mysterious emulsion/dmt precipitate

[acacian]

hey all

yesterday I had quite an interesting thing happen with an extraction. What was seemingly an emulsion formed and I am stumped as to how exactly.. and whether it is emulsion at all. I am extracting from some active acacia bark at the moment and I extracted via the following process:

. ground bark to fine fibers.. not quite powder
. boiled x 3 in ph 4 water
. combined boils and reduced to 500ml
. filtered twice with cotton balls
. defatted once with 175ml xylene
. converted to freebase by adding roughly 30g caustic soda dissolved in 150ml warm water (didn't have scales but added until it cloudded strongly with precipitates and then went black)
. added 200ml water with dissolved 1-2 tablespoons of rock salt to the soup
. added 100ml xylene .. now at this point the extraction started behaving very strange. whenever I turned the bottle over and mixed it, it seems all these light coloured bubbles kept rising to the top below the xylene layer. I continued to mix for a while and allowed the xylene to separate.. though the layer was still below the xylene. I pulled the xylene and added another 100ml and repeated the process. same thing again. So at this point I gave it a heat bath for around half an hr.. nothing. still there. I then proceeded to add anoter generous amount of base... still there. I then quickly evapped the xylene with a hair drier and was left with hardly anything. certainly nowhere near the amount that precipitated out upon basing..

this morning I looked at the bottle. the layer was not bubbly and just looked like precipitates. its not xylene as the remainder of the xylene that was emulsified cleared and sat on top and of course the other 80ml from the 2nd pull was already removed. so that seems to account for all the xylene leading me to think this isn't an emulsion but rather the spice.. I don't know what is causing this. I am using a differen't brand of caustic soda, and I am not sure whether rock salt was the right kind to use.

pics below:

 

[acacian]

also I am using a differen't brand or lye this time. I am wondering if that could be causing issues? the brand is "mechanix"

 

[acacian]

so i went and bought some of the normal lye I use..
my plan is to pull the precipitates, convert back to salt by washing in vinegar, adding a bit of water again and then re-basing with the other caustic soda and pulling again with xylene. I just remembered a similar thing happened with this last time I used the mechanix brand so hopefully this is where the problem lies. Thoughts?

 

[cyb]

Bizarre...

Are you sure the acacia was legit?
You've tried everything I would do...

Hmmm

BTW did you know you've got a big black monster roaming round your garden?

 

[acacian]

its definitely legit i've extracted from it many times. its a reliable species.. it smells strongly of dmt when i burn the bark and it precipitates like crazy when i add base. I have a feeling its the brand of caustic soda because i bought a different one when i came back to stay at my parents.. added the top layer of precipitates to vinegar and it theres still stuff floating around.. very strange

is there a possibility that other chemicals in certain brands of lye prevent alkaloids being able to mix with the non polar layer?

 

[Ambivalent]

i think the caustic soda is forming some thick sludge. and my assumption is that they add something to prevent missuse. something like this happened to me when i was extracting rue, and the precipitates got trapped in this viscous liquid, like gel and it was nearly immpossible to wash them. the only stated ingredients were sodium hydroxide and waterL(it was dissolved_, but it was not behaving as such.

i dont have a suggestion how to proceed. from here on, i think every salvage operation will be a bit messy and smelly,however you proceed. i hope you will get the goodies out.

 

[acacian]

i think the caustic soda is forming some thick sludge. and my assumption is that they add something to prevent missuse. something like this happened to me when i was extracting rue, and the precipitates got trapped in this viscous liquid, like gel and it was nearly immpossible to wash them. the only stated ingredients were sodium hydroxide and waterL(it was dissolved_, but it was not behaving as such.

i dont have a suggestion how to proceed. from here on, i think every salvage operation will be a bit messy and smelly,however you proceed. i hope you will get the goodies out.

yeha i was thinking the same thing... this brand is sold at the two major supermarkets after all. Even after shaking hard in vinegar theres still stuff floating around and I couldn't even dissolve it in acetone! the acetone sits on the top as if its like a non polar layer.. i bought some of the other caustic soda hoping i could convert the sludge back to salt and then rebase and pull but its not looking like that will even be a viable option because i dont know how to separate it :s

 

[infinitynlove]

hi

some people have good results with emulsions by combining a hot bath with some gentle vibration.

you could place your bottle under a cheep ladies vibrator (sealed in a beg etc) in a hot bath and leave it going for a wile and see if it makes any differance.... worth a try.

best of luck

 

[acacian]

already heat bathed it and even added more lye and salt. I recently strained the precipitates off and tried to salt them with vinegar.. the layer still sits on top! it wont even dissolve in acetone. i think there was somehting in the lye

 

[acacian]

so this is what was left after evapping the 2 xylene pulls.. its a gooey waxy texture. haven't weighed yet as I am lacking scales but it looks probably about a gram.. i have another pull evapping as we speak and i am going to rebase the vinegar which I tried to salt the emulsive layer with