brown goo at bottom of stb extraction

[manicorganic]

Swim tried his first spice extraction a few days ago. Used 500 grams MLRB, 2L of distilled h20, 250 grams lye. 400 ml naptha. Any way the result after 1`st and 2`nd pull of naptha was put in freezer for 24 hrs when it was taken out the sides and bottom of jar were covered in pure white goodness but under the bottom layer of white was a layer of brownish goo. My best guess is that the brown goo was due to a combo using very fine pre powdered bark and shaking the hell out of the jug insted of just turning it. I know none of the bark base layer got into the mix so that is my best guess.
As an experiment i took a half gram of the brown goo (dried to brownish powder) and added it to 50 ml of water based to 12.5 ph added 30ml naptha and let it sit over night. Eveperated the naptha and it came back with .3 grams of white powder

but it had a bit of a lite blue color to it. Almost the color of the colman fule i use. Could this be because of the impure colman or ........(other ideas)

 

[manicorganic]

Swim put 2 grams in vinager/water ph`ed to 2. Shook it up for a few hours and then added lye to bring it back up to ph 12.5. Added naptha and have let it sit for about a day. I now have three different layers a dark watery layer on bottom a lighter kinda thick layer in the middle and a nice yellow layer of naptha on top. Swim is Going to pull naptha layer tomarrow and air evep to see what comes back. So far swim has only sampled the pure white crystal that he must say is far better quality that what he has tried before in the few times he has had the chance to sample the rare spice. AFOAF did try the brown dust even after the disclaimer of impurity and said he was happy with the results. To each there own. Looks scarry to me.

Will post results of a/b extraction on brown stuff.

 

[endlessness]

Dont shake the hell out of it. What color was the naphtha when you separated?

When you added the water to that, what happened with the brown goo, did it get dissolved in the water or?

You can also try doing sodium carbonate washes after pulling and before freeze precipitation, maybe that helps.

As for the 3 layers thing, thats called an emulsion. Check the FAQ for how to solve that.

I have two guesses regarding the brown goo: Either its dmt+impurities (like, plant oils and other things), or it can also be small droplets of the mimosa solution that came across, even if you think you didnt get any of the basified liquid, and once that settled it went to the bottom. More careful mixing and separation, doing sodium carbonate washes or recrystallization should help cleaning that up.

good luck

 

[CraigRap]

AFOAF is very interested in your results as he's getting the same brown stuff (after 1 hour in the freezer).

Sodium Carbonate washes sound interesting ... what are the volumes?

See the brown goo ....

 

[manicorganic]

The brown powder disoved in the base water almost at once. Turned the water into a hot coco looking mix. Seemed to be much cleaner than the start product but like i said had a bit of a light blue color to it. The a/b clean up worked much better first pull was nothing but pure white crystals going to do a few more pulls on it and check the faq for the solution to the elmultion problem (if it is a problem). Want to find out how pure this brown nasty is. If swim get 50% goodness back swim will see it as sucsessful and extract all the brown with a/b tek. Then will start trying To clean it up more with wash and or recrystalliation . And yes that is the same brown goo i got craig. Dont throw it out. Lots of goodies left in that junk. Thanks for the help.

 

[CraigRap]

Dont throw it out. Lots of goodies left in that junk.

Hmmm can too high a PH destroy spice?
SWIM acidified,defatted and then basified.
The first pull looked a bit yellow ... carbonate wash and evap'd
All that was left was a bit of clear oil ... was BAD!!!!

Don't know where to go from here ...

The picture shows the re-basified goo waiting for the second pull ... can't see any point in doing that one.

 

[endlessness]

High pH cannot destroy spice

Why evaporating instead of freeze precipitating? I suggest redissolving that oil in warm naphtha and freezing for crystals.

 

[CraigRap]

I suggest redissolving that oil in warm naphtha and freezing for crystals.

Now I'm confused :?

SWIM said that he can't get the PH high enough (at 11). No matter how much NaOH added. Perhaps the PH meter? He even waited for the solution to cool first BUT (and this is the confusing bit) if water is added then the PH goes up. Mor water, the higher it goes. Up to 13 now but VERY dilute ... that orange solution got out into a pot (ran out of room) and then split again amd dilued even more ... it's nearly colourless.

If what SWIM is telling me is true, then this defies my memory of 1st year college Chemistry.

Or ....... Is it SWIM's cheap PH meter?