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Emulsion like I've never seen

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Northerner

Northerner

Rising Star
So I've been mucking about with psychotria trying to figure out a better extraction tek and have hit a bit of a sludge wall with one attempt.

The leaves were dried and cut up in small pieces than based for a maybe a month in a large jar. I hit the leaves with a stick blender and added plenty of solvent. As the glug was gluggy under the solvent I was struggling to get much surface contact, so I used the stick blender to spin the glug under the solvent. It actually worked great. Then a second time about 20 minutes later, and about 30 seconds into the spin, the glug swallowed my solvent and it hasn't been seen since. This was about a month ago.

I've added copious amounts of salt and tried vibrating and heating it, pH is already over 12... I'm kind of at a loss right now.

Any ideas?
 
Haha.. okay. :lol:

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A thick glug indeed! When I had a thick mimosa mix absorb naphtha in the same way, I added a little more NaOH and tried again with more solvent. Rolling the additional solvent seemed to retrieve some of the lost solvent from the mix. I don't know why or how.
 
I've been heating and cooling it today and it seems to be separating a little, maybe.

I was thinking about adding more solvent earlier too, seems like a good idea somehow. I couldn't find a logical reason why it would help. Worth a shot.
 
stick blender
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There's the root of your problem! Caustic chacruna mayo :!:

The fine particulates from the blending action have provided a wonderfully large surface area for your finely dispersed solvent to stick to, along with the greater proportion of fatty (soapy...) materials present in the leaf when compared to barks.

If I could turn back time... Have you tried swapping the wires over inside the blender so it runs backwards? Maybe that'll untwist the emulsion :lol:


More sensibly, you could try securely placing the jar on top of the washing machine during its spin cycle.

Adding solvent may help by providing a non-dispersed body of solvent for the emulsified solvent to... recongeal?
 
Oh what a mess 😁 :(
Freeze/thaw has undone hard emulsions for me, 1x , sometimes 2x, but dunno about your version of emulsions, maybe worth a try, in a recipient that will not crack!!! Like a wide shallow tray where you freeze-precipitate in. Metal recipients like a little pan or pot....
 
I'm not sure a washing machine would help tremendously.
I've tried sex toys [I really love my lab] and vibration doesn't tend to do a whole lot for really nasty emulsions. That really isn't even an emulsion, more of a thick mixture.
If I had that jar and I were to exhaust all other options I would in the end dump in a large volume of warm water and give it gentle mixing until it separated into a water+solids fraction, a water+solvent emulsion, and a solvent layer. I would then work from there.
DMT is essentially insoluble in basic water so adding four to six times its volume in warm water wouldn't cause massive loss of DMT the way it might with mescaline.

Some emulsions take truly drastic measures. The worst emulsion I ever broke was broken by acidifying with a non-volatile acid, steam distilling off the xylene in an appropriate lab setting, basing, saturating with salt, extracting with isopropanol, acidifying, distilling off the alcohol, basing, and extracting into the distilled xylene.
Isn't chemistry fun? :lol:
 
Well guys, I've been mucking around with it, if anything it looks even worse. This is not the extraction tek that I had hoped for.

It looks like the only way I'm going to break it is to dilute it. It currently has the consistency of greek yohurt. :lol:

I've got a really large jar, hopefully that will be big enough, I don't really want to split it up. Will post an update, maybe a couple of pics later.
 
Did you try more heat? Avoid open flame but keep it HOT for a long time (eg. Jar submerged in water brought up to a gentle boiling water with the lid on but loose). I have never met an emulsion (so far) that didn't resolve near the solvent boiling point. I allow to cool before pouring off.

Just be careful since this is a hot base (very corrosive) and hot solvent (very easily ignitable). Know the risks and make your own call (as you may know already).

