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Extracting mescaline from dried Peruvianus skins


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#61 greenskeeper

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Posted 13 May 2021 - 04:29 PM

Separating funnel!! fuck yeah I wish I could get one. Actually I get a stolen one once but it broke before I used it :(

Are you planning to use to drain off sediment? I'd like to see how that goes.

 

The finest filtering is achieved when the sediment layer becomes the filter, on top of the cloth. For this, the whole amount to be filtered goes in the filter (in my case, cloth on a strainer) and is left to settle. The first liquid to come through the cloth has particles in it but once the sediment layer has settled on the cloth it will come through clear. The whole thing must be left undisturbed and totally still until it is finished.

 

Edit: I never worked with powdered cactus so your particulate matter might be different to what I had.


Edited by greenskeeper, 13 May 2021 - 04:41 PM.


#62 greenskeeper

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Posted 13 May 2021 - 04:35 PM

At this stage you could reduce the volume first for practical reasons.



#63 el_ronhub_bird

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Posted 13 May 2021 - 04:51 PM

@greenskeeper yes I have a little setup doing exactly what you describe; solution filtering through fabric but also through the layer of fine silt sediment that has settled on top of the fabric. The pic shows the only remaining solution, maybe 50ml tops, slowly dripping through the fabric. The rest of the solution is reducing on the stovetop. And yes I intend to try to separate out any sediment using the funnel if there is any sediment left

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#64 Phineas_Carmichael

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Posted 13 May 2021 - 10:04 PM

Looking good, Bird!

Piece of advice, don't try to use your Sep funnel to get rid of the sediment, it'll just clog the funnel.

If you really want to get every last bit of sediment your best bet is to use a pair of regular funnels with cotton balls stuffed in the neck. Pour your reduced solution into the first funnel & let it drain until it clogs. Then pour that clogged funnel into the 2nd funnel & replace the cotton balls in the first. Go back & forth like that until all the solution has gone through.

You could also clarify with egg whites like cooks do to make consommé...

Edited by Phineas_Carmichael, 13 May 2021 - 10:04 PM.

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#65 Norman

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Posted 13 May 2021 - 10:31 PM

But don’t try the consommé trick if you reduce your solution too much!
I found that out the hard way. The idea is that you whisk the egg whites into the mix and bring up the heat slowly so the albumen coagulates and floats gently to the top where it is removed. My cactus tea had been reduced to a medium syrup and once the egg coagulated it couldn’t float up through it and the whole thing set up in the pot like a foul jello.
Consommé is clear and it’s also thin. There’s a reason that if you want a clear demi you clarify the stock before you reduce it.
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#66 el_ronhub_bird

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Posted 15 May 2021 - 01:02 PM

Everything has been reduced down to 750ml of a dark brown syrupy substance. I'm preparing to defat and I've gotta couple questions. What type of HDPE plastic container will suffice to shake the xylene and cactus soup, is a regular milk jug good enough? And should I apply heat or do it at ambient room temp? Thanks guys!

Edit: for some reason it didn't occur to me that it will all fit in a half gallon Ball jar along with enough room to shake. This should suffice, no?

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Edited by el_ronhub_bird, 15 May 2021 - 02:10 PM.


#67 greenskeeper

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Posted 15 May 2021 - 05:23 PM

I like HDPE milk bottle because it's light weight and can expand to accommodate the extra gas released by the initial shake. First time I tried this in a glass jar the pressure increase popped the lid off and made a mess.
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#68 Norman

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Posted 15 May 2021 - 07:34 PM

Second that. ^

You’re probably going to want to be using heat throughout since you say the solution is syrupy. Emulsions can be broken but it’s much easier if you don’t get them to begin with.

#69 Phineas_Carmichael

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Posted 16 May 2021 - 01:00 AM

Is there a reason we're not defatting in the Sep funnel?

