separatory funnel users, please help!

[hamhurricane]

I have a 1 liter sep funnel and yesterday i attempted the noman tek with 5 grams of MHRB, the first problem i ran into was i did not have powdered bark and my food processor did an insufficient job of pulverizing it (although most of it was broken into powder and lots fluffy pube like strands.) when pouring the sodium hydroxide/MHRB/water solution into the funnel i did the best i could to leave the sediment out of the funnel but it kept making it inside no matter how careful i was, and forming a hard plug that prevented the passaged of liquid. i would then need to pour everything out clean the funnel and start again over and over and over. the only solution i could figure out was to keep draining the funnel so that the blockage could not form and to only give the liquid about one minute to separate, the yields from this extraction were extremely low.
Another sep funnel question, how clear do you want the naptha solution to be, once i drained out all the basified water the naptha would form a gradation from orangish to clear, i would keep draining and only save the clearest portion, was i loosing DMT? Also i used a little extra naptha because i thought it was a bit safer (about 60ml per pull) if one chooses to do this must you then let it evaporate down somewhat before attempting to crystalize?


Can anyone suggest a better way to remove sediment before the noman tek, or give some tips and or tricks for sep funnel usage?

 

[Entropymancer]

You need to run the liquid through a coffee filters a few times if you don't want to plug the stopcock on your sep funnel. Get all the particulates out that you can.

 

[Entropymancer]

Another sep funnel question, how clear do you want the naptha solution to be, once i drained out all the basified water the naptha would form a gradation from orangish to clear, i would keep draining and only save the clearest portion, was i loosing DMT?

Yes, you were draining off DMT most likely. If you want to seperate out the clearest fraction, that's fine, but you still want to save all of you nonpolar solvent.

Also i used a little extra naptha because i thought it was a bit safer (about 60ml per pull) if one chooses to do this must you then let it evaporate down somewhat before attempting to crystalize?

That depends entirely on how saturated your naphtha got. Chances are, you'll need to reduce it. It's often best to let it reduce until you see seeds of crystals forming, regardless of whetehr you used extra naphtha or not.

 

[hamhurricane]

thank you very much for your help Entropymancer!

so can you help me revise the noman tek? 50 grams of MHRB should yield about 250mg correct? so what if i were to take 50 grams boil it in about 750ml of water for an hour to create a DMTea, filter the tea through a cotton t-shirt, then compensate for evaporation so as to bring the water volume back to 750ml then basify with 15 grams of sodium hydroxide, add naptha and begin the separation...
would a single t-shirt filtering be enough, or should a coffee filtering be done as well. and would a one hour boiling at neutral PH extract the DMT into the water enough to have a proper yield?

 

[Entropymancer]

would a single t-shirt filtering be enough, or should a coffee filtering be done as well?

Definitely filter it through a coffee filter as well as the t-shirt. You don't want to be building up sediment on the inside of the stopcock.

and would a one hour boiling at neutral PH extract the DMT into the water enough to have a proper yield?

Unfortunately not. In order to be properly soluble in water, you need to make a salt of the DMT (i.e. do an acidified extraction). Also, due to partition coefficients, you generally can't get 100% of a chemical with a single extraction.

A seperatory funnel isn't really helpful for pulling DMT with a straight-to-base extraction. It is useful in doing a sodium carbonate wash of the nonpolar solvent once you've extracted.

But if you want to use the seperatory funnel throughout, you'll have to go the acid/base route. Marsofold's is very consistent, and Coschi's looks good as well.

 

[Volvox]

thanks for that last post and this thread. My friend swim was about to get one but on the fence and swim thinks he is going to wait now as he does STB and this seems like overkill. Maybe a tiny cheap one for the SC wash, but not a biggon for the separation. Thanks!