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Never ending emulsion problems... Options
 
blue.magic
#1 Posted : 2/7/2019 9:41:28 PM

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I stopped counting how many times I tried mescaline extraction. I tried different methods (A/B, STB, alcoholic + A/B), different solvents, acids, bases etc ... and it always, always ended up the same: horrific emulsion that simply does not go away.

Last time I placed a bottle with emulsified xylene on a bench and left it there for 3 weeks. Guess what. The emulsion stayed the same.

Today I tried again, 14th time or so. Even de-fatting resulted in basically pure foam, trapping lots of mother liquor in it.

I applied heat, gentle stirring, even added fresh xylene and brine only to thicken the emulsion even more.

I am out of ideas and utterly frustrated.

I have even tried to break the emulsion with anhydrous calcium chloride, which works in such cases and clears up the solvent. Not in this case. It only created cloud of bubbles that simply sit in the flask for weeks. Adding more salt has no effect whatsoever...

The mother liquor behaves in mysterious way since mere defatting causes appearance of chunks in it. Adding base followed by acid also results in chunks. There are probably some reactions not documented and affecting the extraction.

I am probably done with mescaline extractions and learning the synthesis will be much more fruitful. Maybe the cactus does not want to give its magic to me.
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endlessness
#2 Posted : 2/7/2019 9:58:28 PM

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From your description it seems you didn't try some of these suggestions: https://wiki.dmt-nexus.m...eparate.2C_what_to_do.3

like the speaker/vibration.

Also you said adding calcium chloride, but did you try sodium chloride instead, and adding tons of it?

Am I right to assume this is not during a defat but during the pulls? How basic is the solution?

Are you shaking it hard, and if so, don't, or how are you mixing the layers?
 
Jees
#3 Posted : 2/7/2019 10:34:50 PM

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Hi BM,

I've hinted before about freeze/thawing the emulsion, have you tried that?
I realize that the expansion could cause a flask to break so that must be taken into consideration. Filling a flask to 50% and then laying it on its side, there must be room enough for the expansion. I had good results in killing hard emulsion in 2 freeze/thaw cycles, but it was not cacti. Just telling.
 
blue.magic
#4 Posted : 2/7/2019 11:38:13 PM

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Hm - I never tried speaker or vibrator, but I don't believe this would work since even gentle swirling caused emulsion. It seems any kind of agitation only worsen the situation.

I added like 200 grams salt and I have 1 400 mL water per 200 grams of cactus powder.

I am actually looking for some way to avoid emulsions altogether - remove the actual cause of them instead treating it once it happens.

Freeze-thawing might work, though again this is treatment of a problem - I would like to avoid it completely.

I though the emulsions are caused by fats so I de-fatted and no - they happed still.

I tried adding ammonia instead of lye only to pH 10.0 - still got emulsions.

In acidic environment, the emulsions slowly die away. But in basic it's permanent.

In one experiment, I added re-acidified the emulsified system and indeed the emulsion died away. The emulsion formation has something to do with solution's pH.

So finally I tried alcoholic extractions (tried MeOH, EtOH and IPrOH with MeOH giving best results). The methanolic extraction didn't cause any emulsions but once I scaled up the extraction to 150-200 grams of dried cactus, the emulsions were as horrible as with A/B or STB teks...

Now I found one interesting paper where they did alcohol extraction, then completely rotavapped off the solvent and dissolved the resin in dilute HCl. Then they de-fatted the liquor with chloroform, basified with NaOH and extracted with chloroform.

I don't have any chloroform at hand (I plan to synthesize some though, just for the extraction) - maybe this might finally work but after so many failed trials, I am skeptical.

I have even dried and powdered only the fresh cactus flesh and sourced different wachuma powders from Peru. I tried freeze-thawing fresh cacti several times to break it down more. I tried mixing it with copious amount of base and let sit for several days. But every time I get the same result, which is an horrific emulsion.

Today I defatted the acidic liquor (acidified with HCl) and left it to stand to think how to extract it without losing everything to emulsion again.

Sorry for sounding negative. I got truly frustrated by this - it's over 2 years of trying. I already mastered all other extractions, but mescaline is the only one that simply does not work.
 
KloudQ7
#5 Posted : 2/8/2019 12:06:28 AM

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Usually if I put excess lyeand salt and let it sit for a day before pulling it kills the emulsions
 
blue.magic
#6 Posted : 2/8/2019 12:28:52 AM

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Okay I will try that.

What is interesting is that almost no tek talks about using salt - like if tek writers never had significant emulsion problems for some magical reason but I had terrible emulsions right from the start. I really wanted to solve this problem once and for all.

I am thinking about removing some component from the cactus that causes it. It's not fine particles as I filtered the tea extensively with very fine filters and still emulsion happened.

Maybe there is something like bound proteins - maybe protein removal - like in Loveall's psilocybin extraction - might help with it.