1) Close the stopcock at the bottom.
2) Pour room temperature cactus solution in & add non-polar solvent.
3) Stopper the funnel at the top.
4) Gently invert the funnel, making sure the stopper doesn't leak.
5) Point the business end away from your face into the hood (or the shower) & slowly open the stopcock. Listen to the WHOOSH!
6) Close the stopcock & gently turn the funnel right-side-up again.
7) Repeat steps 4-6 five or ten times, allowing the layers to settle completely between repetitions, keeping an eye out for emulsions, before draining the cactus solution off the bottom.
8) Discard (save until the end just in case) the non-polar solvent.
9) Repeat steps 1-8 3 times before moving on.

Gentle mixing will help avoid emulsions, shaking will encourage them...

Edited by Phineas_Carmichael, 16 May 2021 - 02:02 AM.

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#70 el_ronhub_bird

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Posted 16 May 2021 - 01:04 PM

Last night everything was placed in a milk jug and shaken (I know some recommend against this but I was reading along a thread where this was the action taken.) Then it was all placed in a jar for observation. This is how it looks after settling overnight. The reason I didn't do it in the sep funnel was because I thought there wouldn't be enough room to shake or roll the contents. My intent was to use it only for the final separation.

How does this look so far? Should I shake or roll it some more? So far this was done without heat, should I warm it up and give it another shake or roll? Thanks!

Edit: I used only 150ml xylene, it's all I had left. I'll have to grab some more

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Edited by el_ronhub_bird, 16 May 2021 - 01:09 PM.

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#71 Norman

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Posted 16 May 2021 - 02:02 PM

I’d siphon off the black layer and shake all that foamy shit with some hot salt water with a splash of acid added to it.
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#72 Phineas_Carmichael

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Posted 17 May 2021 - 12:13 AM

Pour the whole thing into your Sep funnel & let it separate for as long as you can stand to wait, then drain off the bottom layer.

That top layer is a killer emulsion. Norman's got the right idea, break it with salt & acid, but stop shaking shit!

Mayonnaise is a beautiful emulsion; the Condiment of the Gods lol. We make it in the kitchen with egg yolks (non-polar fats) and lemon juice (aqueous/polar acid) and oil (non-polar solvent) by whisking (shaking) them together. Mayonnaise is exactly the emulsion we want to avoid when "defatting" our cactus juice.

Unfortunately, mayonnaise is exactly what you get when you shake a jug of acidic cactus juice with a non-polar solvent. The Mayo just gets trapped between the layers as "foamy shit"...

Be Gentle! Or as my dad always said, "Don't force it!"

(Other Pearls of Wisdom from Mr. Carmichael include "When rushing to the toilet focus on Retention, not Speed" and "It's okay to take to take the pills your Doctor prescribed, but watch your ass if you crave those pills when the refills run out!")

Mix that emulsion layer with a little bit of salty vinegar water in a jar & swirl it around. Put the jar in a hot water bath for awhile & swirl it again. Repeat as necessary. Eventually all 150mL of xylene will float to the top & you can separate it out with your Sep funnel.

[EDIT]You have a Sep Funnel! Use it!!![/EDIT]

Edited by Phineas_Carmichael, 17 May 2021 - 01:35 AM.

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#73 el_ronhub_bird

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Posted 19 May 2021 - 01:42 PM

@Phineas yeah I was just following along a thread and had already shaken up the mixture before you posted your warning not to, I'll avoid it from here on.

Anyway the mixture has sat in the sep funnel for a couple days and I just did the separation. Today I'll work on doing a second fat pull from the bulk of the solution that I've separated out and work on breaking the emulsion in a separate jar. I'll post update pics later on or tomorrow
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#74 el_ronhub_bird

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Posted 20 May 2021 - 12:23 PM

So 100ml water+50ml vinegar+1/2 tbs salt+heat was sufficient to largely resolve the emulsion, all that remains of it is a thin line of foam between the other 2 layers. You can see this in the pic of the sep funnel. The bulk of the solution was heated with another 150ml of xylene for a 2nd fat pull. Even after vigorous shaking the 2 layers would separate completely in a matter of minutes. Now I know I was warned against this (sorry Phineas) but I built up to the shake. I started by just rolling and when I saw how easy it was separating I gradually worked up to a full on shake. So the resolved emulsion and the rest of the solution were separated from their respective xylene layers in the sep funnel and then the xylene was combined in a jar and the solutions were combined in a different jar, this is shown in the other pic. I was told to hold on to the xylene for now so I will. So do you guys think I should do one more fat pull before I proceed?

