zorilla, I’m going to try and be as clear as I can here. After you finish your rxn you take your honey and dilute with 5 times it’s volume of DH2O, I assume you did this. Now, you should your honey first this but I’m not going there right now because that’s not where your immediate problem lies. After cleaning the honey you add 200ml of your NP of choice, then you add a lye base solution to this mixture raising the PH to 13. You said you did this so you are with me so far, right??
Anyway, you stir this up gently and let it set for 15 to 30 minutes then….now listen very carefully to what I’m about to say, you take the TOP LAYER, THE ONE WITH THE NAPTHA and use that for your titration. Now SWID has never used Naphtha but, unless he is mistaken, it floats on TOP of water, not on the bottom. The product in the honey/based solution moves to the top layer, into the NP, when you get the PH above 13. From your reply to my question you stated you collected the BOTTOM layer which happens to be the layer with the freebase in it! Of course you not going to get any separation of layers, you added water with acid to water with lye….guess what water and water DON’T separate! I hope you kept the naphtha that you removed from the base solution, you can take that and citrate it to recover some of your product.
However, all is not lost! Take the aqueous solution, you know the water/lye with water stuff you just made, and add more lye solution to it to raise the PH above 13 again. Understand this, you have added acid to this solution so it will take a little doing to get the PH up but you can do it. Also, you should be prepared, because of this total brain fart on your part you are going to lose some of the product you could have otherwise recovered if this had not happened. Don’t be surprised if you only get 30%, maybe 40% back if you are lucky on the E you invested.
Here’s a link for something I think you should read, it will save you a lot of heartache in the future. Copy the link and post it in your browser address bar and it will take you there. Good Luck!
Post 428410
(geezmeister: "The post-reaction workup: a cook's summary", Stimulants)