My goal is to have a clean, scaleable and reproducible extraction. So far every cactus extraction turn out very differently - sometimes it magically works and sometimes it fails completely.
 
pete666
#7 Posted : 2/8/2019 6:21:38 AM

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You have likely seen in this thread STB with salt can be used with very good results. There is no emulsion in any stage of the process. Yes, it was tested just with 3 various fresh cacti and one type of powdered one, but the results are very positive as you can see.

I have many various cactuses waiting for extraction, so this method will be tested much more thorougly shortly, but even with current results, I am quite convinced it can be used for most trichos.

What cactus are you extracting?
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Psilosopher?
#8 Posted : 2/8/2019 7:59:30 AM

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I don't know if this will help, but may be worth a shot. If you have a washing machine, place the flask on top of the washing machine when it's going high speed. Don't walk away from it, cause it may shuffle off the washing machine and shatter on the floor. I use an ultrasonic water bath to resolve emulsions extremely effectively, so a washing machine may serve as a ghetto ultrasonic surface.
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endlessness
#9 Posted : 2/8/2019 10:09:06 AM

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blue.magic, before saying vibration "wouldnt work", maybe try it out. It has been tested many times and shown to work. The more techniques the better no?

Im still wondering how is it that you get so much emulsion. How are you mixing your layers?

You say you want to not fix the emulsion but prevent it in the first place... Try adding the tons of salt and lye before the first pull.. And then only do gentle stirring with a spoon (or a magnetic stirrer on low speed first) , dont agitate it all, dont shake... I've done this many times with cactus and never really had such problematic emulsion, either none at all or just a bit that is resolved. That being said, I've always worked with fresh cact, never powder, I wonder if that might be related.
 
pete666
#10 Posted : 2/8/2019 10:37:27 AM

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Just my experience...

Vibrations are not bad, but for me definitely less effective than heat and time. Sometimes it is even better just to turn the bottle over now and then without shaking than continuously vibrate.

I understand bm wants to find the way how to live without fear of emulsions. I shake without limits and I really appreciate it.

Nevertheless, I strongly suggest asking the powers behind the medicine. This helps a lot.
Acceptance of the fact that our reality is not real doesn't in fact mean it is not real. It just leads to better understanding what real means.
 
endlessness
#11 Posted : 2/8/2019 10:54:22 AM

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pete666, yeah I think to resolve complex emulsions all the techniques should be used together to maximize the effect, including heat and time. Vibration is just one more, but since blue.magic said he didn't try it, I thought he might as well try it.

Do you extract with powdered cact too?
 
pete666
#12 Posted : 2/8/2019 11:36:28 AM

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Yes endlessness, that is clear and fully agreed.

All my full-blown extractions were with powder, which was torch from Peru.

Those with live material were just for testing purposes. But this is gonna change, as this season I expect first self-grown species ready to go. I don't see any reason why I should do powder onwards.
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DansMaTete
#13 Posted : 2/8/2019 1:51:55 PM

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I rarely have problem with emulsion (and i shake like crazy) but when it happens it's cause i reduced too much before adding lye and/or didn't cook long enough during the acid phase.
Most of the time i work with fresh material (freeze/thaw, pressure cooker) so ymmv.





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blue.magic
#14 Posted : 2/8/2019 7:20:48 PM

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Pete666 - I tried this but this didn't work. It took lots of KOH and the soup sat in a pot for several days, it haven't helped with the emulsion a bit. So I am skeptical about that approach at the moment. I made a photo assay earlier showing how it went. I am glad it works for you though.

endlessness - I said I just don't believe vibrations would work, I would be pleasantly surprised if it will of course. The problem is I have very little time and busy with so many projects, lots of stress. Any extra experimentation is now just another time killer and more stress so maybe I will leave the extraction for another time...
I use 2 000 mL separatory funnel for the layer separation. Just pouring xylene in it will result in some stationary bubbles. Swirling is mostly okay, but slightest agitation or inversion will immediately emulsify the layers.

I also don't like to use excess base to avoid:
1) breaking down mescaline
2) causing saponification of fats - leading to even worse emulsions

I also wanted to extract at least 15-20 good doses of mescaline and I calculated this would require huge amounts of base - I try to limit purchasing chemicals to a minimum so always looking for ways around. I also want to make my extraction as eco friendly as possible, so right now I am almost at the point of abandoning the extraction due to the amount of chemicals, waste and work involved.

I will try the vibrations. I may try an unused vibrator from my GF Embarrased . Ultrasonic bath is a great idea. Adding it to my wishlist!

I am not sure about the cactus species. The powder was obtained from a peruvian vendor as is, most likely some generic T. Pachanoi.

Yes concentration is definitely a factor. But I made 1 200 mL from 200 g of powder, which should be OK. It is still thick though and the bubbles of xylene have hard time to travel up. I can add more water but then I won't be able to fit it in my 2 000 sep. funnel and do twice amount of work.
 
