techcruncher said:
thanks! so just add to some low ph water then basify again?
69ron said:
There's no telling what kind of crap is now in it.
Do a small scale A/B extraction on the spice, and then a freeze precipitation. That should purify it pretty well.
Suggestions:
First you might try just doing a recrystalization from what you've got, and see what you can come up with. Completely disolve the questionable product in some 150F Heptane, just enough to get dissolution. Slowly cool it to room temp. While doing so, if you detect a layer of gunk distinguishable from the clear part, remove it with an eye-dropper. Then put it in the freezer, overnight. Hopefully you'll have some crystals, pour off the solvent onto a glass plate. Repeat if thought helpful. Some of any contaminates may be removed.
And/or, go for a fullblown A/B like 69ron is saying.
Here's some suggestions for what you could do:
1. Completely disolve the product in a solution of water and vinigar at a PH around 3.
1a(option). wash the water solution in VMP naptha, seperate it and discard the Naptha.
1b(option2). wash the solution in xylene, and then discard the xylene. Then wash the solution in Naptha, and then discard the naptha.
1c(option3). Heat the remaining (acid) water solution (for an hour or so), by a double boiler method (uncovered), in boiling water, to remove any possible volotiles that could be part of the suspected contaminants. (and then let it cool to room temp!) before you-
2. Basify the solution to a PH of 12.5.
3. Do a pull with VMP naptha from the basified solution. Seperate it and collect it. Do another pull with heptane. Seperate it and collect it. Do a third heptane pull etc... On your final pull you can seperate a small amount of solvent and quickly evap it and see if your still getting anything.
Now discard the (basified) water solution.
4. Wash the Naptha and Heptane solvents you've collected in water basified to 10-12.5. That's to remove any remaining water soluables (like soap, detergent etc...). Seperate and toss the water layer.
(each wash/pull can be repeated as you think needed if you want to be hardcore.)
5. Put the final solvents that you've collected and washed in a dish and evap them down to a minute layer. If you see a "film" developing on the surface, that's it.
6. Cover the dish and put it in the freezer overnight. See if you have any crystals. pour off the solvent.
7. report your findings....
(allow plenty of time for your layers to completely seperate, since your solutions will be concentrates, to avoid loss, be meticulous.) Use a sep funnel!
Or you could dissolve the questionable product in Heptane, and then wash the Heptane in basified water several times (to remove water soluables ie... detergent)...and then recrystalize (as above, elsewhere on this forum)...skipping a full blown A/B...
Live long and prosper.