Ethnochemist
Rising Star
So swim followed the basing technique in the pdf given here.
SWIM's just curious. He mentioned this in another thread, but just wants to provide background for this one. He dissolved about 1 gram of fairly pure dmt-fumarate in approx. 25ml of warm tap water. He then mixed 2 grams of sodium carbonate into 15ml of tap water and added that to the fumarate solution.
NOTE: The dmt-fumarate still smelled mildly of xylene, so there are definitely traces of it in the solution (swim probably should have done more acetone washes).
The solution was at first, as expected, very milky. But after 1 day, the crystals don't look like something recognizable. On the bottom there are brown blobs that resemble caviar. The solution is a little bit clearer, these blobs are growing on the sides of the test tube and seem to just float in solution, swim's wondering if anymore will even settle. As a test, swim took a spatula and scraped some down the side of the tube, they didn't move very much. The spatula was taken out and had very sticky/slippery liquid on it, after about 10 min, it was much drier and there was a considerable amount of crystals on the spatula.
He should probably be getting needle-like crystals at least somewhat forming in the solution, but all swim is getting is these blobs. SWIM wants to wait one more day to see if more crystals will form and settle, otherwise he's moving to plan B, which invokes some more questions.
He wants to then just use a non-polar solvent to get out all the freebase. He has naphtha and xylene available to him at the moment. He wants to use naphtha because it's easier to evaporate (he doesn't want to use a freezer btw); however, naphtha does not pick up all the other alkaloids like J. Spice and the Oxides. But if he has to, he might have to use Xylene, but xylene is very annoying to evaporate...even if it's only ~100ml.
Worst case scenario is that he has to evaporate the Xylene (water bath, fan and all), which swim can deal with, but would prefer to avoid in all circumstances.
SWIM had one more question though. SWIM has 8um filter paper. It's been sitting for a day, so some crystals have formed, and swim assumes that almost everything should be bigger than 8um. Could swim just filter it now? (or tomorrow, giving it 2 days to crystalize). Then put the filter paper in the oven at 120F until the water goes away....then just run acetone through the filter? Hopefully the Na2CO3 will stay on the filter paper (actually, swim doesn't think it would matter anyway, Na2CO3 won't evaporate when vaporizing), and the goods come out the other side. SWIM has no problem evaporating acetone. SWIM's a little worried about the actual filtering. He doesn't have a vacuum, and swim is worried that toward the end it will be a large gel collection that won't filter through, meaning more oven time.
Thanks for the help,
E.C.
7) dissolve the alkaloid-fumarate salts in 5ml of tap water, then and then add saturated sodium carbonate to make the solution basic. The alkaloids will be freebased and the solution will become milky. In 3 days they will precipitate out forming nice needle-like crystal in the basic solution. At this stage, one can filter the solution (nasty procedure since the crystals tend to be sticky and waxy) and retrieve any left alkaloids by dissolving them in acetone.
SWIM's just curious. He mentioned this in another thread, but just wants to provide background for this one. He dissolved about 1 gram of fairly pure dmt-fumarate in approx. 25ml of warm tap water. He then mixed 2 grams of sodium carbonate into 15ml of tap water and added that to the fumarate solution.
NOTE: The dmt-fumarate still smelled mildly of xylene, so there are definitely traces of it in the solution (swim probably should have done more acetone washes).
The solution was at first, as expected, very milky. But after 1 day, the crystals don't look like something recognizable. On the bottom there are brown blobs that resemble caviar. The solution is a little bit clearer, these blobs are growing on the sides of the test tube and seem to just float in solution, swim's wondering if anymore will even settle. As a test, swim took a spatula and scraped some down the side of the tube, they didn't move very much. The spatula was taken out and had very sticky/slippery liquid on it, after about 10 min, it was much drier and there was a considerable amount of crystals on the spatula.
He should probably be getting needle-like crystals at least somewhat forming in the solution, but all swim is getting is these blobs. SWIM wants to wait one more day to see if more crystals will form and settle, otherwise he's moving to plan B, which invokes some more questions.
He wants to then just use a non-polar solvent to get out all the freebase. He has naphtha and xylene available to him at the moment. He wants to use naphtha because it's easier to evaporate (he doesn't want to use a freezer btw); however, naphtha does not pick up all the other alkaloids like J. Spice and the Oxides. But if he has to, he might have to use Xylene, but xylene is very annoying to evaporate...even if it's only ~100ml.
Worst case scenario is that he has to evaporate the Xylene (water bath, fan and all), which swim can deal with, but would prefer to avoid in all circumstances.
SWIM had one more question though. SWIM has 8um filter paper. It's been sitting for a day, so some crystals have formed, and swim assumes that almost everything should be bigger than 8um. Could swim just filter it now? (or tomorrow, giving it 2 days to crystalize). Then put the filter paper in the oven at 120F until the water goes away....then just run acetone through the filter? Hopefully the Na2CO3 will stay on the filter paper (actually, swim doesn't think it would matter anyway, Na2CO3 won't evaporate when vaporizing), and the goods come out the other side. SWIM has no problem evaporating acetone. SWIM's a little worried about the actual filtering. He doesn't have a vacuum, and swim is worried that toward the end it will be a large gel collection that won't filter through, meaning more oven time.
Thanks for the help,
E.C.