Too little lye to continue Cybs Tek

[FiniteFox]

Fellow Travellers,

Here is the deal. I had some ~250g of ACRB laying around and wanted to experiment.

I started extracting 250 g of ACRB using Cybs salt tek.
I added 600 ml of vinegar, 400 of water and then froze/thawed the mix 4x times. Then I added salt (~180 g?) but noticed that I only had 200 g of lye left.

So I drafted off 20% of the mix (so approximately 50g of ACRB) to another bottle and basified it with lime, shifting it a q21q21 extraction with lime.

The rest (the ~200 g) I basified with lye and moved on with the Cybs tek.

Now I'm doing my nap pulls from the cyb's batch except the nap is pretty dirty. (The ACRB was really pulverized during powdering and the freeze/thaws made it moreso). I'd just do a clean up as the tek suggests with lye, but I'm out and its tricky for me to get more. I've let it settle and can decant pretty clean looking nap away from a blackish ink sediment at the bottom.

Question 1: Any way I can clean up my naptha without lye? Maybe I can do a freeze precip an then do some kind of washing?

Question 2: I have a mad emulsion going on with my Q21Q21 tek. I added some extra water to it early on so that the limonine would near the neck of the bottle and easier to pull off, but could the extra water and salt be messing with it? I've let it settle for over a week and still quite ... emulsed. See attached pic.

Thanks!

 

[FiniteFox]

A little commentary on the above pic:

There is the bottom layer with the bark; the middle layer of added water; the top layer of D-limo and gunk emulsified into it. Its hard to tell, but the top layer is only a half inch so the line of separation is obscured by the threads on the neck of the jar.

 

[Godsmacker]

How long after mixing solvents did you take that picture? As a rule of thumb, if anything funky happens with nps layer (i.e. emulsions, etc), I either let it sit overnight, pipette the solvent into another (water-free) container and let it sit overnight, or re-agitate the layers and wait.

Also, adding 200 grams of sodium hydroxide to a litre of water will get it far beyond the minimum amount of basification needed to pull DMT from it (in fact, I have never used this amount of lye in a single extraction in my life. I find that adding as little as 30-50g to a litre of acidic water can get the ph to shoot up to 13 in a jiff). You should be fine with regards to lye.

If I were you, I would look up how to get rid of emulsions via google or just wait an hour to a day or so to let it separate on its own. IME I always get emulsions when I work with powdered bark and find that it takes much longer for the layers to separate.

Personally I don't really think cleaning nap with lye would do anything. NaOH isn't soluble in non polar solvents and by shaking up nps with heavily basified water as you did so already you've already done exactly what a lye wash could do. If you're still getting emulsions after adding 200 grams of lye, I highly doubt that adding moar lye could help at all.

One technique i use for emulsions is letting pressure escape from the vessel (i.e. opening up cap and letting it stay open as they separate, lightly tap sides of glass where emulsion is in the hopes that the trapped bubbles can rise to the surface and things can start moving again). Again, google and all the organic chemistry info she holds is your best friend at this point.

If this still doesnt work with your emulsion or dirty nps, i'd suggest making some sodium carbonate, diluting it with H2O to make a solution with ph greater than 10, wash the dirty solvent with this a couple times, separate layers. To the cleaned nps with goodies in it, i'd do an acid wash with a solution of fumaric acid dissolved in water (enough fumaric acid to lower ph to 4-6 and sufficiently salt/absorb alkaloids). After a few shakings up, separate layers and add sodium carbonate to dmt-water-fumaric acid solution until the ph hits 10-11. At this point you can either A) evaporate water and recrystallize/purify DMT via acetone
B)pull DMT from basic solution with nps and proceed to collect goodies from there on

I hope that this was of help to you and that the spice gods bless you with goads of DMT