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Powder MHRB STB Extraction with NaOH, NaCl and toluene => Huge emulsion

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pete666

Esteemed member
Hi guys,

should be in DMT Extraction-STB thread, but I don't have access there. Please move it if you can.

This post is meant to be purely informational for someone who might think the same way as me - to add plenty of NaCl and don't have to bother with emulsions.

Well, I am just in the middle of STB MHRB extraction, from powderized bark. I have decided to test how good is NaCl at preventing emulsion problems, so decided to go with (rather low) 10ml of water for 1g of bark and 1g of lye. Vessel was left one day with occasional shaking before np was added. After additon the mixture was violently shaked for about 3 minutes in total. Plenty of air in the vessel allowed to shake it really well.
After few minutes two layers separated perfectly, without any "emulsion" layer in between. The problem was that what was missing was not the emulsion layer, but the np layer. The top layer was consistent emulsion, without any bigger bubbles. The bubbles were impossible to see by eye, they were very small. The emulsion was very stable.

In short, emulsion was separated, excess water wass added - nothing. Excess (more than could be dissolved) NaOH was added - nothing. Excess (more than could be dissolved) NaCl was added - nothing. 60C bath with stirring for about one hour - nothing. 20 minutes heated on vibrating washing mashine - nothing.

I will try alcohol and water washes and let you know whether it worked.

*EDIT : Emulsion was solved, if interested, just read on...*

But the result is : DO NOT EXPECT WONDERS FROM NaCl FOR EMULSION PREVENTION. At least for some kinds.
NaCl helped me a lot with mescaline extractions, but here it is another tale...
 
Thanks for your answer.
The aim is to place everything into the vessel at the beginning and flush it at the end. All is fully isolated within the vessel, no cooking, no filtering, no mess.
Another reason is to avoid any temperatures higher than 30C
 
You may try very slow and long stirring and/or vibration. There was a thread where people attached a mobile phone or vibrator to the container to break the emulsion.

I was researching some advanced emulsion breaking agents but it was very complicated topic and totally not worth the extra effort (required at least 3 extra steps).

Now I simply filter the bark, reduce and filter again using round paper filter (I have a very large Buchner funnel). It is more work but less emulsion in the end.

The pressure cooking looks promising - will try that!
 
I liked the tip to use some vibrating device attached to the vessel and used my powerful aquarium pump fixed by tapes. The glass vessel was vibrating quite a lot.

After 10 hours - nothing :( The emulsion is still intact

I've read somewhere that the emulsion could be dissolved by ethanol. I believe it might be true. The problem is I don't have an idea what to do with the resulting mix. DMT is soluble in ethanol and I suspect some would go there rather than to np. So this is probably not the path to go...

Anyway, my aim is not to break the emulsion, but to find the way how to prevent it. I will discard this and try few another combinations of water/lye/NaCl.

If anyone wanted me to try something with the emulsion, just let me know before I flush it
 
blue.magic said:
The pressure cooking looks promising - will try that!
180mins @ 15 psi, you can literally shake it on the first pull. Emulsion doesn't form.

It does pull a lot of oils though so a backsalt is essential with Acacia plant sources, or you could just be loving cheese and bright yellow xtals with MHRB.
 
pete666 said:
If anyone wanted me to try something with the emulsion, just let me know before I flush it
Add acid, evaporate all volatiles and start again. Be more careful with the shaking next time!

There's no need to chuck it away, especially since it contains toluene. If you have distillation apparatus you can recover your toluene as well.
 
downwardsfromzero said:
Add acid, evaporate all volatiles and start again. Be more careful with the shaking next time!
Yes, I was thinking about that as well. Acidification of the emulsion is one of the advices I found on the web. PH to 2-3. It was not dmt-related source but maybe it is worth try. If it doesn't help, I might try to simmer it for a while. Once dmt is in the salt form, it should be ok. If that doesn't help, the evaporation seems to be the only remedy.

Initially I was not interested in solving emulsion :) I wanted to avoid it. I was shaking violently intentionally hoping that the excess NaCl will help.
Anyway, when I have such a nice emulsion, I will try the acidification an simmer.

downwardsfromzero said:
There's no need to chuck it away, especially since it contains toluene. If you have distillation apparatus you can recover your toluene as well.

I have, but I am trying to stay on the safe side
 
Thanks for tips guys

Anyway, I have successfully broken the emulsion yesterday.
The emulsion was separated from the extraction vessel, put into beaker and HCl was added. When PH was about 2-3, the emulsion magically disintegrated. Within seconds I had toluene and white water layer perfectly separated. No even simmering needed

The solution was basified again and exctracted 3x with toluene. Then it was returned back to the extraction vessel for next pull(s)

I would say there had to be some water, so it wouldn't hurt adding some if the emulsion was separated without it.

So, just a small tip how to get rid of this nasty emulsion for someone who might be so lucky to have it. Just bear in mind that I have used NaCl in the extraction, so maybe the emulsion may (or may not) be correlated with that.
 
downwardsfromzero said:
The emulsion is correlated with the particulates from the powdered bark used, combined with excessive shaking and maybe insufficient water. IMHO.
I think so as well. But there is no enough data to be 100% sure, therefore the notice.
The water was fully satrurated by NaCl, so there might be enough water, but it was too 'thick'
 
pete666 said:
downwardsfromzero said:
The emulsion is correlated with the particulates from the powdered bark used, combined with excessive shaking and maybe insufficient water. IMHO.
I think so as well. But there is no enough data to be 100% sure, therefore the notice.
The water was fully satrurated by NaCl, so there might be enough water, but it was too 'thick'
If the brine is too viscous, that's the same as insufficient water :D
 
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