One hasnt posted in a while but here goes.. 2 situations, same result in the wash

Situation 1
100 g bark acidified in 100 ml vinegar for 30 min

150 g lye dissolved in 500 ml water and added to bark mixture (a meter was never used to start but after 24 hrs ph was only 10)

to this solution another 1150 ml water was added for a total of 1750 ml (or 17.5 ml liquid per 1 gram bark...as its prepowdered and from experience wont separate unless more liquid than normally prescribed is used)

let to sit for ~ 12 hours

3 pulls of 100 ml, 100 and 50 mL naphtha yielded low results after 24 hr freeze precip (havent scaled it out yet, but it looks quite small)....

... so another pull of 100 mL was performed to see if anymore goodies could be obtained...

the pull separated from the basified liquid fine..

however when a pinch of Sodium Carbonate was dissolved in 50 mls water (as per usual) and added to the NP and shaken (again as per usual) crazy emulsions formed... one separated (keeping the emulsion layer) and washed 2 x more but the emulsions are still there

some 24 hrs later there is a clear yellow top layer (naphtha), a white bubbly middle layer (emulsions still there) and a light brownish bottom layer (wash water that was caught in the emulsions????)

This is the first time emulsions have formed during the wash stage for one and he is confused...

he has read that salt or more base breaks emulsions but he is not sure what to do....


Situation 2
after these emulsions formed during the wash one decided to do another small 50 g experiment....

50 g bark was added to 50 ml vinegar and 100 ml water and left to sit for an hour in a warm water bath

125 g lye, dissolved in 500 ml water was then added to acidified solution ...

along with another 350 ml water to bring the total liquid to 20 ml per 1 g bark .... the pH was 13 (pH meter was used this time)

(one finds that anywhere from 15 to 20 ml liquid is required for his prepowdered bark to separate from his NP solvent))

.. this basic solution was left to sit for an hour

after an hour 3 pulls of 50 ml each (again using naphtha) was performed ...

as always, for one, a sodium carb wash was performed (pinch of Sod Carb disolved in 25 ml water, added to NP and shaken)....

however once again emulsions formed (this is only the 2nd time this has happened.. and it happened in less than 6 hours)



Questions
This is the first time one used Reverse Osmosis water for extraction/washes (tho distilled water was used before)... could this be responsible for the emulsions created during the wash?

One has read both more base and adding salt removes emulsions... what should he do? (heat doesnt seem to touch these emulsions as it usually does)

Edit... Well one is going to try adding some salt water to the wash / NP in the first situation to see if it works.. he will post his results as the occur..


Thanks in advance for any replies...
The Dude

sorry to double post but..
thank you thank you thank you... to all those who contribute to this site


a single pinch of (unmeasured) salt to the NP, emulsions and left over water in Situation 1 ...

create an INSTANT fix!

emulsions disappeared instantly! leaving a distinct line between the two layers!


....


Now onto situation 2's mess (fingers crossed for the same results!)

again.. sorry to double post (or i guess triple post) but...
in situation 2

an unmeasured amount of salt was added to the NP, emulsion and lower brown (presumably water layer)..

and an instant separation occurred!!!

.. will post with final results...



Never underestimate the power of coarse (un iodized salt) salt!

Amazing results!!!! Thanks again everyone!!!

Re Situation 1:
You can't go wrong adding more lye - pH 10 is too low

L

all the goodies were in the NP/wash/nasty emulsion mix ...

can you add base to this? (tho one didnt need to as adding salt worked amazingly!)

If I may ask, what is the purpose of the vinegar presoak?
And are you sure on that pH? That much lye should have taken you way past pH 14.

My imaginary simian friend, Pithecus Trog, recently performed his first sodium carbonate wash and was happy with the results, but he too experienced the same three layers. He was decanting a fairly large amount of solvent however, so he temporarily disregarded the foamy layer, and took only the clean naphtha layer for his evap/freeze precip. He then collected the foamy layer from his several quart jars, and combined them into one jar separate from the dirty sodium carbonate wash. He covered this and let it settle for a few days, and found that most the foam dissolved into, again, a top layer of naphtha and a small bottom layer for emulsion.

He was able to take all but a negligible amount of the solvent from the mix, and just dumped the small amount of emulsion left over. But it seems that perhaps if one were to add a bit of naphtha to a jar with the foamy emulsion, one could break it down further, if needed.

RE: AlexanderD
- try adding a pinch of salt to the mix... broke one's emulsions instantly

RE: Noman
as per the vinegar presoak
- one read the blab and liked the idea of this soak, though others have said it is unnecessary. A/B experiments were ones first, where an acid soak is critical, so he just kinda carried it over to this hybrid stb

as per the pH.
- the pH meter was calibrated right before measuring the solution, using a standard pH 10 solution...
..but that doesnt mean the meter is reading correctly.. the solution was actually 12.9 but he rounded up for simplicity

- how would one go about calculating the amount of lye needed to neutralize the acetic acid found in x ml's of vinegar?


Thanks for the replies,

The Dude