquid is left, which is needed to collect it from the round bottom flask. The solution is then dried and stored in the freezer and possibly added to the next batch.
14. Take a small amount of the crystal, put it in a small amount of hexane and evaporate it to get seed crystals
15. The crystals are gently tapped in to heptane and the filter paper is dropped in to heptane solution in another flask and the flask is rotated until the rotator is satisfied. The filter is then removed and placed in to the Buchner funnel and the solution is poured through it and combined with the other heptane solution.
16. Recrystallization step starts, of which I don't yet know much about but I try to say something to get more solid picture through corrections and suggestions: The hexane solution is heated up and activated charcoal is added. Our pharmacies sell white activated charcoal. I know people usually think that it just means very porous black coal, but this is actually white. I was thinking about testing it. Anyways, I don't know the amount needed, but it shouldn't matter since it is then filtered off and washed. I would store it and possibly add it to the evaporated leftovers from step 13.
17. The solution is allowed to cool to RT. If the solution becomes cloudy, more hexane is added. If it doesn't become cloudy, some of the hexane is distilled and the solution is very near its saturation/precipitation point.
18. Solution is pipetted in to a glass jar (or what would be the best option?) and the lid is replaced with a filter paper. The solution is allowed to stand over night and the seed crystal is added. The filter is reattached and the jar is allowed to be perfectly still until the solution seems to be gone. The temp is raised to 40 C or so to evaporate the rest before scraping and weighting. Any unnecessary air flow over the crystals is avoided to prevent oxidation.
I was also thinking that could I use an electrode instead of the seed crystal. If the product is in its freebase form, it should be attracted towards the cathode and coat it. This is a possibility at least with some non-aqueous solvents
http://en.wikipedia.org/...ectrophoretic_deposition The electrode could also reduce the freebase in to its acid form which doesn't seem to form crystals, but you never know if you don't test it.
Regarding this electrophoretic deposition, here's a nice page about it
http://people.bu.edu/str...master/silvergrowth.htmlCould you please comment on the idea and guide me to do a better job? I thank you all in advance!
P's