Freebase dark grey and solvent not rising to the top

[babagmn]

Just had the above issue.

I did a warm acid extract with phosphoric acid 3 times with about 1 litre and then boiled it down and added noah to basefy it. But when I added the benzene the benzene is not separating out. It seems to be mixed in with the free base.

What went wrong? Did I add too much lye? The pH went from 2/3 to 13/14.

Is there anything I can do to rescue this?

 

[babagmn]

Ok, I did a sample filtering and this helped a little bit. But while it was still alkaline. So I have a coffee filter full of table salt that is now black.


In order to filter while acidic, should I turn my soup back into an acidic solution with the addition of acid, filter it through salt and then turn it alkaline again, and then extract using nph?

This particular extraction has not gone as well as my first one did!!!

 

[drpotato]

i would like to point out the german word benzine can be interchanged with petroleum ether, or gasoline. Probably naptha.

Also, the presence of dust/silt is problematic, it can also create emulsions. after filtering make sure no acid or water used is tap water. try only using demineralized/distilled water afterwards if you get something that looks like emulsion bubble-skin that wont mix back into the solvent. salt is fine, the problem is things like calcium and other dissolved minerals that can react with bases to form a very inconvenient precipitation. filtering through proper filter paper is also advisable, or at least coffee filter. for best results, chill the solution so it warms up to room temp while it is filtering, this ensures the amount of precipitating solids is constantly decreasing not increasing, and makes the filter less likely to clog.

Lastly, your solution is probably black due to being riddled with dissolved metal phosphates from whatever the pot was that you boiled the soup down in. this can include chrome and is not healthy. using carbonate instead of hydroxide may yield different results. carbonate is an acceptable base if you are basifying filtered acid soup rather than pulling from the bark directly