What's going on here? (pictures included)

[rudder]

At the preliminary defatting stage with some big jars with 300g each of bark powder. Vinegar, vodka, and a little water was used for the acid cook. The pot was simmered for about 3 hours, then poured back evenly into both jars. 250mL of naphtha was added to each jar (500mL total). This was stirred/rotated, and consquently heated by the hot, acidic plant soup, and then left overnight.

The next day, the jars were stirred again then left for 24 more hours. Today, the jars had separated into what looks like three layers:

1)Bottom layer clearly looks like bark powder
2)Middle layer looks like a dark liquid
3)Top layer looks like bark powder mixed with the naphtha

It's that top layer that I'm mostly worried about. Ideally I would just see 250mL of Naptha in the top layer, unless it's extremely fatty, and even then I don't see why bark would be trapped in that layer especially with a liquid layer below it, and then another layer of bark powder below the liquid layer.

 

[rudder]

Ok so the top layer is about 250mL thick, which basically matches the amount of naphtha added to each jar...BUT there is a lot of other stuff floating in it, and I'm not convinced that it is entirely plant fats/oil, so here are some pictures so more experienced people can tell me what's going on here, and what should be done. Hopefully just decant the top 250mL layer - plant gunk and all.

(Each line on the jars corresponds to an increment of 250mL)

 

[trooth seeker]

Hey Rudder, Did you basify your mixture? From what you described you may have to add some lye or other base to the mix. Just a thought... Happy Extracions:d

 

[rudder]

NO I didn't nor did I intend to yet. This is a preliminary defat step.
The why and the how are covered in this thread, which I recommend:

DMT Extraction Overview - FAQ - All your basic questions and answers - Welcome to the DMT-Nexus

 

[Jorkest]

its possible the alcohol is causing this...

if there was any alcohol left from the boil...it could be mixing with the solvent layer..bring over all sorts of fun stuff

 

[rudder]

I somehow doubt that's what's happening, since the alcohol is usually the first thing to evaporate, and since the top layer is equal to the amount of naphtha that was added.

Maybe it's just some sort of emulsion? would it hurt to add salt at this point?

 

[Ambivalent]

looks like trapped material in emulsion layer, usualy thats what forms in between the solvent and the mhrb soup. have you checked your ph, maybe you still need to put it down a bit and it will help dissolving that stuff. add salt to try to break that layer also. looks like it was caused by emulsion to me. good luck and report further results.

 

[rudder]

Shouldn't be an acid problem since a very generous amount of vinegar was used. Will try salting and stirring lightly. Thanks.

 

[The Day Tripper]

I somehow doubt that's what's happening, since the alcohol is usually the first thing to evaporate, and since the top layer is equal to the amount of naphtha that was added.

Maybe it's just some sort of emulsion? would it hurt to add salt at this point?

Depending on how much alcohol you used there could still be a significant amount in the concentrated tea. You really don't want a solvent that mixes with both your polar and NP during a defat, or any stage of a liquid/liquid a/b. I would avoid using it in the first place. Most may have boiled off, but not all of it. There will still be alcohol in that solution until you fully evaporate it.

Salt is a good thing to try at this point, but in the future i wouldn't use alcohol in your acid cooks, it doesn't really serve any purpose and can cause problems later on.

 

[rudder]

I somehow doubt that's what's happening, since the alcohol is usually the first thing to evaporate, and since the top layer is equal to the amount of naphtha that was added.

Maybe it's just some sort of emulsion? would it hurt to add salt at this point?

Depending on how much alcohol you used there could still be a significant amount in the concentrated tea. You really don't want a solvent that mixes with both your polar and NP during a defat, or any stage of a liquid/liquid a/b. I would avoid using it in the first place. Most may have boiled off, but not all of it. There will still be alcohol in that solution until you fully evaporate it.

Salt is a good thing to try at this point, but in the future i wouldn't use alcohol in your acid cooks, it doesn't really serve any purpose and can cause problems later on.

Thanks for your kind and helpful response:thumb_up:

 

[rudder]

(The salt didn't really do anything)

Well somebody who isn't me decided to take off the naphtha floating at the very top of the jars, and then just dump the rest of the jar contents back into a stainless steel pot and boil the mixture for another 2 hours until reaching an apple sauce consistency. Then they put it back into the original jars, added a bit of water, and then added a lot of liquid NaOH and KOH.

Then about 250mL of bestine (N-heptane) was added to each jar and tilted/rolled/inverted/etc. slowly.

 

[The Day Tripper]

(The salt didn't really do anything)

Well somebody who isn't me decided to take off the naphtha floating at the very top of the jars, and then just dump the rest of the jar contents back into a stainless steel pot and boil the mixture for another 2 hours until reaching an apple sauce consistency. Then they put it back into the original jars, added a bit of water, and then added a lot of liquid NaOH and KOH.

Then about 250mL of bestine (N-heptane) was added to each jar and tilted/rolled/inverted/etc. slowly.

Thats a good idea, another thing you could do, is create an acidified salt saturated solution, and mix your naptha from the first pulls with that. Should pull any crap out of the naptha, and allow you to re-use it to defat in the future, the water should pull out the alcohol, and the salt/acid should help with emulsions.

Adding a lot of koh/naoh definitely is one of the better ways to kill emulsions ime. At least it worked with cactus alot of the time. Better than salt, but you are using something harder to acquire (relative to your location), and more expensive than salt. A hot water bath with the lid open to prevent pressure build-up, and a few hours on top of a sub-woofer or other vibrating surface can help alot too. Rolling works pretty good, but takes alot of time effort, yet is somewhat relaxing and meditative, if that makes any sense. Your just occupied with such a simple task, your mind is free for all kinds of stuff, or nothing at all, which is something in and of itself, and what many call meditation.

 

[rudder]

the rolling mentioned in my post is for mixing the layers, not for breaking emulsions. I only do it for about five minutes.