Good luck
 
Keep in mind that hot base eats through glass [not to mention flesh] and naphtha water mixture makes the naphtha boil below the boiling point of water. How far below depends on your naphthas constituents, for instance n-heptane and isoöctane get reduced to boiling at 79°C.
I don't like heating water-xylene emulsion to 60° because it suddenly makes the whole house just stink of xylene despite water-xylene not boiling until 92°.
Use very good ventilation with heat.
I'd just dilute rather than going above 60°.
 
Hopefully Northerner doesn't mind me tacking onto his thread but I'm having a similar problem with no-man's tek. I followed all the proportions but I've been using 1-2 days for each pull and aggressively shaking each pull throughout the day.

After the third pull each pull comes out with less than half the amount of hexane that went in. Adding salt did nothing. At least 30ml of hexane has simply disappeared into 500ml of water. I'm thinking its gone into the sludge at the bottom which appears thicker and less silty then at the beginning of the tek.

Its also unlike other emulsions I've experienced which are clearly bubbly and eventually resolve with time and salt. I guess with these thicker STB teks it really is like we're making mayo, and mayo attracts more mayo (hence why I only had problems with the later pulls.) Not aggressively shaking / blending seems like a must.

Thinking about leaving the jar in the cold weather for a month or so then pouring off the basic solution from the sludge, letting the sludge dry and adding it to my collection of filters and left over dry base teks for a later A/B. Or just throwing it down the toilet as I already got about 0.5% yield ¯\_(ツ)_/¯

Does room temp / cold base eat through glass too? Is my jar in danger of cracking at some point?
 
Lye attacking glass is an acid/base reaction so it happens at any temperature. The reaction speeds up with increasing temperature and increasing lye concentration. Food grade glass reacts much faster than lab grade borosilicate glass, but even lab glass reacts unless its solid quartz. I inherited a 4 litre nitric acid bottle someone filled with 4M NaOH, it never ate through that thick glass but the lye is now converted in part into sodium silicate. :lol:
Back before my time at the nook a guy put a substantial volume of highly concentrated lye in a glass container and then when he lifted it the glass fell apart and covered his lower body, a mad dash to the shower prevented severe burns.

Don't assume glass in the laboratory is borosilicate, it will either say on it or the manufacturers information on the part number will say. I inherited lab equipment from my grandfather and the way I found out his glass mortar and pestle was cheap soda lime glass was I put it in the oven on low to dry the stuff in it and the glass got filled with cracks. :?
 
I've let food grade glass sit for months with basic solutions and they've not crumbled on me. Though I don't tend to keep using that glass again and again. Once it gets a bit old I toss it and grab a fresh one out of the pile.
 
I second what Elrik said. The glass etch rate can increase rapidly with pH and temperature, so if all else fails and if want to you use more heat to deal with the emulsion, then it makes sense to (1) assume the glass can crack (keep a secondary container under it), (2) discard the glass when done, and (3) have easy access to a shower + PPE + all the other usual recommendations.
 
So I added some ethanol. The glug promptly swallowed it all after a very short and very gentle stir and is now bubbling. I was doing my best not to mix the two. With the shocking amount of salt that is in there not surprised there's some sort of reaction, though I am surprised it's visible.

It's on low heat again now and does appear to be separating a little, but has 95% of the way to go. The vapours coming off it smell like hydrocarbons and ethanol mixed.

I don't know if it getting worse or better. :lol:
 
Well time has gifted me something that is akin to jam.

This experiment is getting more interesting all the time.

I'm now considering press filtering the mixture.
 

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At this point I would slowly acidify it (e.g. with citric acid), spread it out in a flat container, let it dry completely, and start over.

I would then do an A/B. The first water pull will be salty, but other than that it should be pretty standard.

However you proceed, best of luck.
 
There's a hell of a lot of solvent and salt in there, as well as the plant fibre.

I was even thinking if I dilute it with water significantly to free that solvent, then use the inverted funnel trick to raise the solvent off the large surface area so I can pull it.

I'm loath to start again... though that may be the solution.
 
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