Mayo level emulsion - please help

[Anciaki]

*record scratch*
*freeze frame*
Yep, that's me. You're probably wondering how I got here.
*flashback*

I start by saying that this is the third time I have done an extraction: the first time I did a simple StB with Naphta and the second one was an A/B with limonene that yielded Jungle Spice.
This time, however, things went differently. The initial plan was to follow this Tek ( Lextek - DMT-Nexus Wiki ). Right when I finished the acid cook, since until then the two Teks were pretty identical, and given that I was using a starting amount of Mimosa that is much less than in the Tek of my choice, a friend suggested to instead follow this other Tek: Cybs' Hybrid ATB 'Salt' Tek - DMT-Nexus Wiki .
Everything was going smoothly until I started getting some nasty clumps already in the Acid Cook phase. Something similar happened in this other thread from Reddit: Did I just ruin my acid boil?!, but adding more vinegar didn't resolve the issue.
Well, I thought that after the caustic soda part everything would have resolved, given the strong corrosive power of the chemical. Initially, thanks - I guess - to the heat released by the exothermic reaction of NaOH solution into water the clumps dissolved. I exulted euphorically and proceeded to add the NPS of muy choice, hexan, but later when it cooled down, I was negatively surprised to find new nasty clumps and they were getting bigger minute by minute. It was then that I thought I had an ingenious idea: I had a full stainless steel immersion mixer and thought to use it to solve the clumps problem... Soon after I realized the magnitude of my mistake. I just made a very thick emulsion.

Since, I tried few things:

• add more water along more NaCl and NaOH, to increase ionic strength and maybe aid in the separation of the non polar solvent: it only made the solution thicker;
• use a vibrator that I happened to have laying around, for hours on end in the hope that vibrations would contribute to break the emulsion, with little succes;
• heat and cooling cycles, that probably resulted in the evaporation of a good bit of the hexane supersaturating the solution and making it possible for crystals of this size to form at room temp (~22 degrees Celsius).

48 hours later now, hasn't still fully separated and DMT crystals started forming on top...
I really do not know where to go from now onwards. Any suggestions?

• Should I dilute more, given that the thickness of the base soup might hinder the separation between the two phases?
• Should I try a second pull and maybe some of the emulsified hexane will be retrieved by the new non-emulsified hexane?
• Anything else?

Thank you in advance for you attention and for helping me in this difficult situation.

 

[pantostao]

If you dillute it, it will resolve easily. How is the MHRB to water ratio? I've had good results using around 1g to 10ml of water, some people prefer 1g to 15ml. Less than that, and emulsions can be very tricky to resolve.

Other than that... yeah, you've said it all: Water, salt, base, heat, vibrations. All of those can help, but it won't help if the soup is too thick in the first place.

 

[Anciaki]

I used 100g MHRB, so for a total of 600mg of liquid (before adding 100ml hexan) the ratio is 5:1

 

[The Traveler]

I used 100g MHRB, so for a total of 600mg of liquid (before adding 100ml hexan) the ratio is 5:1

Adding more water will certainly help, a ratio of 5:1 is really low on the water side. I myself prefer 15:1 to have no issues with emulsion.


Kind regards,

The Traveler

 

[Tryptamineenthusiast]

Hello Anciaki.

Here are some thoughts that might or might not be helpful from a third-year undergraduate chemistry major (not that that means much). Hexanes evaporate very quickly even at room temperature so it seems somewhat possible that a large portion of your solvent evaporated over the course of your process, this is especially possible if some of your NaOH was not fully dissolved before the immersion blender step as it may have increased the temperature of your mixture. The fact that crystals formed on the top means that there is simply no longer enough solvent to dissolve them (and I doubt that the emulsion would would effect solubility much) so it is quite possible that there is much less emulsified solvent than you think. If you have already considered that (which you very well may have) then I agree with others' posts and your only options are to increase the amount of water even more or wait up to a month. I have personally found that, given enough time, even the toughest emulsion will separate.

One final thought. Though I do not know very much about chemical means of emulsion breaking preliminary research on my part suggests that hydrocarbons containing alcohol groups can chemically break emulsions, this is probably more of a last resort, but if nothing else works that might (though perhaps this is through the same mechanism as you mentioned with NaOH). Obviously alcohols are pretty polar so some research on solvent miscibility would be important as well to ensure that you are still effectively dissolving the DMT. There may be other ways of chemically breaking emulsions which could be useful to research if you havent already.

I hope I have offered something you have not yet considered,

Sincerely,

Tryptamine enthusiast

 

[Anciaki]

a ratio of 5:1 is really low on the water side

I see your point. Well, now I did dilute it by doubling the volume with distilled water and more salt (about 15 grams per 100ml of water) so it should be closer to 10:1.
As I did that, I saw already a thin layer of oil forming on top.
Anyway, to avoid confusion, I have to mention that, as the Lextek indicates, I have filtered already all the plant matter with a cotton cloth and discarded it. And the 600ml liquid is what is left over from reducing the liquid obtained with the acid cook. So it was 500ml of reduced and filtered acid cook liquind and 100ml hexan.
Now what I have is a more or less a liter of black hexan smelling soup.

there is much less emulsified solvent than you think.

well. yesterday I diluted the soup with boiling water and as it mixed many tiny bubbles creeped on the surface. So there is definitely still hexan.

As another extreme situation I was thinking to boil the hexan off while keeping it in a hot bat at 70° to 80° as it is the alkane's boiling point.
This way I could have a fresh start and proceed again and perform new clean pull.


Bonus picture, before melting it back in the soup, I collected one of the crystals and took a nice shot!

 

[The Traveler]

Bonus picture, before melting it back in the soup, I collected one of the crystals and took a nice shot!

Lovely crystal!


Kind regards,

The Traveler

 

[Transform]

Beware of evaporating significant amounts of n-hexane - it's neurotoxic!

Heating base soup is also a bit risky as it can cause glass vessels to fail. Decent newish lab glass should be OK.

One more thing - are you sure your hexane is hexane and nothing else? I recall this one time a guy thought he was extracting with limonene. It turned out he'd used citrus-based cleaner, which was detergent and about 5% limo.

 

[Anciaki]

are you sure your hexane is hexane and nothing else?

Thank you for warning me. Yes I am sure 100% it's hexane. I bought it from a chemical supplier. It smells like hexane. I have used hexane in the past.

Beware of evaporating significant amounts of n-hexane - it's neurotoxic!

Heating base soup is also a bit risky as it can cause glass vessels to fail. Decent newish lab glass should be OK.

And thank you for the disclaimer! I will take all the precautions: windows open and I'll use borosilicate glass.
I have put the project on standby as I had some work and life urgencies to deal with. Next week will resume the extraction.

 

[Transform]

Main thing is if you've added enough water yet. The delay may help the situation clear up at least a little bit.

If it still persists you can try vacuum filtration or, in the absence of that option, vibration. A sex toy is useful here but an electric toothbrush might do the job too.