Elrik
#15 Posted : 2/8/2019 7:40:25 PM

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Some thoughts:
Is your cactus brew too concentrated? I would always get emulsion problems until I set a rule for myself on concentration of cactus tea. I now will not exceed 100 grams of dried cactus, boiled 4 times, for each 400 ml of final tea volume. That rule greatly improved my process.
I've tried the sex toys and heavy metal tactics for breaking emulsion. Sex toys do help some but a magnetic stir bar set to low speed helps more.
What water are you using? Contaminants in the water could be contributing.
Are you doing acid boils in aluminum pots? Sodium potassium tartrate is quoted as helping to resolve emulsions caused by aluminum salts. If you add cream of tartar to a based solution, sodium potassium tartrate is formed.
Is it possible your NPS contains some compound promoting emulsions?
If you can do distillation, an equal mixture of water and xylene boils at only 92º and most of our other solvents behave similarly. Once I got the appropriate glassware I stopped using solvents straight from the can.

I've heard of people adding lye to isolated emulsion to break down the cause of the emulsion.
Similarly, if you have very good pots and ventilation, after making the cactus tea hydrochloric acid could be added to pH 1 and it could be kept warm for hours to try and hydrolyze things.
At times I resort to centrifugation, in fact I did last night and am doing so again tonight. Its a pain in the ass, though, my old centrifuge only holds 90 ml Laughing

But I agree with you, best to find and eliminate the cause.
I'd be looking at the water, the concentration, and possible contaminants.
 
endlessness
#16 Posted : 2/8/2019 8:05:22 PM

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blue.magic,

I totally understand if you dont have the time for this atm or dont want to spend the resources. In any case...

blue.magic wrote:

I also don't like to use excess base to avoid:
1) breaking down mescaline
2) causing saponification of fats - leading to even worse emulsions



I assume you are talking theory, right?. Is there any specific fat you know in cact or evidence they saponify and create emulsions? Or any sign of mescaline breaking down?

So far anecdotally AFAIK everybody seems to confirm that more base makes things easier, not more complicated, and yields dont seem diminished and neither any breakdown by-product is found when testing the final product.

You are correct though that this would mean more chemicals and I understand if you don't feel like using up such chemicals. Unless you are doing huge extractions, though, I'd imagine proportionately it is only a small percentage of resource spenditure/ecological footprint in our daily lives in the modern world. I do think it is reasonable to avoid it for your reasons stated, though, so go for whatever you feel is right, I think we gotta follow what our heart says and adapt our research to our context and moment
 
pete666
#17 Posted : 2/8/2019 8:08:11 PM

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blue.magic wrote:
Pete666 - I tried this but this didn't work. It took lots of KOH and the soup sat in a pot for several days, it haven't helped with the emulsion a bit. So I am skeptical about that approach at the moment. I made a photo assay earlier showing how it went. I am glad it works for you though.


I remember that. I just checked again and I can see the main difference between your and my extraction - xylene instead of toluene. This may be the key in your failure. I have some xylene too, maybe I might try it sometimes to confirm that.

But yes, this TEK is definitely not for someone who is limited in chemicals, regardless how reliable it is.

Acceptance of the fact that our reality is not real doesn't in fact mean it is not real. It just leads to better understanding what real means.
 
blue.magic
#18 Posted : 2/9/2019 1:49:23 AM

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It's funny I switched to xylene from toluene extactly because having harder emulsion problems with the toluene Big grin

Well toluene, unlike xylene, bubbles even when poured pure, which made me suspicious. Plus most teks I read called for xylene. But in the end, it's probably not so much a solvent issue.

I watched Willy Myco's Patreon video on mescaline extraction. He used benzene, which is the least polar of the BTX solvent trio, but I would avoid trying tat one due to its carcinogenicity.

I would however try A/B extraction (with HCl, NaOH and chloroform) on resin from alcoholic extraction.

I have currently a flask with the acidic tea waiting for extraction and I will try the emulsion breaking techniques advised (ridiculous amount of salt + vibrations). I am a bit worried about the salt as it released lots of sludge out of otherwise clear soup, which caused technical issues (e.g. clogging of the funnel).
 
AcaciaConfusedYah
#19 Posted : 2/9/2019 4:00:14 PM

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Hi blue.magic,

I've had issues with irritating emulsions from cacti extraction. I'd begun exploring a few methods to avoid it. I started working on something that I think could be promising - but many obligations took precedence. When I have the time, I'll revisit my experiment and get the last component of the marquis reagent. If it works, I'll let you know.

Yeah, emulsions can be a pain in the ass.

ACY
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KloudQ7
#20 Posted : 2/9/2019 5:53:16 PM

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If you want to get 20 doses you need lots of cacti, I extracted a half bucket of powder and got around 10 grams. I use a pint mixer on a drill to do pulls and it takes 2-3 pounds of lye and a lb of salt to get it to separate. Even at such a high pH I haven't seen any evidence of mescaline breaking down.
 
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