I did add more naptha. It sat on top until I shook it and now it all looks like solid black again. I don't see how they aren't separating either because one is non-polar and the other is polar, and they have different densities as well. How can they not separate?

Mimosa really likes to form emulsions.

When you say "shake it", do you mean like a moderate swirling, or like actual shaking? I've seen some teks that say "shake vigorously"... this is not what you want to do!

The problem is that the aqueous phase isn't sufficiently polar. You need to increase the ionic strength of your solution. Try adding a whole bunch of salt (non-Iodized) (30 gram per liter of water if you want to be precise... adding too much is no problem at all, so no worries there), and warming the mixture up. This should help the seperation go much more quickly. If you just wait for it to seperate, it will take days.

The conventional wisdom here is that you need more lye, but as 69Ron has pointed out, that makes no sense; the only benefit that the lye can be providing is increasing the ionic strength of the solution. This is much cheaper to do with salt than lye.

SWIM says you cant shake it. theres SWIY problem... Hardcore emulsion. If SWIY shook the shit out of it then SWIY is gonna have emulsion that may never go down. and it will seem all black. SWIM not sure but swim believes swiy should add more base.. NOT DIRECTLY!! Dissolve in some distilled water in separate jar, using the same ratio but cut it in half, even a quarter if swiy wants. wait for it to cool(important) then add it to your mix and let it sit. STIR GENTLY OR Gently turn end over end, being careful not to splash, for a couple min or so. SWIY then just needs to let it sit and leave alone for awhile. SWIY should see what he saw before as the emulsion goes away. FYI theres better info on some other posts. look around.

Well said man! See that does make sense. Like I said Swim is inexperienced...

Yeah, but my friend has tried it with 60g salt added per liter and there are still horrible emulsions to deal with until at least pH 13 is achieved.
Once one hits 13, you can shake the shit out of it and there's no emulsion at all.

Damn, really? My friend was thinking about trying to develope a lye-free process, since it's such a watched chemical with the "fight against meth" these days. He still has access to sodium hydoxide that can be bought w/ cash, would like to be able to break the MHRB extractor's dependence on this caustic base.

Maybe by saturating the solution with salt after an aqueous acidic extract, a defat might net more impurities and decrease the emulsions?

So adding salt or more base should fix the problem? I have already added a lot of base. I don't know if there is a point where there is too much.

Added lots of non-iodized salt and still can not see any layers. What's going on?

You have an emulsion. You're trying to break that emulsion. Have you tried warming the stuff up yet?

No I haven't had time yet. But isn't the emulsion the foamy layer that sits on top when it separates into layers? Cause mine has no layers, just all black

An emulsion is anytime the layers won't seperate. It's like freshly shaken Italian dressing. The layers don't yet appear seperate, because all the nonpolar liquid is trapped in suspension in the water.

If you're using an STB tek and there's no separation at all, your problem is probably not enough water rather than not enough lye. All that lye in STB's can tend to reduce the bark to a gummy sludge that traps the solvent. The foamy emulsions on top that you're talking about happen with A/B's and are a result of under basification, but they don't happen with STB's - you get these super emulsions instead. Happily, the solution is to simply add an equal quantity of warm water to your solution and some more solvent and agitate gently. The solvent should pop right up to the top.



Noble goal - and one my friend has been reaching for as well. See this discussion that an associate of mine was involved in over at Drugs Forum:
http://www.drugs-forum.c...m/showthread.php?t=60035

Another clean up possibility that the Antarctican is looking into is a jello or egg white clarification of the acid solution before basification. This is the same concept as the procedure for clarifying consommé - mix the adjunct into a cold solution and slowly heat it up. As the gelatin (or albumen) coagulates, it sweeps up undissolved impurities in the solution and can then be strained out.
Maybe by removing the majority of those proteins (he suspects that proteins are the main thing holding these emulsions together) basification can happen at a lower pH without the problems and low yields.

Adding more water and solvent broke the emulsion right away, but I lost my syringe... oh well

So frustrating. It separated into layers but now only a tiny bit of naptha sits on top, not nearly as much as should be there after many hours

You could very gently turn it end over end. Cuz the naptha couldn't have gone anywhere. It's probly just trapped in the basified mix. Just dont shake the shit out of it.. lol

That's what I've been doing. I just don't get it. Only about one tenth of the napthat that should be on the top is. Why is the rest stuck?

Hmmm really? Thats strange. Have you tried a warm water bath? That could possibly help it out a little. And if that dont bring more up then just pull what you got there, evap it and see what you got... If nothing then dont worry cuz all the good stuff is still in the jar. Keep searchin for other info. scroll thru some other forums see if anyone knows there. thats the great thing about the web

It has been in a warm water bath for a few hours. Doesn't seem to help it. I will try to search around a little

hey could be that you are using a really crappy naphtha? i had that happening to me with a certain brand that i bought from a chinese shop.

Yeah thats what i thought too but, i asked him and he's using VM&P, which seems to be a popular one.