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#75 Phineas_Carmichael

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Posted 20 May 2021 - 03:46 PM

If you absolutely feel the need to shake, that's the way to do it; gently at first with increasing intensity & allowing the layers to separate between step-ups. You'll almost never see anyone shaking anything in a chemistry lab, but I have to remind myself that this is clandestine chemistry, & there are multiple routes to the same end product.

One more defeat can't hurt, especially if the xylene keeps coming out that discolored. Keep up the good work!
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#76 greenskeeper

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Posted 20 May 2021 - 03:57 PM

Isn't most of the mixing in chem labs done by machines? Swirling a bottle is nice and relaxing at first but can get quite tiring after an hour or two.



#77 Phineas_Carmichael

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Posted 20 May 2021 - 05:54 PM

Long-term mixing (say in a reaction vessel for polymer synthesis) is usually done with magnetic stirring. Often there's an undesirable product (water or an alcohol) that is being distilled off the reaction vessel to drive the reaction to completion so one is left with just the desired polymer.

Mixing for liquid-liquid extraction (what we're doing here) is done in the Sep funnel as I described above. The organic phase is usually saturated after a few inversions of the funnel & subsequent separation of phases (layers) due to the ratio of aqueous (polar) to organic (non-polar). More mixing at this point can't force anything more into the organic. That ratio is also why we do multiple extractions (pulls) to get all the stuff we want out of the aqueous.
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#78 pharmer

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Posted 20 May 2021 - 07:02 PM

Phineas, if he does more defatting should he be bumping up the acidity with each defat to be sure to keep the target isolated in an acid environment or would the acidity remain constant?



#79 el_ronhub_bird

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Posted 20 May 2021 - 07:25 PM

Here is the 3rd fat pull. It was completely separated but mixed up a bit when poured into the sep funnel. The other pic is the xylene left after separating the solution off the bottom.

If everything looks good then I'll move on to basifying. How much lye should I start with? Any other advice for this step? I have ph papers for testing. Thanks!

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#80 Phineas_Carmichael

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Posted 20 May 2021 - 07:47 PM

Phineas, if he does more defatting should he be bumping up the acidity with each defat to be sure to keep the target isolated in an acid environment or would the acidity remain constant?


Acidity should remain constant as the acid is not soluble in the non-polar and the stuff that is doesn't affect pH in theory. Theory and Practice are 2 very different animals though, so a quick check of the pH between defats is not a bad failsafe. Probably not necessary, but not a horrible idea either. Kind of like wearing a motorcycle helmet & a seatbelt in your car on the off chance that your seatbelt fails & you get ejected in an accident.

...
If everything looks good then I'll move on to basifying. How much lye should I start with? Any other advice for this step? I have ph papers for testing. Thanks!

Theoretically, 40g NaOH per 1L of distilled water gives you a pH of 14. Since you're starting with 750mL of an acidic solution I would start with 40g & see where that gets you. I've never added crystalline lye directly to the acidic solution, so I hope Greenskeeper will chime in, but here are my precautions:

Chill the solution in the fridge for a while and put the jar in an ice bath for the basifying. NaOH releases a lot of heat as it dissolves & we want to keep the solution from heating up so much that it damages the freebase. Add the crystals slowly, 5-10g at a time with constant stirring during each addition. Make sure all the lye dissolves & give the solution time to cool down between additions. Might even start checking pH halfway through...

Oh yeah, don't forget your gloves and goggles!
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